Professional Documents
Culture Documents
116
2017
Tp ch Khoa hc v Cng ngh 116 (2017)
MC LC
1. Xy dng h INS/GPS theo c u truc ghep long s du ng b lo c Kalman trn c s h INS a c 1 16-152
cai thi n chinh xac
Triu Vit Phng1,2, Nguyn Th Lan Hng1*, Tri nh Quang Thng1
1
Trng i hc Bch khoa H Ni
2
Vin o lng Vit Nam
2. Xy dng thut ton iu khin mng nron da theo m hnh mmen tnh ton cho robot almega 16 6 15-107
V Thu H - Trng i hc Kinh t K thut Cng nghip
3. S dng cc tiu ha tng on sai lch u ra trong min thi gian iu khin d bo h bung 12 16-084
sy giy a bin
Trn Kim Quyn1, Bi Quc Khnh2, Nguyn Don Phc2*
1
Trng Cao ng Cng nghip Tuy Ha
2
Trng i hc Bch khoa H Ni
4. iu khin phn hi v tr b kch hot tnh tin ng dng cho vi bm kiu xi lanh 20 16-140
Nguyn Anh Tun, Phm Hng Phc* - Trng i hc Bch khoa H Ni
9. Numerical Investigation of Solidification around a Circular Cylinder with the Presence of the Free 47 16-119
Surface in a Rectangular Cavity
Vu Van Truong*, Truong Viet Anh - Hanoi University of Science and Technology
10. Nghin cu kho st kh nng phn tch ph liu da thuc ca sn xut giy thnh vt liu c cu 52 16-135
trc dng x
on Anh V 1*, Dng Th Hon 1,2
1
Trng i hc Bch khoa H Ni
2
Trng i hc Cng nghip Dt May H Ni
11. Effects of Milling Time on the Properties of In-Situ Binary Niobium-Titanium-Carbide Reinforced 58
Cu Based Composite
Le Minh Hai, Tran Duc Huy - Hanoi University of Science and Technology
13. Tnh cht nhy kh H2S ca cm bin mng mng SnO2/NiO 68 15-138
Nguyn Vn Ton, Nguyn Vn Duy, Nguyn Vn Hiu*
- Trng i hc Bch khoa H Ni
14. Tng hp ng nano ccbon bng phng php CVD nhit: nh hng ca kim loi xc tc 72 16-131
Nguyn Cng T*, Nguyn Hu Lm - Trng i hc Bch khoa H Ni
16. S dng graphene a lp lm cht mang xc tc trong phn ng hydro ha cinnamaldehyde nhm 16-075
thu c hydrocinnamaldehyde vi chn lc cao
Trng Hu Tr - Trng i hc Bch khoa - i hc Nng
Tp ch Khoa hc v Cng ngh 116 (2017) 001-005
Tm tt
Kt hp INS/GPS l gii php hiu qu trong bi ton dn ng kt hp a cm bin. Bi v GPS v INS
c th b sung cho nhau t kt qu ti u da trn nhng u, nhc im ca chng. Trong bi ton
kt hp thng tin t cc h thng c lp, h kt hp s t chnh xc v tin cy tt hn trn c s thng
tin cung cp bi tng h l ng n. Bi bo ny tp trung trnh by xy dng h kt hp INS/GPS theo
cu trc ghp lng s dng b lc Kalman trn c s h INS c tc gi ci thin qua nng cao
chnh xc IMU v chnh xc xc nh gc nh hng ca vt th. Kt qu th nghim trn i tng
chuyn ng mt t cho thy h ghp lng INS/GPS xut c cht lng, chnh xc v tnh ng dng
cao hn so vi h ghp lng INS/GPS truyn thng.
T kha: H dn ng qun tnh, H thng nh v v tinh ton cu, cu trc ghp lng, b lc Kalman,
khi o lng qun tnh
Abstract
The INS/GPS integration is an effective solution in multi-sensors navigation. This is because, GPS receiver
and INS sensors can complement each other to achieve optimal results based on the advantages and
disadvantages of them. In an information integration system from independent systems, the integration
system achieve accuracy and better reliability based on information provided by each system is correct. This
paper focuses on presentation of a loosely coupled integration INS/GPS using Kalman filter based on INS
system has been improved the accuracy of IMU, objects orientation. Testing results on land vehicle are
shown the quality, accuracy and applicability of the proposed loosely coupled integration INS/GPS higher
than tradition loosely coupled integration INS / GPS.
Keywords: Inertial Navigation System, Global Positioning System, Loosely Coupled, Kalman Filter, Inertial
Measurement Unit
1
Tp ch Khoa hc v Cng ngh 116 (2017) 001-005
chinh xac c cai thi n ro r t so vi h ghp lng T nguyn ly hoa t ng cua h INS m ta trn
INS/GPS s du ng h INS truy n th ng. hinh 1, c th thy cht lng ca h INS ph thuc
trc tip vo chnh xc ca khi o lng qun
2. Ci thin chinh xac h INS
tnh (IMU). V vy, vic quan trng cn thc hin
Nguyn l xc nh v tr vt th ca h INS trc khi a IMU vo s dng l hiu chun (xc
kiu strapdown truy n th ng trong h e-frame c nh, loi tr hoc gim thiu nh hng ca cc sai
thc hin theo s Hnh 1. s). Cng vic ny u c cc nh sn xut IMU
thc hin trc khi xut xng, cc gi tr sai s c
Initial Attitude
ghi r trong ti liu k thut. Tuy nhin do mi
trng lm vic thc t khc vi iu kin th
Gyroscope
Gyroscope Attitude
nghim ca cc nh sn xut, cng vi nhiu nguyn
Signal
Initial
Initial Velocity Position
nhn khc, m bo yu cu s dng thc t cn
Project
thit phi thc hin li qu trnh hiu chun ny. Do
Accelerometer Accelerations Correct for Moving
Accelerometer Velocity Position
IMU phi hot ng trong nhiu iu kin mi trng
Signal onto Global Gravity Acceleration
Axes
vn m bo chnh xc.
Trong :
Do cm bin gia tc s dng trong h INS l
r e : vector v tr vt th xt trong h e-frame cm bin 3 chiu, thng tin o c t cm bin bao
v e : vector vn tc vt th xt trong h e-frame gm gia tc trng trng v gia tc chuyn ng.
Cbe : ma trn chuyn h ta t h b-frame sang Trong trng hp ng yn, thng tin o c ca
cm bin chnh l gi tr gia tc trng trng ti v tr
h e-frame
t. M gi tr gia tc trng trng ti mt v tr c
f b : vector gia tc o c bi cm bin gia tc coi l khng i (thay i v cng nh theo thi
gn trn vt th gian), v vy hon ton c th dng gi tr ny lm
iee : ma trn m t cc thnh phn vn tc gc chun hiu chun cm bin gia tc. Trong [2] tc
gi trnh by phng php mi dng gi tr gia tc
ca h e-frame quay quanh h i-frame
trng trng ti v tr t cm bin lm chun (khng
0 iee 0 cn thm chun, phng tin o tham chiu bn ngoi
m vn m bo chnh xc, tin cy) cho php xc
ie iee
e
0 0 ;iee 7,2921159.105 (rad / s)
0 nh chnh xc sai s h thng (sai s t l v sai s
0 0 bias) ca cm bin gia tc bng vic c lng ln
lt cc sai s s dng phng php bnh phng cc
g e : vector gia tc trng trng xt trong h e-
tiu. Tng t, do t trng Tri t ti mt v tr c
frame thay i rt nh theo thi gian, nn gi tr t trng
eeb : ma trn m t cc thnh vn tc gc ca vt Tri t ti v tr t cm bin cng c s dng lm
th xt trong h b-frame vi e-frame chun hiu chun cm bin t trng trong h INS
theo phng php trnh by trong [2]. Vi cm bin
0 zeb
b
yeb
b
vn tc gc, sai s bias c xc nh bng vic tin
b b hnh thu thp kt qu o trng thi ng yn, sau
eb zeb
b
0 xeb
ly gi tr trung bnh cng loi tr. Bn cnh
yeb
b
xeb
b
0
, t vic c th xc nh chnh xc s nh hng
ca cm bin vn tc gc trong khng gian t kt qu
ebb ibb ieb ibb Cebiee o ca cm bin gia tc v cm bin t trng trng
thi ng yn, hon ton xc nh c gi tr sai s
ibb : vector vn tc gc o bi cm bin vn tc t l ca cm bin vn tc gc da trn so snh gc
gc gn trn vt th quay ca cm bin xc nh t kt qu o ca cm
2
Tp ch Khoa hc v Cng ngh 116 (2017) 001-005
3
Tp ch Khoa hc v Cng ngh 116 (2017) 001-005
Thng s k thut
4
Tp ch Khoa hc v Cng ngh 116 (2017) 001-005
5
Tp ch Khoa hc v Cng ngh 116 (2017) 006-011
V Thu H
Trng i hc Kinh t K thut Cng nghip, 456 Minh Khai, Hai B Trng, Ha ni, Vit Nam
n Ta son: 19-8-2015; chp nhn ng: 20-12-2016
Tm tt
Bi bo cp n vn xy dng thut ton iu khin s dng mng nron da theo m hnh mmen
tnh ton cho Robot Almega 16. Khi khng bit chnh xc cc thng s ng lc hc ca Robot Almega 16,
lut s dng mng nron da theo m hnh mmen tnh ton gii quyt vn ny bng vic c lng
cc thng s v b nhiu da theo m hnh mu. Kt qu m phng trn phn mm Matlab-Simulink cho
thy h iu khin chuyn ng Robot Almega 16 p ng c yu cu iu khin: m bo sai s ca
cc khp quay nhanh chng t ti khng v thi gian qu nh.
T kha: Robot Almega 16, iu khin mment tnh ton, iu khin mng nron
Abstract
This paper presents a problem of building up a control algorithm for the Robot Almega 16 using neural
network based on computed torque method. To control the Robot Almega 16, the problems with unknown
kinematic and dynamic parameters is solved by implementing neural network based on computed torque
method to estimate the parameters and compensation the disturbances from the sample model. The
simulation results in the control requirements: steady-state errors of robot joint angles quickly converge to
zero and transient time is short.
Keywords: Robot Almega 16, Computed torque control, Neural network control.
7
Tp ch Khoa hc v Cng ngh 116 (2017) 006-011
u ra l ma trn k c kch c 1 x 3. Vy hm lp ra
D (q)(U b ) h(q, q) (7) l hm tuyn tnh, [4]:
f ( x) x (11)
T (5) v (7), xc nh c:
T thit lp c cng thc tnh u ra k theo
E K E K E D 1 D(q)q h(q, q) b
D P
(8) u vo v cc ma trn thnh phn theo :
tha mn (6), b cn xc nh: n
H 2 1
wik bk
2 (12)
Trong :
nH - n s mng n ron lp n;
nI - s u vo mng n ron;
- phn t thuc ct th k ca ma trn k ;
k
wij1 - phn t thuc hng i ct j ca ma trn w1 ;
Hnh 4. Cu trc mng nron hai lp
wik2 - phn t thuc hng i ct k ca ma trn w 2 ;
2.2. Thit k mng nron Robot Almega16 X i - phn t thuc ct th i ca ma trn X;
8
Tp ch Khoa hc v Cng ngh 116 (2017) 006-011
phng php trung bnh bnh phng sai lch. Hm Cng thc tnh u ra sau lp ra ca mng nron:
thng s ca mng c xc nh theo biu thc n
H
(15),[4-6]: y y j 2 b2 (26)
k j 1 jk k
1
J T (15)
Trong : y , y
2
j k l phn t ct j,k ca vc t u ra
Thc hin tnh o hm ca J theo cc trng s ca
mng xc nh c, [4],[5]: ca lp u.
3. ng dng iu khin s dng mng nrron da
J vT
. . (16) theo m hnh mmen tnh ton cho 3 khp u
w w robot Almega16
v
T (8) cho thy mi quan h gia v nh M hnh ng hc ca Robot Almega 16
w w
c tnh ton theo [2]. Chng trnh m phng
sau : mng nron ti ph lc [7]. M phng Robot Almge
v 16 vi cc thng s sau: Khi lng khp 1 : m1 =
b (17)
w w 67 kg ; Khi lng khp 2 : m2 = 52 kg ; Khi lng
khp 3 : m3 = 16 kg .
T (16) v (17) thit lp c mi quan h gia o
hm ca J theo cc trng lng vi o hm ca u Tham s b iu khin v cc gi tr t, bng 3.1.
ra b vi cc trng lng :
9
Tp ch Khoa hc v Cng ngh 116 (2017) 006-011
K P =3000
1 q d1 q d2
KP
H s K P =3000
q1
q2
t l 2
K P = 3000
3
K D =250
1
KD
H s K D =250
vi phn 2
q d3
K D = 250
3 q3
K D1 20 K D 2 20 2.5
K P1 100 K P 2 100 2
Truc z (m)
1.5
0.5
K D 3 20 0
1.5
K P 3 100 1
2.5
2
0.5
1.5
0 1
Truc y (m) Truc x (m)
Hnh 6. Biu din p ng gia cc gc khp t Hnh 8. Biu din chuyn ng t gc khp t (qd)
(qd) v gc khp thc (qthc) n gc khp thc (qthc) trong khng gian 3 chiu
Nhn xt: Vi nhiu tc ng th h thng b Nhn xt: Cc gc khp thc (qt) ca ba khp
dao ng, khng n nh. T kt qu m phng trn u bm gc khp t (qd) vi sai lch gia cc gc
ta c th thy kh nng chng nhiu ca b iu khp t (qd) v gc khp thc (qt) nhanh chng tin
khin m hnh mmen tnh ton l cha tt. Tuy ti 0, h khng c dao ng. B iu khin mng
nhin m hnh iu khin da theo mng n ron c nrron da trn m hnh mmen tnh ton loi b
th khc phc c iu ny. c hon ton nhiu tc ng vo h thng.
Trng hp khng bit r cc thng s ng lc 4. Kt lun
hc ca h thng v c nhiu tc ng ng dng b
iu khin mng nrron da theo m hnh momen Qua l thuyt v kt qu m phng cho thy, h
tnh ton. thng iu khin Robot Almega 16 s dng mng
Nron da theo m hnh mment tnh ton khc
Vic xc nh c chnh xc thng s ng lc phc c hu ht cc nhc im ca cc b iu
hc ca h thng Robot ALmega16 l rt kh khn khin truyn thng, c kh nng thch nghi cao,
dn n cc thng s ng lc hc a vo b iu chng nhiu tt, n nh bn vng, c kh nng iu
khin l khng chnh xc. kim chng thut ton khin cc i tng c cng m hnh vi tham s
iu khin bi bo gi thit Robot ALmega16 c khc nhau, thm ch l bin thin. c kim chng
khi lng v chiu di cc thanh ni khng xc nh trn m hnh m phng ca h thng iu khin bng
c chnh xc cc thng s ny nn cc thng s Matlab-Simulink, kim nghim thnh cng cc vn
ng lc hc a vo b iu khin l cc gi tr c l thuyt. nh hng m rng l thit k m hnh
lng : m1 , m
2,m
3 , gi s cc thng s iu khin vn
10
Tp ch Khoa hc v Cng ngh 116 (2017) 006-011
[1]. Bi Quc Khnh, Nguyn Phm Thc Anh, V Thu [5]. Seul Jung; Neural network controllers for robot
H, Xy dng thut ton iu khin thch nghi Li- manipulators University of California (1991)
Slotine cho Robot IRB 2400, tp ch khoa hc cng [6]. Howard Demuth , Mark Beale, Martin Hagan; Neural
ngh cc trng i hc k thut, s 69, (2009). Network Toolbox 6 - The MathWorks, Inc (2008).
[ 2] . V Thu H, Lun n tin s: Trng H BKHN, [7]. Phm Tun Anh, n tt nghip: Trng H
2012 BKHN, 2009.
[3]. o Vn Hip: K thut Robot, NXB khoa hc v k
11
Tp ch Khoa hc v Cng ngh 116 (2017) 012-019
Tm tt
Bi bo xut mt phng php iu khin d bo cho h MIMO vi m hnh d bo l h phng trnh
sai phn trong min thi gian. Phng php iu khin d bo xut ny lm vic theo nguyn tc cc
tiu ha tng on sai lch u ra ca h trong min thi gian. B iu khin ny c cu trc tng t nh
ca GPC truyn thng, ch thay i khu d bo tn hiu ra v khu ti u ha tnh hm iu khin trc
tip trn min thi gian thay v trong min tn s, nh khng cn phi tm nghim phng trnh
Diophaltine m vn m bo c cht lng iu khin bm gi tr t trc. Hn th na, b iu khin
xut ny cn c tnh tch knh v khng nhiu cao hn b iu khin GPC truyn thng. minh chng
cho kt lun ny, bi bo cng trnh by mt ng dng ca b iu khin xut vo iu khin a bin
bung sy giy, sau so snh cht lng iu khin thu c vi cht lng ca h khi c iu khin
bng iu khin phn hi u ra kt hp vi b iu khin truyn thng tch knh, cng nh cht lng
ca h khi c iu khin vi b iu khin GPC truyn thng.
T kha: m, Ti u ha tng on, Bung sy, MPC, Min thi gian
Abstract
The paper proposes a model predictive control method for MIMO system, in which the difference system
equations are used for output prediction. The proposed control method is based on piecewise minimizing of
output tracking errors in time domain. The structure of proposed controller is similar to that of conventional
GPC, except that its system output prediction and minimization of tracking error will be carried out directly in
time domain instead of frequency domain. Hence the solution of Diophaltine equation can be avoided but
the tracking control performance to a desired value is still guaranteed. Moreover, the decoupling and
disturbance attenuation behavior of proposed controller is much better than conventional GPC. To
demonstrate these assertions, the paper presents also an application of proposed method to control the
multivariable paper drying system and then compares the resulted system control performance with which
obtained by using the output feedback control system in combination with the feedforward controller for
system decoupling, and also with which obtained by using conventional GPC.
Keywords: Moisture, Piecewise optimization, Drying section, MPC, Time domain
Ws 700kg / h
Ps 3.5Bar Air
TC TC
LC
Td ,
TT
Wa1 23447kg / h
1100 C Wa 2 33445kg / h
Ttb 750 C
kt 0.15kg / kg
T 1100 C
u 0 . 001 kg / kg
LT
26 28 30 32 34 600 m/pht
Tp , nh lng 50 g / m 2
13
Tp ch Khoa hc v Cng ngh 116 (2017) 012-019
dng m hnh hm truyn khng lin tc ca qu Xt h hai vo, hai ra, c tr vi m hnh tng
trnh (i tng iu khin). Phng php GPC p qut trong min thi gian:
dng c cho nhng i tng, qu trnh khng n
nh [8]. Hn th na n cng cn c th p dng y1[k ] a11 y1[k 1] a1n1 y1[ k n1 ]
c cho c nhng qu trnh c tnh pha khng cc b10u1[k m11 ] b11u1[k m11 1]
tiu [8], v cho ti nay n c bit l phng php
iu khin d bo ph thng v p dng nhiu nht b1q11 u1[ k m11 q11 ]
trong thc t, c th pht trin m rng cho h MIMO c10 u2 [k m12 ] c11u2 [k m12 1]
[8].
Do phng php GPC c xy dng trn nn
c1q12 u2 [ k m12 q12 ]
(1)
m hnh hm truyn khng lin tc, c cc tham s y2 [k ] a21 y2 [k 1] a2 n2 y2 [ k n2 ]
rt d c xc nh bng nhng thut ton nhn
dng, nn GPC hon ton c th c pht trin
b20u1[k m21 ] b21u1[k m21 1]
thnh b iu khin vng kn mang tnh thch nghi b2 q21 u1[ k m21 q21 ]
nu nh ta b sung thm khu nhn dng trc tuyn
cc tham s hai a thc ny. c20 u2 [k m22 ] c21u2 [k m22 1]
14
Tp ch Khoa hc v Cng ngh 116 (2017) 012-019
T y ta c cc u ra d bo ca h l B0,2 B0,1
y[k i], i 0,1, , N 1 , vi N max(n, q) , nh B1,2 B1,1
sau: B2,2 B2,1 A1,1 B0,0
Khi i 0 th:
A1,0 y[k 1] A2,0 y[k 2] (5) Bq 2,2 A1,1 Bq ,0 (7)
A1,1 A2,0 A1,0 A1,0
Khi i 1 th:
A2,1 A3,0 A1,0 A2,0
y[k 1] B0,0 u[k 1] Bq ,0 u[k q 1]
A1,0 y[k ] A2,0 y[k 1]
An,0 y[k n 1] An 1,1 An ,0 A1,0 An 1,0
B0,0 u[k 1] Bq ,0 u[k q 1] An ,1 A1,0 An ,0
A1,0 B0,0 u[k ] Bq ,0 u[k q ] Tng qut cho tt c cc ch s i 3, 4, , N 1
cn li, ta c:
A1,0 y[k 1] A2,0 y[k 2] An ,0 y[k n]
y[k i ] B u[k i ]
0,i Bq i ,i u[k q ]
A2,0 y[k 1] An,0 y[k n 1] (8)
hay:
A1,i y[k 1] A2,i y[k 2] An,i y[k n]
15
Tp ch Khoa hc v Cng ngh 116 (2017) 012-019
v: v
B0, N
v l k hiu ca ma trn c tt c cc phn t u u
T
B Q B
T
1 k 1
Rk u 2(w g )T Qk B1 u
bng 0. Vi cc k hiu ny, cc phng trnh (5)-(8) (g w ) Qk (g w )
T
16
Tp ch Khoa hc v Cng ngh 116 (2017) 012-019
khi p dng phng php Newton-Raphson, ta c 7. Xc nh vector g theo (12) v w theo (14).
nghim ti u ca n nh sau:
8. Tnh u theo (16) v u[k ] theo (17) ri a vo
u B1T Qk B1 Rk B1T Qk w g
1
(16) iu khin i tng.
Nu vit ra mt cch chi tit nghim ti u u 9. o tn hiu ra y y1 , y2 ca h ri sp xp li
T
tm c trn thnh: / /
hai mng d liu u , y nh sau:
u col u[k N ], u[k N 1], , u[k ]
ui/ : ui/ 2 , i 2q, 2q 1, ,3
ta s thy lun ly ra c t tn hiu iu khin
hin ti: u1/ : u1[k p ] v u2/ : u2 [k q ]
u1[k m1 ] y /j : y /j 2 , j 2n, 2n 1,
u[k ] , , , I 2 u ,3 v
(17)
u2 [k m2 ]
y1/ : y1 , y2/ : y2 .
iu khin i tng, trong I 2 l ma trn n
v kiu 2 2 . Tt nhin ta lun ly ra c c nhng 10. Gn k : k 1 v quay v 6.
gi tr tn hiu vt trc: 2.2. p dng vo iu khin bung sy giy
u1[k p ] M hnh bung sy giy c xy dng theo ti
vi m1 p N , m2 q N
u2 [ k q ] liu [4] cho nh my giy Bi bng c cu trc ma
trn hm truyn nh m t hnh 2 gm bn hm
t u theo cng thc: truyn nh sau:
u1[k p ] 0.000815 14 s
G11 e ,
C(2 N 1 2 m1 2 p ),(2 N 2 2 m2 2 q ) u P *
48s 1
u2 [ k q ]
0.0007945 28 s
G12 e
trong C( i ),( j ) l ma trn 2 hng, 2( N 1) ct c hai Wa 2 *
68s 1
phn t (1, i ) v (2, j ) bng 1, cc phn t cn li Td 0.334 50 s
G21 e
ng nht bng 0. P* 210 s 1
Tng kt li th b iu khin ti u ha tng Td 0.2671 45 s
G22 e
on iu khin bm gi tr t trc cho h a Wa 2 *
202 s 1
bin s lm vic theo cc bc sau:
1
1. Chn rng N max(n, q) cho ca s d bo `
v xy dng cc ma trn: S P P *
GD1
`
Gc1 ` G11 `
A1,0 , , An ,0 , B0,0 , , Bq ,0
/ /
u c 2q phn t v y c 2n phn t nh
ngha theo (13) vi th t nh sau:
Hnh 2. M hnh bung sy giy
u u1/ , u2/ , , u2/ q , y y1/ , y2/ , , y2/ n
/ /
Chn chu k trch mu T 5s v khi k hiu li
cc u vo ra:
5. Gn u 0, y 0 v k 0 .
/ /
y1 , y2 Td , u1 P* , u2 Wa 2*
6. Chn Qk , Rk i xng xc nh dng .
17
Tp ch Khoa hc v Cng ngh 116 (2017) 012-019
th h phng trnh sai phn ca n dng (4) s c cc nhit u vo tng ln, tc l chnh p P tng, lu
tham s ln lt l n 2, q 9 v: lng hi vo nhiu hn tng nhit sy, ko m
giy u ra bm theo gi tr t. Mch vng nhit
a11 1,8302, a12 0,8372 im sng tc ng tc l Wa 2 tng, lm gim nhit
a21 1,9521, a22 0,9527 im sng. Kt qu m phng ny cho thy h
b10 1, 68.105 , b11 1,561.105 , hot ng n nh p ng tt vi nhiu m u
vo, m cht lng giy u ra.
b12 0,382.105 , b13 3,549.106 ,
2.3. So snh kt qu khi iu khin vi b iu
b14 b15 b16 b17 b18 b19 0,
khin GPC truyn thng
b20 b21 b22 b23 b24 b25 b26 b27 0,
Kt qu m phng bung sy giy dng b iu
b28 0, 007858, b29 7, 666 khin MPC trong Toolbox Matlab Simulink, c tn
gi l b iu khin GPC cho hnh 5 v hnh 6.
c10 2,303.105 , c11 3,33.105 ,
T kt qu m phng ny v khi so snh vi cc
c12 2, 07.105 , c13 3.105 ,
hnh 3 v hnh 4 ta thy nu tc ng nhiu u vo
c14 c15 c16 c17 c18 c19 0 gama1, m ca giy tng ln ng thi gy nh
c20 c21 c22 c23 c24 c25 c26 c29 0, hng n mch vng nhit im sng. Di tc
ng ca b iu khin MPC trong toolbox Matlab
c27 0, 00653, c28 6,3765.103 Simulink iu khin m ca giy v gi tr t
p dng thut ton iu khin ti u tng on nhng thi gian iu chnh ln (ln n 104 s ), iu
trnh by trn iu khin h bung sy giy, ny chng t b iu khin mc nh hot ng cha
ta thu c kt qu nh m t hnh 3 v hnh 4. tt nh hng n cht lng sn phm giy.
18
Tp ch Khoa hc v Cng ngh 116 (2017) 012-019
19
Tp ch Khoa hc v Cng ngh 116 (2017) 020-025
Tm tt
Trong nghin cu ny, chng ti kho st, nh gi ng dng ca b kch hot tnh tin ECLIA cho vi bm
kiu xi lanh vi phng php iu khin phn hi v tr c v khng s dng tham s iu khin Kp. Thanh
trt vi bc dch chuyn nano mt tc ng vo pt tng c th y ra lng cht lng vi th tch rt nh
(pL). Kt qu cho thy, th tch cht lng c y ra u xi lanh t l thun vi dch chuyn ca thanh
trt/pt tng. Trong trng hp iu khin c tham s Kp th mc tuyn tnh ca th tch cht lng y
ra tt hn do khng c s dao ng v vt qu im ch xc lp ca pt tng. Kt qu ny hng ti cc
ng dng hiu qu ca ECLIA nh mt b kch hot trong cc h vi c in t (MEMS).
T kha: ECLIA, b kch hot tnh tin, iu khin phn hi v tr, vi c in t.
Abstract
In this study, we investigate a microsyringe pump application of a linear actuator using a position feedback
control with and without a tuning gain KP. The slider pushes the microsyringe directly in step motion with
nanometer resolution that repels a very small volume of liquid (pL). Experimental results show that the liquid
volume was direct propotion to the sliders stroke. The repeled liquid volume was better linear when using
the feedback control with the the tuning gain K P compared to that without KP; it was due to no overshoot and
no ossilation of the slider/piston. These results intent to a significant implementation in MEMS of the linear
actuator.
Keywords: ECLIA, linear actuator, position feedback control, MEMS
Hnh 1. ECLIA: (a) s cu to, (b) tit din ngang A-A, (c) tn hiu in p iu khin, v (d) th m t
chuyn ng ca PZT v thanh trt
21
Tp ch Khoa hc v Cng ngh 116 (2017) 020-025
22
Tp ch Khoa hc v Cng ngh 116 (2017) 020-025
Cc thanh trt ca b kch hot tnh tin thi gian iu khin v cho php chn tham s iu
ECLIA c truyn ng nh c cu kp tnh in. khin nh. Bi ton iu khin phn hi ny c
C cu ny ph thuc vo lc ht tnh in v ma st trnh by trong nghin cu trc y ca chng ti
ca b mt tip xc gia thanh trt v in cc dn [13]. thy c s nh hng tch cc ca tham
ng/gi. N c th gy ra s trt tng i ca s iu khin KP chng ti so snh vi iu khin
thanh trt trong qu trnh truyn ng v kp gi. dng tn s khng i f = 100 Hz. Khi tn s khng
iu ny dn n di cc bc dch chuyn ca i th vn tc ca thanh trt cng khng thay i
thanh trt khng u nhau. Do vy khng th dng khi tip cn ti v tr mong mun. Mt khc vi tn
vic m cc bc tnh chuyn v c. Trong s cao th dn n s dao ng v kh dng chnh
nghin cu ny chng ti s p dng iu khin phn xc ti v tr thit t ca thanh trt. Hnh 5 so snh
hi v tr nhm dn ng thanh trt n v tr chnh p ng ca iu khin phn hi vi tn s in p
xc, ng dng y ng lng dung dch mong mun khng i 100 Hz v c dng cc tham s iu
ca vi bm xi lanh. khin khc nhau, KP = 5 v 10. Kt qu cho thy c
hin tng dao ng v vt qu im thit t ca
Hnh 4 m t s khi ca h thng iu thanh trt khi tn s in p khng i (100 Hz).
khin phn hi. Trong cu hnh ny, khi iu khin Hin tng ny khng cn na vi iu khin c
tnh ton v xut tn hiu iu khin cho ECLIA. tham s KP. iu ny ph hp vi nhng phn tch
Cm bin v tr xc nh v tr thc ca thanh trt Vr. v nhn nh cp trn. Vi kt qu ny chng
Sai s Err l sai khc gia gi tr thc Vr v gi tr ti hng n ng dng ca b kch hot tnh tin
thit t Vd. Gi tr sai s ny c dng tnh ton dng iu khin phn hi c tham s KP cho vi bm
v xut tn hiu iu khin u vo U(t) cho h thng xi lanh trong phn tip theo.
nhm t ti v tr mong mun ca thanh trt.
Phng thc iu khin y l dng tn hiu phn 4. Thit lp th nghim v nh gi kt qu
hi tnh ton in p vi tn s thay i. Nu sai
Vi c im ca b kch hot tnh tin nh
s ln th tn s iu khin cao, thanh trt chuyn
trnh by cc phn trn. Chuyn ng tnh tin ca
ng nhanh tin v v tr thit t. Khi sai s gim,
thanh trt theo tng bc nh nm, hnh trnh ln
tn s in p c pht ra cng gim dn, iu ny
mm cng vi lc y c mN. V vy trong nghin
lm cho thanh trt tip cn v tr thit t mt cch
cu ny chng ti ng dng b kch hot tnh tin vi
n nh v chnh xc. Vi cch thc iu khin ny
iu khin phn hi v tr y pt tng cho vi bm
b kch hot s gim c thi gian iu khin cng
kiu xi lanh. Vi chuyn ng tng bc nh c nm
nh s dao ng v vt qu v tr xc lp ca thanh
ca pt tng cho php y lng dung dch c pL.
trt. Tham s iu khin ph thuc vo bc di
iu ny rt hu ch trong cc ng dng y t hoc
chuyn ca thanh trt v s trt ca c cu kp
cc phn ng ha hc.
tnh in. Bc chuyn ng cng ln th cng gim
23
Tp ch Khoa hc v Cng ngh 116 (2017) 020-025
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Tp ch Khoa hc v Cng ngh 116 (2017) 020-025
Li cm n
Nghin cu ny c ti tr bi Qu Pht trin khoa
hc v cng ngh Quc gia (NAFOSTED) trong
ti m s 107.01-2015.18.
25
Tp ch Khoa hc v Cng ngh 116 (2017) 026-030
Abstract
This paper proposed solutions for profiling the disc tool in machining a helical cylindrical surface with
constant pitch. A section method has been developed in AutoCAD environment together with a Boolean
operation. Especially, this work presented a computational problem of determining the any section of a
helical surface, while other documents only refer to the section along axis and cross section. The authors
used a combinative method of analytics, graphics and programming to solve that problem, applying in
designing cutting tool for machining helical cylindrical surfaces. The proposed method has been
implemented and verified through subroutines written in Visual C running in AutoCAD. The testing results
have confirmed that the proposed methods achieve high accuracy for variant profiles of helical surfaces in
short time conputation.
Keywords: Helicoids, Profiling, Disc tool
Tm tt
Bi bo xut nhiu gii php to bin dng c dng a gia cng mt xon vt c bc xon khng i.
Phng php mt ct cng phng php s dng ton t Boolean c trin khai trong mi trng
AutoCAD. c bit, cng trnh trnh by vn tnh ton xc nh tit din bt k ca mt xon vt trong
khi cc ti liu khc ch trnh by tit din dc trc v tit din ngang. Cc tc gi kt hp phng php
gii tch, ho v lp trnh gii quyt vn , ng dng vo thit k dng c gia cng mt xon vt.
Phng php xut c thc hin v kim tra thng qua nhng chng trnh con vit bng Visual C
chy trong AotoCAD. Nhng kt qu kim tra khng nh phng php xut t chnh xc cao cho
cc bin dng khc nhau ca mt xon vt trong thi gian ngn.
T kho: Xon vt, To hnh, Dng c dng a.
*
The generating process kinematics in the case of
Corresponding author: Tel.: (+84) 903463737 helical surface generation using a tool delimited by a
Email: long.banhtien@hust.edu.vn
26
Tp ch Khoa hc v Cng ngh 116 (2017) 026-030
27
Tp ch Khoa hc v Cng ngh 116 (2017) 026-030
28
Tp ch Khoa hc v Cng ngh 116 (2017) 026-030
29
Tp ch Khoa hc v Cng ngh 116 (2017) 026-030
30
Tp ch Khoa hc v Cng ngh 116 (2017) 031-036
Abstract
The most economic speed for the truck in transportation is from 60km/h to 150km/h. When the truck
operates at high speed, the air resistances acting on it increase significantly. In case of bad weather
operating conditions as strong wind, the aero dynamic forces acting on the truck cause safe situation. In this
paper, the authors present a study on aero dynamic performances of a 40 feet container truck and the
effects of 20 feet container which locates on truck at several positions to reduce its air resistances by using a
commercial Computation Fluid Dynamic (CFD). By using CFD, the pressure distribution, velocity distribution
around truck and air resistances acting on the truck are investigated. From analysis simulated results of aero
dynamic performances of the truck, the authors give some comments and propose ideas to reduce air
resistances acting on the truck. The study on reduction of resistances acting on truck contributes improving
economy efficiency of the truck transportation.
Keywords: Truck; air resistance; aero dynamic force; CFD; reduce air resistance.
Tm tt
Trong qu trnh vn ti hng ha chuyn tuyn ca on xe ch container, vn tc xe lu thng kh cao,
trong khong t 60 n 150 km/h. Khi on xe lu thng vi vn tc cao, lc cn gi tc ng ln thn v
on xe tng ln ng k. Trong trng hp iu kin thi tit xu, gi mnh, lc kh ng tc ng ln thn
v on xe c th gy mt an ton cho xe. Trong nghin cu ny, tc gi thc hin kho st cc c tnh
kh ng lc hc thn v on xe ch container 40 feet v nghin cu s nh hng ca v tr xp container
20 feet n c tnh kh ng hc on xe ch loi container c kch thc ny. Thng qua vic s dng
cng c m phng s, tnh ton ng lc hc cht lng CFD (Computation Fluid Dynamics), tc gi c th
tnh ton m phng s cc yu t phn b p sut, vn tc dng bao quanh thn v on xe v lc cn kh
ng tc dng ln thn v on xe. T kt qu ca vic phn tch cc yu t kh ng lc hc thn v xe,
tc gi a ra mt s nhn xt v xut gii php nhm gim lc cn gi tc ng ln on xe gp phn
nng cao hiu qu khai thc cho on xe ch container.
T kha: on xe ch container; lc cn gi; lc kh ng; CFD; gim lc cn gi.
32
Tp ch Khoa hc v Cng ngh 116 (2017) 031-036
33
Tp ch Khoa hc v Cng ngh 116 (2017) 031-036
Hnh 6. th h s lc cn kh ng theo vn tc
ca on xe
5. nh hng ca v tr xp container 20 feet n
c tnh kh ng lc on xe
Trong phn ny, vic nghin cu nh hng ca
v tr t container 20 feet n cc c tnh kh ng
lc on xe c thc hin da trn c s so snh,
phn tch cc kt qu m phng s on xe trong 3
trng hp b tr container 20 feet khc nhau khi vn
chuyn hng ca on xe. Hnh 7 th hin m hnh Hnh 8. Phn b p sut v vn tc dng bao quanh
tnh ton m phng 3 trng hp xp container trn xe ti mt ct dc tm, N1
xe vi cc v tr khc nhau tng ng N1, N2 v N3.
34
Tp ch Khoa hc v Cng ngh 116 (2017) 031-036
(1)
Trong : R l lc kh ng tc dng ln xe, N
V l vn tc chuyn ng, m/s
S l din tch mt hng gi, m2
Hnh 12 th hin kt qu so snh h s lc cn
kh ng trong cc trng hp xe ch container 40
feet v xe ch container 20 feet. Kt qu so snh chi
Hnh 9. Phn b p sut v vn tc dng bao quanh tit c th hin trong bng 3. T kt qu ny cho
xe ti mt ct dc tm, N2 thy, h s lc cn kh ng tc ng ln thn v
on xe xp x gi tr bng 1. Tuy nhin c s khc
bit r rt v cng sut tiu hao trong cc trng hp
xe ch theo container v xe khng ch theo container
nh th hin trn biu lc cn hnh 12 v bng so
snh cng sut Bng 3.
Bng 3. H s lc cn kh ng v cng sut tiu hao
cho thnh phn lc cn kh ng
Phng n ch
Cx Pw, CV %Pw
container
Khng ch
0.724 48.33 -52.9
container
20 feet 1.100 98.55 -3.9
40 feet 1.145 102.55 0.0
Hnh 10. Phn b p sut v vn tc dng bao quanh
xe ti mt ct dc tm, N3
Hnh 11. H s lc cn kh ng tc ng ln on xe
ti vn tc khai thc 80km/h Hnh 12. Lc cn kh ng tc ng ln xe
35
Tp ch Khoa hc v Cng ngh 116 (2017) 031-036
c bng thc nghim, tuy nhin tn km hn rt Bluff bodies aerodynamic and applications, Milano,
nhiu. Italy (2008), pp.1-14.
- Thng qua kt qu ca bi bo cho thy, khi xe lu [6] Ngo.V. H, Y. Ikeda. A Study on Interaction Effects
thng vi vn tc cao lc cn kh ng tng nhanh between Hull and Accommodation on Air Resistance
of a Ship. Proceeding of the JASNAOE, Hiroshima,
theo tc khai thc. Vic b tr xe chy khng ch Japan (2013), Vol.16, pp.278-281.
theo container v xe ch ch 1 container 20 feet vi
cc v tr t khc nhau c nh hng n lc cn kh [7] K. Mizutani, D. Arai, N.V. He, Y. Ikeda. A Study on
ng tc ng ln on xe. Ngoi vic nghin cu v Reduction of the Wind Resistance Acting on a Wood
v tr xp container c li nht v gim lc cn kh Chip Carrier. Proc. of the JASNAOE, Hiroshima,
Japan (2013), Vol.16, pp.282-285.
ng, cn thit phi nghin cu thm v nh hng
ca vic xp container n tnh an ton cho xe khi [8] K. Mizutani, Y. Akiyama, N.V. He, Y. Ikeda. Effects
quay vng, i hng xe c th c kt lun c th of cargo handling equipment on wind resistance
v vic p dng gii php k thut ny. Vn ny acting on a wood chip carrier. Proceeding of the
cn lin quan n cc quy nh v lut xp hng khi JASNAOE, Hiroshima, Japan (2014), Vol.18, ISSN:
2185-1840, pp.421-424.
lu thng xe trn ng. Vi hn ch v ni dng
nghin cu, trong bi bo ny tc gi cha thc hin [9] Ngo. V.H, K. Mizutani, Y. Ikeda. Reducing air
nghin cu ni dng ny. resistance acting on a ship by using interaction effects
between the hull and accommodation. Proceeding of
- Trn c s phn tch kt qu tnh m phng s CFD the 7th AUN/SEED-Net RCMME 2014, Hanoi,
nh phn b p sut v lc tc ng ln on xe Vienam, ISSN: 978-604-911-942-2, pp.497-501.
cho thy nguyn nhn lm tng hay gim lc cn kh
[10] Ngo. V.H, Phan. A.T, Luong. N.L, Y. Ikeda. A Study
ng tc ng ln thn xe. Cc kt qu nghin cu v on interaction Effects on air resistance acting on a
s nh hng ny s l c s ti u hnh dng kh ship by shape and location of the accommodation.
ng cho on xe c li nht v lc cn kh ng. Journal of Science and Technology, Vietnam (2015),
y chnh l c s gim tiu hao nhin liu cn Vol 27, ISSN:1859-3585, pp. 109-112.
thit cho on xe v nng cao hiu qu kinh t khai
[11] Ngo V. H, Mizutani. K, Ikeda. Y. Reducing air
thc on xe. resistance acting on a ship by using interaction effects
Ti liu tham kho between the hull and accommodation. Ocean
Engineering Journal (2015), Vol. 111, pp. 414-423.
[1] K. Salari. DOEs Effort to Improve Heavy Vehicle
Aerodynamics though Joint Experiments and [12] Ng Vn H, L Quang (2015). Nghin cu nh
Computations. DOE annual merit review, Lawrence hng ca hnh dng thn v n c tnh kh ng
Livermore National Laboratory (2013). on xe ch container. Tp ch giao thng vn ti
(2015), s 56, pp.194-196.
[2] European Federation for Transport and Enviroment
AISBL. The case for the exemption of aerodynamic [13] Trn S Phit, V Duy Quang. Thy kh ng lc hc
devices in future type approval legislation for heavy k thut (1979). NXB H v TH CN H Ni.
goods vehicles (2010), pp. 1-25. [14] Nguyn Phc Hong ( Ch bin), Phm c Nhun,
[3] H. Chowdhury, H. Moria, A. Ali, I. Khan, F. Alam, S. Nguyn Thc Tn. Thy lc v my thy lc. NXB
Watkins. A study on aerodynamic drag of a semi i hc v trung hc chuyn nghip, H ni 1979.
trailer truck. Journal of Procedia Engineering (2013), [15] ITTC (2008), The proc. of the 25th International
Vol.56, pp. 201-205. Towing Tank Conference, Fukuoka, Japan, Website:
[4] Ch. Hakansson, M.J. Lenngren. CFD analysis of http://ittc.sname.org/proc25/assets/documents/V
aerodynamic trailer devices for drag reduction of olumeI/Proceedings.
heavy duty trucks. Master thesis of Chalmers
University of technology, Sweden (2010). [16] ITTC (2011), The proc. of the 26th International
Towing Tank Conference, Rio de Janeiro, Brazil,
[5] GM.R. Gandert, V. Raemdonck, J.L. Michel, V. Website:
Tooren. Design of an aerodynamic aid for the http://ittc.sname.org/proc26/assets/documents/V
underbody of trainler within a tractor-trailer olumeI/Proceedings.
combination. BBAA VI International colloquium on
36
Tp ch Khoa hc v Cng ngh 116 (2017) 037-041
Nghin cu nh hng ca gc ln ci
n qu trnh dp thy tnh phi tm kim loi
Effect of the Die Conner Radius on the Sheet Metal Hydroforming Process
Tm tt
Nguyn cng dp vut c s dng rt nhiu trong qu trnh to hnh cc chi tit phc tp trong bao
gm c cng ngh dp vut truyn thng, dp vut thy c, dp vut thy tnh. Mi cng ngh c nhng u
im khc nhau v ng dng ph thuc vo vt liu, sn phm, iu kin sn xut ... Cng ngh dp thy
tnh c s dng cho nhng chi tit cn c bn knh gc ln chi tit nh m cc phng php khc kh
hoc khng th ch to. Mc tiu ca nghin cu ny l xc nh nh hng ca bn knh gc ln ci
trong qu trnh dp thy tnh chi tit tm n kh nng to hnh v thng s lc chn. Nghin cu c thc
hin vi thp ZAM dy 0,8 mm vi cc bn knh gc ln ci 2mm, 3mm, 4 mm, 5 mm v 6mm..
T kha: Dp thy tnh, Bin mng, Nhn, Rch
Abstract
Drawing is used a lot in the process of the intricate part shaping including traditional drawing, hydro-
mechanical deep drawing, and hydrostatic deep drawing. Each technology has different advantages and
applications that depend on the materials, products and production conditions... Hydrostatic deep drawing is
used for the products, required die shoulder and die radius little, that is difficult or impossible to fabricate by
other method. The objective of the present study is to determine the influence of work piece materials on die
shoulder radius in sheet hydrostatic forming process. The die shoulder radius plays a vital role in
manufacturing the product in deep drawing process to formability and holder force. The present work deals
with ZAM steel blank of 0,8 mm in thickness, and 2mm, 3mm, 4 mm, 5 mm and 6mm for corner radii of the
die.
Keywords: Hydrostatic Forming, Thinning, Wrinkle, Crack
*
Corresponding author: Tel.: (+84) 915021575 Hnh 1. S nghin cu
Email: kien.letrung@hust.edu.vn
37
Tp ch Khoa hc v Cng ngh 116 (2017) 037-041
Zn Al Mg
91% 6% 3%
Bng 2.Thnh phn ho hc thp cn nng SPHC(%)
C Mn P S
0.15 0.60 0.050 0.050 Hnh 4. Chi tit hnh thnh khi rc = 2mm, rct = 2mm.
Gii hn chy ca vy liu thp ZAM c c Khi bn knh gc ln ming ci rc = 2mm,
nh th nghim ko trn my MTS809. tt c cc trng hp vi cc di lc chn khc nhau
Axial/Torsional Test System: u gy nn rch phi, khng in y c.
38
Tp ch Khoa hc v Cng ngh 116 (2017) 037-041
39
Tp ch Khoa hc v Cng ngh 116 (2017) 037-041
40
Tp ch Khoa hc v Cng ngh 116 (2017) 037-041
- Mt l do khi bn knh rc tng ln lm kh [3] A.G. Mamalis, D.E. et al., On the finite element
nng ko phi vo trong ci r dng hn, cn bng modelling of the deep-drawing of square sections of
ng sut bt buc phi tng ng sut chn ln. coated steels, Journal of Materials Processing
Technology 58 (1996), 153159.
- Hai l s mt n nh ti bn knh gc ln
[4] Taylan Altan (2006), Processes for hydroforming
ca ci gy nhn ti phn vnh khi tng rc, khng sheet metal 1,Stamping Journal, (Feb 2006), 40-41
mt n nh th phi tng gi tr lc chn khi tng rc.
[5] R. Narayanaswamy et al., A comparative study of
2. Vi bn knh gc ln y chi nh (1mm), deep drawing with conventional, isostatic, and
s in y l rt kh (do t s S/D ti bn knh gc hydrostatic pressure, Journal of Mechanical Working
ln ln). Khi tng bn knh gc ln chi tit rct ln Technology, 6 (1982) 227-234
mt n v, gi tr lc chn y thay i khng
[6] S.A. Zahedi et al., Investigation of conventional deep
ng k. in y cc bn knh gc ln chi tit th drawing and hydroforming deep drawing via
cn tng p sut cht lng trong lng ci p0. experimental and finite element simulation, Indian
Journal of Science and Technology, Vol. 3 No. 9 (
Ti liu tham kho
2010), 1009-1013.
[1] J.P. Fan et al., 3D finite element simulation of deep
[7] M. Jurkovi, I. Mamuzi, E. Karabegovi. The sheet
drawing with damage development, International
metal forming with Hydraulic fruid pressure.
Journal of Machine Tools & Manufacture 46 (2006),
Metalurgija 43 (2004), 315-322
10351044
[8] Nisshin Steel Quality Products, ZAM.
[2] Marcelo Elguela, Ductile damage analysis of sheet
metal forming, Journal of Materials Processing [9] Pha m Vn Ngh . Cng ngh d p thuy tin h, NXB
Technology 121 (2002), 148 156. Bach Khoa Ha N i, 2006.
41
Tp ch Khoa hc v Cng ngh 116 (2017) 042-046
Cng ngh ch to in cc hn
cho dy chuyn hn bn t ng xch neo tu hi qun
Welding Electrode Manufacturing Technology
for Marine Anchor Chain Flash Butt Welding Machine
Tm tt
Bi bo ny tin hnh nghin cu thc nghim ch to cc in cc hn t brng BCuNi3Si ( 1-3) cho
dy chuyn hn tip xc bn t ng xch neo tu hi qun. Thng qua thc nghim cc ch nu luyn
v nhit luyn hp kim BCuNi3Si c xc nh. Nhit c c xc nh trong khong (1170 oC -
1200 oC). Nhit ng u ha thnh phn thi c khong 90010 oC vi thi gian gi nhit 4 h. Nhit
rn phi in cc hn (750-900) oC. Sau rn, phi c kt tinh li nhit 60010 oC trong 2 h.
Nhit luyn kt thc bao gm ti v ha gi, trong , nguyn cng ti c thc hin nhit 850 oC,
ha gi nhit 450 oC vi thi gian gi nhit 4 h. Khi cng ca hp kim t 240 HV5, gii hn bn
nh nht t 757,9 MPa, gii hn chy nh nht t 559,8 MPa, gin di tng i nh nht t 8,5 %,
dn in nh nht t 35,4 % IACS. Cc in cc hn u t cht lng tng ng in cc hn
nhp khu i km theo dy chuyn hn.
T kha: in cc hn, hp kim BCuNi3Si ( 1-3), c tnh, cng, dn in.
Abstract
In this paper, a study on manufacturing technology of welding electrodes from CuNi3Si alloy for marine
anchor chain flash butt welding machine was reported. Remelting regime and heat treatment are clearly
determined through experimental process. Casting temperature was established in the range of (1170-1200)
oC. After casting, the alloy was homogenized at temperature 90010 oC for 4 hours. Forging temperature for
casting blank was in the range of (750-900) oC. After forging, the electrode blank was recrystallization
annealed at 60010 oC for 2 hours. Finish heat treatments for electrode blank consisted of solution heat
treatment and aging. The solution treatment temperature was set at 850 oC. Optimum aging temperature
appeared to be 450 oC and time at this temperature was 4 hours long. Then alloy reached the hardness of
240 HV5, minimum tensile strength of 757.9 MPa, minimum yield strength of 549.8 MPa, elongation at
fracture of 8.5 % and minimum electrical conductivity of 35.4 % IACS. Welding electrodes had absolutely
equivalent quality in comparison with accompaniment standard ones of butt welding machine.
Keywords: welding electrode, CuNi3Si alloy, mechanical properties, hardness, electrical conductivity.
42
Tp ch Khoa hc v Cng ngh 116 (2017) 042-046
Zn Pb Sn Fe Ni Si Cr Al Ti Cu
0,10 0,01 0,01 0,05 3,07 1,00 0,01 0,03 0,02 95,7
Hnh 2. T chc t vi hp kim BCuNi3Si sau c
Qu trnh thc nghim bt u bng vic tnh
ton phi liu, nu luyn v c thi hp kim
BCuNi3Si trong l nu in tr Nabertherm (c).
Phi c sau khi ct u rt c ng u ha
thnh phn, sau tin hnh rn nng v kt tinh
li chun b t chc cho nghin cu xc nh ch
nhit luyn kt thc. Sau nhit luyn, tin hnh gia
cng c kh ch to hon chnh b in cc hn cho
thit b hn xch neo tu hi qun. Phng php
nghin cu ch yu gm o cng HV5 (c xc
nh trn my o cng Vickers Wilson Wolpert
Trung Quc), o dn in (c xc nh thng Hnh 3. T chc t vi hp kim BCuNi3Si sau ng
qua o in tr ca mu trn thit b Megger Digital nht
Microhmmeter DLRO-10 Anh Quc) v th ko
xc nh cc ch tiu c tnh (c tin hnh trn my Khun kim loi c chun b sn v sy
th ko nn vn nng 60T Trung Quc). trc t nhit (300-400) oC. Qu trnh rt phi rt
t t kim loi lng in y khun v b ngt kp
3. Kt qu v tho lun thi. Do h s co ngt ca hp kim kh ln nn cn
3.1. Nu luyn v c phi in cc hn rt vi tc chm nhng lin tc trnh khuyt
tt, giai on cui tc rt cng chm cng tt
Vt t nu luyn bao gm Cu nguyn cht mc m bo lng kim loi b ngt, trnh co ngt
M1 v cc hp kim trung gian CuSi10, CuNi15 c mnh to lm co ln dn n ph phm.
sch cao c nu luyn trc t ng nguyn cht
43
Tp ch Khoa hc v Cng ngh 116 (2017) 042-046
44
Tp ch Khoa hc v Cng ngh 116 (2017) 042-046
45
Tp ch Khoa hc v Cng ngh 116 (2017) 042-046
46
Tp ch Khoa hc v Cng ngh 116 (2017) 047-051
Abstract
This paper presents numerical simulation of solidification around a cooled circular cylinder with the presence
of a free surface in a rectangular cavity. The free surface is introduced to account for volume change due to
density difference between the solid and liquid phases during solidification. Pure tin with the solid-to-liquid
density ratio sl = 1.05 (shrinkage) is investigated as a phase change material. The front-tracking method
combined with an interpolation technique, in which the interface separating two phases is represented by
connected elements laid on a stationary grid, is used for solving the problem. The case of no volume change,
i.e., sl = 1.0, is also calculated and compared with the case of sl = 1.05 to see how volume shrinkage
affects the solidification process. The numerical results show that shrinkage reduces the solidification rate,
and thus results in a decrease in the form, i.e., the area, of the solid layer around the cylinder. In addition,
the liquid level decreases in time due to volume shrinkage upon solidification.
Keywords: Numerical simulation, Front-tracking, Solidification, Shrinkage, Circular cylinder
Tm tt
Bi bo gii thiu m phng s qu trnh ha rn xy ra xung quanh mt tr trn c lm lnh vi s hin
din ca mt thong trong mt khoang hnh ch nht. Mt thong c a vo b vo s thay i v
th tch do s khc nhau v khi lng ring gia pha lng v pha rn trong qu trnh ha rn. Thic
nguyn cht vi t s khi lng ring gia pha rn v pha lng sl = 1.05 (co th tch) c nghin cu nh
l mt vt liu chuyn pha. Phng php theo du bin kt hp vi k thut ni suy m bin phn cch
gia hai pha c biu din bi cc on thng lin kt, c s dng cho vic gii bi ton. Trng hp
khng c s thay i v tch vi sl = 1.0 cng c tnh ton v so snh vi sl = 1.05 thy c nh
hng ca s co th tch n qu trnh ha rn. Kt qu m phng cho thy, s co th tch lm gim tc
ha rn, v ko theo gim s hnh thnh ca min rn xung quanh tr. Thm vo , mc mt thong gim
dn theo thi gian do s co li v th thch trong qu trnh ha rn.
T kha: M phng s, Theo du bin, Ha rn, Co th tch, Tr trn
In the present study, we present numerical of the one-fluid representation, the momentum and
investigations for solidification around a cooled thermal energy equations are
cylinder with natural convection and with the
presence of the free surface. The method utilizes the u t uu p ( u uT )
front tracking technique [6] to represent the solid
liquid interface and an interpolation technique, i.e., an +f n f ( x x f )dS g T Tm (1)
f
immersed boundary method, to deal with the no-slip
and constant isothermal temperature boundary C pT t C pTu k T
conditions [4]. Pure tin with the solid phase denser
q x x f dS C p h
than the liquid phase, i.e., with volume shrinkage
(2)
upon solidification, is used as an investigated phase f
change material.
2. Numerical problem and method u 1 s 1 l x x f qdS Lh (3)
f
Fig. 1 shows the investigated problem, a Here, u is the velocity vector, p is the pressure, g is
solidification layer forming around a cooled circular the gravitational acceleration, and t is time. T and the
cylinder held at temperature Tc with a free surface in superscript T denote the temperature and the
a rectangular cavity. The diameter of the cylinder is transpose. D/Dt is the material derivative. f is the
denoted by d. The fusion temperature of the liquid (or momentum forcing term used to impose the no-slip
melt) is Tm greater than Tc. Initially, the gas and liquid condition on the solidliquid interface, and h is the
phases are at temperature T0 (T0 Tm). To save the energy forcing term used to impose a constant
computations, the half of the physical domain is temperature on the cylinder boundary [4]. The fourth
investigated as shown in term on the right-hand side of Eq. (1) accounts for the
Fig. 1a. The fluid and thermal properties of each interfacial tension force at the free surface [7]. The
phase are assumed constant, and the presence of the last term in Eq. (1) is the Boussinesq approximation
gas phase (i.e., free surface) is to account for volume for density changes due to thermal gradients [8],
change due to density difference between the solid and is the thermal expansion coefficient of the
and liquid phases during solidification. The fluids fluids. At the interfaces, denoted by f, is the
assumed incompressible are driven by buoyancy- interfacial tension acting on the liquidgas front. is
induced natural convection, i.e., Bussinesq twice the mean curvature, and nf is the normal vector
approximation. We treat all phases as one fluid with to the interface. The Dirac delta function (x xf) is
variable properties such as density , viscosity , zero everywhere except at the interfaces xf. q is the
thermal conductivity k and heat capacity Cp. In terms heat source at the solidification interface, given as
Fig. 1. Solidification around a cooled cylinder with the free surface in a rectangular cavity: (a) computational
domain; and (b) front-tracking representation for the solidification and free surface interfaces.
48
Tp ch Khoa hc v Cng ngh 116 (2017) 047-051
I x x f n f dS (6)
f
Fig. 2. Evolution of the solidification layer around the cooled cylinder with sl = 1.05. In each frame, the left
shows the velocity field normalized by Uc, and the right shows the isotherms plotted every = 0.1
49
Tp ch Khoa hc v Cng ngh 116 (2017) 047-051
As previously mentioned, in this study, we focus large, resulting in a high solidification rate, i.e., high
only on the effects of volume change (sl) and thus Vn , and high Nusselt number (Fig. 3). When the
other parameters are kept constant, i.e., Pr = 0.01, St temperature in the liquid phase decreases and reaches
= 0.02, Ra = 1104, We = 510-4, 0 = 1.42, gl = gl the fusion temperature m, the temperature gradient
= 0.05, ksl = 1.0, kgl = 0.005, Cpsl = Cpgl = 1.0, and gl
= 0.003. The values of these parameters correspond to drops down, and Vn and Nu decrease (Fig. 3).
pure tin with the cylinder diameter d of a few
centimetres. The computational domain is WH =
2d7d with a grid resolution of 64224. The cylinder
center is at x = 0, y = 2.5d, and the initial level of the
liquid is 5.5d. Method validations have been
extensively carried out in our previous works [4,7],
and thus are not presented in this paper.
4. Results and discussion
Fig. 2 shows the temporal evolution of the
solidifying and liquidgas fronts with the temperature
and velocity fields. The density ratio sl is set to 1.05.
This density ratio is for tin. At early times of the
solidification process, downward flow arises along
the solidliquid interface, at which the temperature is
m = 1.0, because the density of the liquid increases Fig. 3. Variations of the average solidifying velocity
with a decrease in the temperature. As shown in the and of the space-average Nusselt number at the
left frame ( = 0.6) of Fig. 2, the downward flow is solidification interface with respect to time ( sl =
strong with the cooled liquid accumulating at the 1.05).
bottom part of the cavity. As a result, a thermally
stratified region is formed. At later time = 4 (middle
frame of Fig. 2), the flow decreases and three
circulations with the strongest one at the bottom form.
These circulations are induced by buoyancy, i.e., the
last term in Eq. (1). As time progresses, the
temperature of the liquid phase decreases to near the
fusion temperature m. Consequently, the flow is
suppressed. At = 56 (right frame of Fig. 2), the
liquid temperature is uniform in the entire cavity, and
almost no flows are evident at this time, and the
solidification process is merely controlled by
conduction.
For tin, the solid is denser than the liquid, i.e.,
sl = 1.05, and this causes volume shrinkage during
solidification. Accordingly, looking at the level of the
liquid in the cavity, we can see that it decreases with
time as shown in Fig. 2.
Fig. 3 shows the temporal variations of the
average of the normal velocity of the solidifying
Fig. 4. Solidifying front and free surface location at
interface, and of the space-averaged Nusselt number,
= 60 for sl = 1.0 (left) and sl = 1.05 (right).
at the sodifying interface, defined as
Lf
To consider how volume change affects the
1 solidification process, we also perform simulation of
Nu
Lf
0
dl
n f
(9)
a case with no density difference, i.e., sl = 1.0, and
compare its results with those for sl = 1.05, as shown
where Lf is the length of the solidifying interface. in
During the initial stages of solidification, the
temperature gradient at the solidifying interface is
50
Tp ch Khoa hc v Cng ngh 116 (2017) 047-051
Fig. 4. We can see that at this time as sl solidication rate, and thus results in a decrease in the
decreases from 1.05 to 1.0 the solid layer forming form, i.e., the area, of the solid layer around the
around the cylinder is wider. This indicates that the cylinder. In addition, the liquid level decreases in
solidification rate decreases as sl increases. This is time due to volume shrinkage. The results for sl =
confirmed by Fig. 5, in which the area of the solid 1.2 are also presented.
phase increases with a decrease in sl from 1.2 to 1.0 Acknowledgments
(one more case of sl = 1.2 has been calculated to
show the effects of volume shrinkage). This is This research is funded by Vietnam National
understandable since there is flow induced by density Foundation for Science and Technology
difference between the solid and liquid, coming to the Development (NAFOSTED) under grant number
solid layer to compensate [7,10] for sl = 1.05 and 1.2 107.03-2014.21.
(volume shrinkage). This flow reduces the References
solidification rate. Accordingly, the solid layer
forming around the cylinder decreases for the case of [1] K. Sasaguchi, K. Kusano, R. Viskanta, A numerical
shrinkage. In addition, as prevously mentioned, the analysis of solid-liquid phase change heat transfer
around a single and two horizontal, vertically spaced
level of the liquid phases decreases with time for the
cylinders in a rectangular cavity, Int. J. Heat Mass
case of shrinkage while it does not change in the case Transfer. 40 (1997) 13431354.
of no volume change, i.e. staying at 5.5d, as shown in
Fig. 5. Fig.5 also indicates that increasing this density [2] M. Sugawara, H. Beer, Numerical analysis for
ratio results in a faster decrease in the liquid level. freezing/melting around vertically arranged four
cylinders, Heat Mass Transfer. 45 (2009) 12231231.
[3] Y.-C. Shih, H. Chou, Numerical study of solidification
around staggered cylinders in a fixed space, Numer.
Heat Tr. A-Appl. 48 (2005) 239260.
[4] T.V. Vu, A.V. Truong, N.T.B. Hoang, D.K. Tran,
Numerical investigations of solidification around a
circular cylinder under forced convection, J. Mech.
Sci. Technol. 30 (2016) 50195028.
[5] S. Sablani, S.P. Venkateshan, V.M.K. Sastri,
Numerical study of two-dimensional freezing in an
annulus, J. Thermophys. Heat Tr. 4 (1990) 398400.
[6] T.V. Vu, G. Tryggvason, S. Homma, J.C. Wells, H.
Takakura, A front-tracking method for three-phase
computations of solidification with volume change, J.
Chem. Eng. Jpn. 46 (2013) 726731.
[7] T.V. Vu, G. Tryggvason, S. Homma, J.C. Wells,
Fig. 5. Temporal variations of the level of the liquid Numerical investigations of drop solidification on a
phase and the area of the solid layer As around the cold plate in the presence of volume change, Int. J.
Multiphase Flow. 76 (2015) 7385.
cylinder for sl = 1.0, sl = 1.05, and sl = 1.2. Ac is
the area of the cylinder. [8] H. Gan, J. Chang, J.J. Feng, H.H. Hu, Direct
numerical simulation of the sedimentation of solid
5. Conclusion particles with thermal convection, J. Fluid Mech. 481
(2003) 385411.
We have presented the numerical results of
solidification around a cooled cylinder in a cavity [9] F.H. Harlow, J.E. Welch, Numerical calculation of
with the presence of volume shrinkage. To account time-dependent viscous incompressible flow of fluid
for volume change during solidification, a gas phase with free surface, Phys. Fluids. 8 (1965) 21822189.
was introduced at the top of the domain. Tin with sl [10] V.V. Truong, Direct numerical simulation of
= 1.05 was considered as a phase change material. solidification with effects of density difference,
The case of no volume change, i.e., sl = 1.0, was also Vietnam Journal of Mechanics. 38 (2016) 193204.
calculated and compared with the case of volume
change to demonstrate the effect of volume change on
the solidication process. The front-tracking method
combined with the interpolation technique [4] was
used for solving the problem. The numerical results
show that the presence of shrinkage reduces the
51
Tp ch Khoa hc v Cng ngh 116 (2017) 052-057
Tm tt
Bi bo nghin cu kh nng phn tch ph liu da thuc dng mnh hnh thnh trong qu trnh sn xut
giy da thnh cc dng vt cht c cu trc x bng cc phng php khc nhau. Loi ph liu c la
chn nghin cu l da b ct v da b vng c s dng rng ri trong sn xut giy ti Vit Nam. Cc
cng ngh phn tch p dng l: nghin x kh trc tip bng phng php c hc s dng my nghin
ba v nghin x t c tin x l bng NaOH v H2SO4 trong cc iu kin nng v thi gian khc
nhau. Kt qu nghin cu thu c cho thy c hai loi da nu trn u c kh nng phn tch thnh cc
dng vt cht dng x bng c hai phng php nghin kh v nghin t. Phng php nghin x t s
dng tin x l bng H2SO4 c kh nng to thnh x vi ng knh nh hn 100 m v chiu di ti vi
cm. Trong khi , tin x l bng NaOH ch ph hp vi da vng v ch nn c s dng nng thp
v thi gian x l ngn. Phng php nghin x trc tip bng my nghin ba c tc nghin nhanh, x
thu c c ng knh nh (nh hn 0.1mm) v ng u nhng chiu di ngn hn so vi phng php
s dng H2SO4. Cc kt qu thu c l c s quan trng la chn phng php nghin ph hp nhm
a cc ph liu da thuc dng mnh thnh dng x ng dng trong vic ch to cc loi vt liu ti
ch.
T kha: X da, Nghin x da thuc, Da thuc ph liu
Abstract
In this research, methods for dissociation of leather fibres from scrap leather pieces of shoe manufacturing
are studied. The types of scrap used are grain and corium cow leathers which are materials for common
shoe making in Vietnam. Dissociation techniques used include: (1) dry crushing by mechanical methods
using a hammer mill and (2) chemical pretreatment - assisted wet milling using NaOH and H2SO4 at various
concentrations and retention time. Experimental results showed that both types are able to dissociate into
fiber form materials by the wet and dry grinding methods. Wet grinding method using the pretreatment in
H2SO4 is capable of forming fibers with less than 100 micron in diameter and up to several centimeters in
length. Meanwhile, pretreatment with NaOH is only suitabe with curium leather and should only be used in
low concentrations and short processing time. Grinding directly by hammer mill is fast and helped obtained
fibres with small diameter (less than 0,1mm) but the length is shorter than those obtained from the H 2SO4
method. These results are important for choosing the suitable crushing method in order to transform scrap
leather into fiber form to be used for recycle materials production.
Keywords: Leather fiber, Leather grinding, Scrap leather
hnh phn r da thuc crom theo nhiu giai on khc v Cng ty Giy Thy Khu. Cc ha cht c bn
nhau thu c cc bo da v ht da mi lm c s dng lm tc nhn tin x l da trc khi
nguyn liu ch to cc vt liu polime compozit c nghin l NaOH v H2SO4 c xut x Trung Quc.
kh nng phn hy sinh hc.
2.2 Ni dung nghin cu v qui trnh thc nghim
Santana v Moreno [5] tin hnh nghin x
2.1.1 Nghin x da theo phng php t:
ph liu da nappa ca qu trnh sn xut giy bng
my nghin ba c kch thc mt sng l 1,5 mm Trc tin cc mu da ph liu c s loi v
thnh cc x da. Cc x da thu c tip tc c s ct ng u ha s b v kch thc sau c
dng ch to vt liu lai ha. tin hnh ngm trong mi trng ha cht cc iu
kin nng v thi gian khc nhau. Mi trng tin
Trong mt nghin cu khc, Madera Santana v
x l trc khi nghin s dng l axit (H2SO4) v
cng s [5], tin hnh nghin da thuc crom thnh
kim (NaOH). Thit b nghin c s dng l thit
cc b vi x v dng lm cht n ch to cc chi
b hot ng theo nguyn l dao ct.
tit giy ti ch.
Tin x l c thc hin dung t 1:50 trong
Nhm nghin cu ca Nahar thuc i hc
iu kin nhit thng. Thi gian lu ca mu
Malaya, Malaysia [6] tin hnh ti ch cc loi da
c thc hin 3 mc khc nhau l 2h, 3h v 4h.
thuc bng cc cht thuc khc nhau bng cch
Vi mi ha cht tin x l tin hnh vi 3 nng
phi trn chng vi polyeste. Trc khi phi trn, cc
khc nhau c th l: NaOH (20 g/l, 30 g/l, 40 g/l);
da thuc ph liu c nghin hai ln bng my mi
H2SO4 (1.5 M, 2 M, 2.5 M).
nhm thu c cc ht da c kch thc 300 - 500
micron. Cc mu sau tin x l c tin hnh nghin
trong cng iu kin cc thi gian nghin khc
Nhm nh sng ch ca Nht do Masahiro Ueda
nhau. Tip theo mu s c lc qua cc sng Inox c
ng u pht kin ra tng ti s dng x
ng knh mt li l 1 mm v c git trung ha,
colagen ca da thuc sn xut cc vt liu c kh
git sch trc khi em sy kh. Qu trnh sy c
nng chu nhit dng lm tc gi (United States
thc hin bng thit b sy gi nng nhit 100 oC
Patent, 2004). thu c cc x colagen th cc
trong 24h.
mnh da thuc c x l trong mi trng axit
v mi trng kim vi cc phng n khc nhau. [7] 2.1.2 Nghin x da theo phng php kh:
C th thy rng, trong tt c cc nghin cu Vi phng php nghin x kh th sau khi
c cng b th trc khi ti s dng ph liu da c ng u ha v mt kch thc, da c sy s
giy u phi tri qua cng on nghin x. Cc b nhit 60oC trong 24h trc khi tin hnh
phng php c nghin cu nghin x rt a nghin. Thit b nghin kh c s dng trong
dng nhng nhn chung c tng hp thnh hai nghin cu l thit b nghin ba hai tng c cng
nhm l: (1) nghin x c hc khng s dng ha sut ng c 15kWh, cng sut nghin ti a 50kg/h.
cht v (2) nghin x c tin x l bng ha cht. Tuy Tc nghin c la chn l khong xp x 1500
nhin cc phng php nghin x ny ch mang tnh vng/pht.
gii thiu m khng c thng tin chi tit trn cc
ti liu v cng b quc t trong lnh vc c lin 2.3 Phng php phn tch
quan. Trc ht, nh gi tnh i din ca mu da
Chnh v vy, vic nghin cu kh nng nghin s dng trong nghin cu th cc tnh cht c bn ca
da ph liu c kim tra theo cc tiu chun sau:
x ph liu da thuc dng mnh thnh cc vt cht
dng x l bc nghin cu cn thit nhm hng ti - dy c kim tra trn thit b o dy
vic ch ng c cng ngh ti s dng ph liu da (VEB Werkstottpfilfi maschmen Leipzig) vi p lc
thuc sn xut cc vt liu mi. ti trng l 500 g, theo tiu chun TCVN 5071-90.
2. Thc nghim - bn ko t v gin t c tin hnh
kim tra trn thit b Tensilon RT- 1250A, theo tiu
2.1. i tng nghin cu
chun EN ISO 3376:2002,.
Mc ch ca nghin cu l kho st kh nng
- bn x c kim tra trn thit b Tensilon
cng ngh nghi n ph liu da thuc ca sn xut giy
RT- 1250A, theo tiu chun EN ISO 3377-2: 2002.
nhm nhn c hn hp sau nghin c nho,
u, ti xp. Xut pht t mc tiu nghin cu, i Hiu qu ca qu trnh nghin x c nh gi
tng nghin cu c la chn nghin x l ph thng qua trng thi mu v hnh dng cng nh kch
liu da b ct v da b vng ca qu trnh sn xut thc ca x sau nghin. Cc mu x sau nghin
giy. Da ph liu c thu nhn t cng ty da i Li c quan st trn knh hin vi in t chp nh vi
53
Tp ch Khoa hc v Cng ngh 116 (2017) 052-057
nh sng phn cc. Thit b c tch hp phn mm th l gii l do da c cu trc protein v cha cc
dinocapture 2.0 t ng xc nh kch thc i nhm (-COOH) trong phn t do vy chng khng
tng o ng knh v chiu di x thu c. bn vi kim. Kt qu l, trong iu kin x l kim,
m bo tnh so snh, phng i c c nh l trc khi din ra s phn tch cc x colagen khi
50 ln cho tt c cc mu. Cc thng s v ng cu trc da th xy ra qu trnh ha tan cc thnh
knh v chiu di x l c s so snh hiu qu ca phn protein v chuyn ha chng thnh cu trc gel.
cc phng php nghin. Do cu trc x ca lp ct rt bn chc do vy tc
phn tch x thp hn nhiu so vi qu trnh ha tan
3. Kt qu v bn lun
lm cho mu c nht ln. Kt qu ny cho thy
3.1 Kt qu kim tra cc c trng da mu vic tin x l da ct trong mi trng kim khng
em li hiu qu v khng p dng c thc y
Cc c trng, tnh cht v dy, bn ko
qu trnh phn tch cc b x colagen ln thnh cc
t, gin t v bn x ca da ph liu c
b x c cu trc mnh hn hoc x n.
kim tra theo cc tiu chun quc t. Cc kt qu v
tnh cht da c tng hp trn bng 1.
Bng 1. Mt s c trng tnh cht ca da ph liu
dng lm nguyn liu nghin x
c trng Da ct Da vng
dy (mm) 1.76 1.23
bn t (N/mm ) 2
15.27 7.44
gin t (%) 22.66 11.55
Lc x ln nht (N) 36.88 29.73
54
Tp ch Khoa hc v Cng ngh 116 (2017) 052-057
ln, khi lng x thu c sau khi lc v sy gim T cc kt qa so snh trn c th thy vi da
i. iu ny c ngha l mt lng x da b ha vng khi tin x l kim nng thp v thi gian
tan bi kim trong qu trnh nghin. ngn c th phn tch c thnh dng x sau
nghin. Tuy nhin vic tng thi gian hoc nng
Vi cc mu tin x l nng 30 g/l hnh
kim khi tin x l lm thu ngn chiu di x sau
nh thu c sau nghin vn c dng x tuy nhin
nghin. Tr mu da vng tin x l nng 20 g/l
khi lng thu c t hn nhiu so vi mu tin x
trong 2 h, cc mu cn li u cho thy mu sau
l 20 g/l. iu ny l do khi nng kim cng
nghin c nht cao, lng da b ha tan trong qu
cao th phn ng phn hy cu trc protein ca da
trnh nghin ln. V vy, nu dng phng php x l
din ra cng mnh. Ngoi ra, x thu c cng hn,
kim cho da vng th ch nn dng li mc khong
v vn cn mt phn keo nht bm dnh. c bit vi
20 g/l.
mu ngm trong 4h phi git bng axit mi c th
loi b hon ton lp vt liu nht. Vi iu kin tin 3.2.3 nh hng ca x l axit ti kh nng nghin
x l nng 40 g/l, sau khi nghin mu c x da ct
nht rt cao, k c thi gian ngm ch l 2 gi. Cc
Quan st s thay i th tch ca cc mu da
x thu c c kch thc gim i r rt.
trong qu trnh nghin c th thy r tc ph hy
4.1a 2.1a 4.1b 2.1b 4.1c 2.1c mu da ph thuc nhiu vo hm lng v thi gian
x l axit. Khi tng nng axit, tc phn tch x
din ra nhanh, tuy nhin bng quan st trc tip c
th nhn thy x b cng. Hnh dng mu da ct sau
nghin x c tin x l bng axit th hin trn hnh 3.
4. 2a 2. 2a 4.2b 2.2b 4.2c 2.2c C th nhn thy, khi tin x l bng axit tt c
cc mu thu c sau qu trnh nghin u c hnh
dng x r rng hn hn s vi x l bng kim. Tuy
vy cc x ny vn dng cu trc th v bt dnh,
khng ti xp, gia cc x vn cn mng bm dnh.
4.3a 4.3b 4.3c
2.3a 2.3b 2.3c iu ny l do trong mi trng axit da khng b ha
tan m ch b trng n lm cho lin kt lin phn t
gia cc chui mch polypeptit ca colagen yu i.
Do vy di tc ng ca lc x v ct ca qu trnh
nghin th s phn tch cc x chim u th so vi s
Hnh 2. Hnh dng mu thu c sau nghin ca da ct ngn mch.
vng vi cc iu kin tin x kim cc nng
Khi nng x l axit tng ln, tc ph hy
khc nhau: (1) 20 g/l; (2) 30 g/l; (3) 40 g/l v cc
chung ca mu c tng ln ng k tuy nhin kh
thi gian khc nhau (a) 2 h; (b) 3 h; (c) 4 h.
nng phn tch cc x khng c s khc bit nhiu.
3.1a 3.1b Hnh nh cc mu cho thy cu trc dng x c chiu
3.1c
di tng ln nhng khi cng ca cc b x thu
c cng tng ln. Cc kt qu ny cho thy, i vi
da ct th tin x l bng axit gip cho kh nng phn
tch x tt hn nhiu so vi x l kim. Mu thu
3. 2a 3.2b 3.2c c khng c dng nht m cng. Tuy nhin cc x
thu c khng ti xp.
3.2.3 nh hng ca x l bng axit ti kh nng
nghin x da vng
3.3a 3.3b 3.3c Thc nghim cho thy, cc mu da vng b ph
hy (khng cn hnh dng ming) trong khong thi
gian rt ngn. Hu ht kch thc cc mnh da u
gim i 50% sau khong thi gian nghin l 1 pht v
hon ton khng cn cu to dng ming sau thi
Hnh 3. Hnh dng mu thu c sau nghin da ct gian nghin l 2 pht. iu ny c ghi nhn vi tt
vi cc iu kin tin x axit cc nng khc c cc mu da vng c x l trong mi trng axit
nhau: (1) 1.5 M; (2) 2 M; (3) 2.5 M v cc thi gian cc iu kin nng v thi gian khc nhau. Hin
khc nhau (a) 2h; (b) 3h; (c) 4h tng ny c th l gii l do cu trc lng lo ca
lp vng da, lm cho kh nng thm thu ca cc
phn t axit vo khong th tch t do gia cc chui
55
Tp ch Khoa hc v Cng ngh 116 (2017) 052-057
mch polypeptit din ra nhanh hn, thc y qu ba. Hnh nh thu c sau nghin ca cc mu da
trnh trng n v lm mm da ngay c nng thp ct v da vng c th hin trn hnh 5.
vi thi gian x l ngn. Hnh nh v hn hp x da
C da ct v da vng th mu thu c sau khi
thu c sau nghin x cc mu da vng qua x l
nghin c dng x r nt. Vi da ct th x thu c
bng axit sunfuric c th hin trong hnh 4.
c chiu di 0,2 mm n 10 mm (ngn hn so vi cc
x thu c bng phng php nghin c tin x l
4.1a 4.1b 4.1c axit) v ng knh 0,020,07 mm. Mu sau nghin
x thu c da mn, an xen c hc vo nhau.
Vi mu da vng, x thu c sau khi nghin
rt mm, mn v ng u. ng knh cc x tp
4. 2a 4.2b 4.2c trung trong khong 0,020,05 mm. Chiu di ca x
gim i so vi cc x thu c khi nghin da ct. Mt
khc, tc nghin i vi da vng nhanh hn so vi
da ct. Thi gian cn thit tch x ch khong 30
giy.
4.3a 4.3b 4.3c
(a) (b)
56
Tp ch Khoa hc v Cng ngh 116 (2017) 052-057
57
Tp ch Khoa hc v Cng ngh 116 (2017) 058-062
Abstract
Mechanical alloying was used to synthesize in-situ copper based composite reinforced by binary niobium-
titanium-carbide from Cu, Nb, Ti and graphite powder mixture. The nominal composition was correponded to
Cu-30 vol.% (Nb,Ti)C. XRD patterns showed that (Nb, Ti)C was not formed in the as-milled powder after 5
hours of milling but was precipitated with a subsequent sintering at 900 oC. Milling time has showed a great
influence on both mechanical and physical properties of the sintered composite pellets. Increasing milling
time leads to an increase of the microhardness of the composite due to a higher degree of deformation that
enhanced hardening. On the other hand, the electrical conductivity decreases considerably when the milling
time increases. This phenomenon could be atrributed to the increase of density of grain boundaries, which
acts as a centre of electron scattering, with milling time.
Keywords: Cu, (Nb, Ti)C, Mechanical alloying, Sintering.
Tm tt
Phng php hp kim ha c hc c s dng tng hp vt liu compozit nn ng ct ht cacbit hp
kim (Nb, Ti)C t sinh t hn hp bt ca cc nguyn t thnh phn bao gm Cu, Nb, Ti v graphit. Ph
nhiu x tia Rnghen ca hn hp bt vi thnh phn tng ng vi 30% th tch (Nb,Ti)C cho thy pha
ccbit cha c to thnh sau 5h nghin nhng xut hin sau khi thiu kt 900 oC trong mi trng kh
argon. Thi gian nghin nh hng mnh n c tnh cht c hc v tnh cht vt l ca vt liu compozit.
Ko di thi gian nghin lm tng cng ca vt liu compozit do s tng mt khuyt tt trong mng
tinh th ca vt liu. Mt khc, tng thi gian nghin lm gim dn in ca vt liu do s tng ca mt
bin gii ht tinh th, qua lm tn x s chuyn ng ca cc in t trong vt liu.
T kha: ng, Cacbit hp kim (Nb, Ti)C, Nghin nng lng cao, Hp kim ha c hc, Thiu kt.
(a.u.)
C
(99.99%), purchased from Sigma Aldrich, with 7000
Lin (Counts)
mixture composition corresponding to Cu-30vol.% 6000
(N
Counts
5000
(N (N (N
(Nb,Ti)C. The mixture of powders was milled using a b, b, b, b, C
Fritsch Pulverisette 6 planetary ball milling in Ti
4000
Ti Ti Ti u
(d) )C )C
3000
compacted in a cylindrical steel mould at 800 MPa Fig. 1. XRD patterns of sintered samples at 900oC/1h
and then sintered in vacuum at 900oC for 1 hour. The from the powders of different milling times: (a) 5, (b)
density of the sintered in-situ (Nb,Ti)C-Cu composite 10, (c) 20 and (d) 30 hours
was determined based on Archimedes principle using
a Satorious electronic analytical balance. Micro- Copper crystallite size was determined by the
hardness and electrical conductivity of the composite Williamsons-Hall method from their corresponding
were measured using a Shimadzu Vickers micro- XRD patterns acquired on the sintered samples of
hardness tester at a load of 100 g and a four-point different milling times. The variations in the average
probe Changmin Tech CMT-SR2000N, respectively. crystallite size of Cu (DCu) in both as-milled powders
and sintered pellets for different milling times are
3. Results and discussion presented in Figure 2. The crystallite size decreases
According to our previous work [8], the as- rapidly, from 41 nm of starting copper powder at the
milled powder showed the diffraction peaks of the initial state of MA to 22 nm after 5 hours of milling.
starting elemental Nb and Ti powders after 5 hours of The average crystallite size of Cu drops slightly from
milling. From 10 hours to 30 hours of milling the 10 to 20 hours of milling time, and after 20 hours of
peaks of Nb and Ti powders are no longer existed milling the crystallite size of Cu decreases to 17 nm.
while almost all of the (Nb, Ti)C major reflections No change of DCu value occurs after 20 hours of
(111), (200) and (220) are detected. milling, indicating that steady-state is attained at 20
hours of milling.
Figure 1 shows the XRD patterns of the in-situ
sintered composites. The peaks of (Nb, Ti)C in the
XRD patterns of sintered samples of 5-hour as-milled
powder (Fig. 1a) are clearly visible. (Nb, Ti)C were
not formed in the as-milled powder after 5 hours of
milling but was precipitated with a subsequent
sintering at 900oC. According to [9], the reaction
temperatures for the formation of the carbide from the
elements Ti, Nb and carbon is higher than 1300oC.
The precipitation of (Nb, Ti)C in this present work
occurred at a much lower temperature with the
enhanced diffusivity of atoms due to the MA process.
The refinement of the grain size during MA increased
the number of grain boundaries. The numerous
interfaces provided a high density of short-circuiting
diffusion paths [10].
In the case of others composites (Fig. 1b-d), the Fig. 2. Copper crystallite size measured from XRD
diffraction peaks from the sintered in-situ composite, pattern for as-milled powders and sintered composite
compared to those of the as-milled powders, are more with different milling times
intense and well-defined than the peaks of as-milled At this stage, a balance was achieved between
powder. This phenomenon indicates that heat the rate of welding, which tends to increase the
treatment recovered considerable internal strains and average particle size, and the rate of fracturing, which
made the crystallite size increase remarkably. tends to decrease the average composite particle size
[10]. Compared to the crystallites of Cu in as-milled
powders, the crystallites of Cu in sintered pellets are
59
Tp ch Khoa hc v Cng ngh 116 (2017) 058-062
larger and follow a similar increasing trend. It is due [10]. The low density of sintered composite after the
to the heat-treatment results in recrystallization and initial milling time may be also due to the low-
crystallite growth. uniform distributions and the larger size of Nb and Ti
particles in 5-hour-as-milled powder.
In contrast to crystallite size, the internal strain
of Cu is increased with increasing milling time as Furthermore, the refined microstructural
shown in Figure 3. At the beginning of milling the features decrease the diffusion distances [10]. The
internal strain in the Cu lattice structure increases mechanisms can easily be understood, the finer
rapidly due to the dissolution of carbon in the copper particle size results in a higher surface energy for a
matrix. After 20 hours of milling, the lattice strain of compact, thus a higher driving force for grain growth
copper increases slightly, possibly because during the (growth of crystallites) and densification to reduce
MA powder particles are subjected to high-energy the system's Gibbs energy [12]. Furthermore, the
collisions, causing a heavy plastic deformation that is higher amount of contact points between the particles
associated with a high density of defects, such as activated the transport of matter leading to a high
dislocations and stacking faults [11], which is the number of necks between particles, motivating the
main contributor to the increase in lattice strain. The diffusion and evaporationcondensation of the matter
internal strain for Cu in the sintered in-situ composite on surfaces with consequent bulk densification [13].
is lower than that in the as-milled powder, probably
because the stored energy in the as-milled powder
particle is released because of a recovery or
relaxation process within the boundaries during the
sintering process.
60
Tp ch Khoa hc v Cng ngh 116 (2017) 058-062
pellet as a function of milling time of the sintered Cu- formation of (Nb,Ti)C, and the porosity of the
-(Nb,Ti)C composite is shown in Figure 5. The composite. As can be seen in Figure 6, the electrical
microhardness value increases from 359 HV to conductivity increases rapidly from 6.02 x 10 8 (m)-1
431 HV as the milling time increases from 5 to 30 after 5 hours of milling to 9.09 x 10 8 (m)-1 after 10
hours. This is to be expected since during MA the hours of milling. It is due to a considerable reduction
crystallite size was regularly refined to a nanometer in the large degree of porosity that had been found in
level, allowing a higher degree of deformation that the 5-hour composite. The electrical conductivity
produced lattice distortion in the matrix copper. This decreases considerably when the porosity increases.
lattice distortion then created lattice strain and The decrease of electrical conductivity with milling
increased the dislocation which enhanced hardening. time is confirmed by the density results. From 10 to
The ultra-fine particles of (Nb,Ti)C increased the 30 hours of milling the electrical conductivity slightly
amount of interfacial bonding between the decreases to 8.17 x 108 (m)-1. The possible cause of
reinforcement and Cu matrix, which also contributed this slight decrease is the increase of density of grain
to the composites enhanced mechanical properties boundaries, which acts as a centre of electron
[14]. scattering, with milling time. According to Murty et
As shown in Figure 5, the microhardness value al. [16], with an increasing amount of grain
rose rapidly between 5 and 10 hours of milling. At boundaries, the mean free conductive path decreases,
this stage, the effect of dislocation is not the main resulting in increased resistivity.
factor in the increased microhardness, instead, the
major influence is the formation of the carbide
(Nb,Ti)C in the Cu matrix. Furthermore, when the
milling time exceeds 20 hours, the Vickers hardness
variation is negligible, suggesting that the MA
process may have reached steady-state by 20 hours of
milling.
The mechanism of strengthening can be
explained using Orowans mechanism. In Orowans
mechanism [15], impenetrable precipitates in the
matrix interrupt dislocation migration and thus plastic
deformation via interaction with dislocations, which
results in an increase in the matrix strength.
The strengthening of the metal matrix by rigid
particles is achieved as follows: Fig. 6. Variation on electrical conductivity of Cu-
(Nb,Ti)C composites with different milling times
(1)
61
Tp ch Khoa hc v Cng ngh 116 (2017) 058-062
microhardness and electrical conductivity after 20 [4] T. Takahashi, Y. Hashimoto, Mater. Sci. Forum. 88
hours of milling, where the microhardness and (1992) 175 182.
conductivity are 420 HV and 8.62 x 108 (m)-1, [5] M. T. Marques, V. Livramento, J. B. Correia, A.
respectively. This finding suggests that to produce Almeida, R. Vilar, Materials Science and Engineering
Cu-(Nb,Ti)C composite with high microhardness and A 399 (2005) 382-386.
high electrical conductivity, in addition to lower [6] M.T. Marques, A.M. Ferraria, J.B. Correia, A.M.
power consumption, the optimum milling duration is Botelho do Reg, R. Vilar, Materials Chemistry and
20 hours. Physics 109 (2008) 174180.
4. Conclusion [7] Z. Hussain, R. Othman, Bui D. L., Minoru U., Journal
of Alloys and Compounds 464 (2008) 185-189.
The in-situ Cu-(Nb, Ti)C nanocomposite pellets
have been successfully synthesized via mechanical [8] L.M. Hai and T.D. Huy, Journal of Science and
alloying and powder metallurgy. Milling time Technology 112 (2016) 80-84.
exhibited a great influence on both the mechanical [9] L.E. Toth, Transition metal carbides and nitrides,
and physical properties of the sintered composite Academic Press, New York (1971) 13.
pellets. Increasing milling time leads to an increase of
[10] C. Suryanarayana, Mechanical Alloying and Milling,
the microhardness of the composite due to a higher
Marcek Dekker, New York, USA (2004) 59-66, 83-
degree of deformation that enhanced hardening. On 87.
the other hand, the electrical conductivity decreases
considerably when the milling time increases. It could [11] M.S El-Eskandarany, Mechanical alloying for
be atrributed by the increase of density of grain fabrication of advanced engineering materials, Noyes
Publications, New York, USA (2001) 16-18.
boundaries, which acts as a centre of electron
scattering. Our results indicated that the in-situ Cu- [12] Q. Jiang, S.H. Zhang, J.C. Li, Solid State
(Nb,Ti)C composite reached a good combination of Communications 130 (2004) 581584.
microhardness and electrical conductivity after 20 [13] C. Santos, M.H. Koizumi, J.K.M.F. Daguano, F.A.
hours of milling, where the microhardness and Santos, C.N. Elias, A.S. Ramos, Materials Science
conductivity are 420 HV and 8.62 x 108 (m)-1, and Engineering A 502 (2009) 6-12.
respectively.
[14] H. Zuhailawati, Y. Mahani, Journal of Alloys and
References Compounds 476 (2008) 142-146.
[1] L. Froyen, J.D. Wilde, Materials Science Forum Vols [15] E. Orowan, Symposium on International Stresses,
437-438 (2003) 141-144. Institution of Metal, London (1947) 451.
[2] M. Krasnowski, T. Kulik, Journal of Alloys and [16] B.S. Murty, T. Venugopal, K.P. Rao, Acta
Compounds 448 (2008) 227-233. Metallugica 55 (2007) 4439-4445.
[3] Zhang. X., Wang H., Liao. L., Ma. N., Composites
Science and Technology 67 (2007) 720-727.
62
Tp ch Khoa hc v Cng ngh 116 (2017) 063-067
Tm tt
Dy nan silic (SiNWs) c tng hp bng phng php bc bay nhit ti nhit cao trong khong t
1100 0C n 1200 0C trn Si (111) s dng vt liu ngun l hn hp bt Si:C. Kt qu nh hin vi in
t qut cho thy kch thc ca SiNWs thu c c ng knh vi chc nanomt. Cu trc li/v ca dy
Si c quan st bng knh hin vi in t truyn qua phn gii cao. Ph pht x hunh quang ca dy
nan silic nhit phng c lin quan n hiu ng giam gi lng t khi thu nh kch thc ca dy.
T kha: SiNWs, phng php bc bay nhit, cu trc li/v;
Abstract
Silicon nanowires (SiNWs) were synthesized on Si (111) surfaces using the vaporliquidsolid technique at
high temperature ranging from 1100 0C to 1200 0C. Si:C mixture powders were used as the material
sources. Scanning electron microscope images were revealed that the Si nanowires had few tens
nanometer of diameter. The Si-core/SiOx-shell structure of the nanowires was investigated via transmission
electron microscopy. The photoluminescence of the nanowires at room temperature demonstrated a
quantum confinement effect because of the reduced diameter of the nanowires.
Keywords: SiNWs, thermal evaporation method, core/shell structure;
63
Tp ch Khoa hc v Cng ngh 116 (2017) 063-067
trng kh nit. Tip theo, mt lp mng vng (Au) Hnh 1 m t c ch VLS ca qu trnh hnh
vi dy 2 nm c ph ln b mt Si bng thnh dy nan Si. Vi mt lp mng Au, nhit
phng php bc bay bng chm in t lm xc cao s lin kt mng b ph v, cc nguyn t s co
tc. H bc bay s dng l Boc-Edward Auto 500 vi cm to thnh cc ht Au nh c ng knh c
chn khng ban u t ~ 10-6 mbar. nanomt. Cc ht kim loi nhanh chng kt hp vi
Si to thnh hp kim Au-Si. Khi c cp ngun
Cc tm Si(111) c ph mng Au ny sau
hi do s bc bay nhit ca bt Si, cc nguyn t Si
c t vo b g mu v chuyn nhanh vo l ca
c th bm vo v khuch tn xung quanh cc ht
h bc bay nhit thc hin qu trnh hnh thnh
nan Au to trng thi qu bo ha. Cc nguyn t Si
dy nan Si. Ngun vt liu bay hi l hn hp bt Si
tip tc khuch tn vo vng hp kim lng Au/Si qu
(Testbourne 200 mesh) v bt C trn vi t l 1:1
bo ha nu trn, sau kt tinh to cu trc mt
[10], c t trong cc ng vt liu bng xt
chiu l dy Si.
nhm gia l ni c nhit c xc nh chnh
xc bng cp nhit. Khong cch gia cc ng vt Hnh 2 th hin cc kt qu ca s to ht nan
liu v Si l 5 cm, m bo nhit bng nhit Au v dy nan Si cc iu kin ch to khc nhau.
tm l nhit. Tc nng nhit, thi gian nng Hnh 2.a l nh SEM ca Si c cha cc ht nan
nhit c iu khin thng qua b iu khin nhit Au khi nhit ti nhit 900 0C i vi mng Au
. Kh Ar tinh khit (99,9%) c a vo bung dy 2 nm. C th thy lp mng vng di tc dng
phn ng vi lu lng kh c gi n nh ~500 ca nhit co cm li thnh cc ht kim loi xc
sccm. Nhit trong l c nng ln n nhit tc, cc ht nan Au ny c kch thc nh vi chc
mc dy Si trong khong t 1100 0C n 1200 0C vi nanomt v c nh hng n ng knh dy Si.
tc nng nhit 10 0C/min. Ti nhit cao, qu Theo c ch pht trin dy VLS, nu kch thc ht
trnh to dy nan Si hnh thnh v thi gian mc l xc tc ln, ng knh dy Si nhn c s ln. Khi
30 pht. kch thc ht xc tc nh th ng knh dy s b.
Tuy nhin, kch thc, s ng u cng nh phn b
Kt thc qu trnh, cc mu c lm ngui t
ht xc tc cng ph thuc vo b dy ca mng
nhin n nhit phng trong mi trng kh tr.
mng Au. Trong mt s nghin cu trc, chng ti
Mu dy Si sau khi ch to s c kho st mt s
cp [11].
tnh cht v cu trc v tnh cht quang thng qua cc
php o hin vi in t qut pht x trng (FESEM-
S4800 Hitachi) kt hp ph tn sc nng lng tia X
(EDX), hin vi in t truyn qua phn gii cao
(HRTEM-JEM 2100 Jeol), v ph pht x hunh
quang (PL - Jobin Yvon) dng ngun kch thch laser
c bc sng 325 nm o nhit phng.
3. Kt qu v tho lun
Trong phng php ch to dy nan Si, c ch
hi-lng-rn (VLS) ng vai tr quan trng trong qu
trnh hnh thnh cu trc nan mt chiu. ng knh
dy Si ph thuc vo kch thc ht xc tc.
64
Tp ch Khoa hc v Cng ngh 116 (2017) 063-067
ch VLS. Hnh 2.c v 2.d l cc nh SEM ca b mt ca SiOx v SiO ni trn. Khi Si khuch tn vo
cha dy nan Si tng hp tng ng cc nhit vng qu bo ha ca hp kim Au-Si v pht trin
1150 0C v 1200 0C. theo hng xc nh v b bao bc bi lp v v nh
hnh SiOx (bao gm c SiO2, SiO).
Khi nhit mc dy tng ln, kch thc ca
dy Si khng ng u. Cc dy Si c ng knh ln Kt qu chp ph tn sc nng lng (EDX) ca
70-90 nm nm xen k cc dy c ng knh nh dy Si th hin trn hnh 4 cho thy ph hp vi kt
~20-30 nm. C th l gii iu ny l do s tip tc qu nh HRTEM nhn c v cu trc li/v. Theo
co cm ca mt s ht xc tc kch thc nh to , nguyn t silic chim 75,5 % khi lng (tng
thnh cc ht c kch thc ln hn khi nhit ng 63,7 % v nguyn t), nguyn t xi chim 24,5
cao gim thiu nng lng b mt, do c s % khi lng (ng 36,3 % nguyn t), s hin din
phn b li v kch thc v mt ht Au. Chnh s ca nguyn t Au gn nh khng c do qu t.
thay i ny dn n s thay i v kch thc v s
khng ng u ca dy nan Si trn b mt
Si(111). S thay i v kch thc ca dy Si ph
thuc vo kim loi xc tc cng c mt s
nghin cu khc cp n [13, [14].
65
Tp ch Khoa hc v Cng ngh 116 (2017) 063-067
66
Tp ch Khoa hc v Cng ngh 116 (2017) 063-067
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[15] R. J. Barsotti, J. E. Fischer, C. H. Lee, J. Mahmood, C. 4836, 2002.
K. W. Adu, and P. C. Eklund, Imaging, structural,
67
Tp ch Khoa hc v Cng ngh 116 (2017) 068-071
Abstract
H2S gas sensor based on SnO2 (40 nm)/ NiO (20 nm) thin film was fabricated by DC sputtering method in
combination with photolithography technique. Morphology, crystal structure, and composition of the
synthesized thin film were characterized by SEM, EDS and XRD. The gas-sensing characteristics of the
fabricated sensor were studied by real time measurement of resistance change in air and different
concentrations of H2S gas. Results show that the sensor can measure low concentrations of H2S (2,5 to 10
ppm) at various temperatures ranging from 250 to 400 oC with fast response time (about 13 - 33 seconds)
and fulfill the requirements in air monitoring.
Keywords: SnO2/NiO thin film, Gas sensors, H2S
Tm tt
Bi bo ny gii thiu cc kt qu nghin cu v cm bin kh H2S trn c s mng mng SnO2/NiO (chiu
dy 40 nm/ 20 nm) bng phng php phn x hot ha. Vi cu trc v tnh cht ca vt liu SnO2/NiO
c kho st bng nh hin vi in t qut, ph tn xc nng lng v gin nhiu x tia X. Tnh cht
nhy kh ca cc cm bin c nghin cu mt cch c h thng trong gii nng kh H2S t 2.5 10
ppm v trong gii nhit 250 - 400 oC theo thi gian. Cc kt qu nghin cu cho thy cm bin c thi
gian p ng nhanh (t 13 33 giy) v p ng c yu cu ng dng trong quan trc nhim mi
trng kh.
T kha: mng mng SnO2/NiO, cm bin kh, H2S
xit kim loi thun khit thng c p ng khng bia: 5 cm, chiu dy bia: 5 mm) phn x mng
cao v c chn lc kh km [8]. Do , nghin cu NiO dy 20 nm (11). S dng cng ngh Liff-off
ch to cm bin kh H2S c nhy cao, gii hn o ty b phn NiO khng s dng (12). Cui cng ta
thp v c chn lc cao vn ang l mt vn cho c phin in cc ch to vo trong mi
thch thc gii nghin cu trn ton th gii. trng khng kh nhit 400oC/2h. Hnh thi v
vi cu trc ca mng mng lp nhy kh c kho
Trong bi bo ny chng ti la chn vt liu
st bi nh hin vi in t qut pht x trng (FE-
mng mng SnO2/NiO (dy 40/20 nm) bng phng
SEM, JEOL 7600) v nhiu x tia X (XRD) v ph
php phn x ch to cm bin o kh H2S. Vic
tn sc nng lng EDS. Tnh cht nhy kh ca cm
thit k v a ra cc quy trnh cng ngh ch to
bin c o c bi h kho st kh t to ca nhm
cm bin trn quy m kch c phin silic (wafer)
iSensor-Vin ITIMS.
c chng ti tp trung nghin cu nhm ch to
c cm bin c p ng cao, thi gian p ng 3. Kt qu v tho lun
nhanh phc v cho vic quan trc nhim mi
Sau khi ch to c th thu c phin Si gm
trng khng kh.
trn 350 cm bin nh trn Hnh 2(a). Hnh dng v
2. Thc nghim kch thc ca cm bin c th thy trn Hnh 2(d),
trong chip cm bin ch to c kch thc 33
Thit k v quy trnh ch to c th hin trn
mm2, trong din tch lp mng mng nhy kh l
Hnh 1. C th, phin Silic loi p (100) kch thc 4
260260 m. Mt v kch thc mng mng SnO2
inch c in tr 1-10 cm c ra sch theo cng
c th quan st trn Hnh 2(c). nh FE-SEM b mt
ngh tiu chun ca cng ngh vi in t (1). Tip
ca mng mng SnO2 sau khi nung nhit 400
theo phin c oxi ha to lp SiO2 dy o
C/2 gi, qua Hnh 2(c) cho thy b mt mng c
ng u cao, cc ht mn nh v c kch thc c 10
(1) (6) n 20 nm. Mc d vy c th thy cc vt dn v
trn b mt mng, y c th l do ng xut ca mng
trong qu trnh ch to.
(2) (7) (a) (b)
(3) (8)
(c) (d)
(5) (10)
5 m
Hnh 1. Quy trnh ch to chp cm bin
1 m lm lp cch in bng cng ngh oxi ha 100 nm
m (1). Sau tin hnh ph lp nhy quang v s
dng mt n th nht tin hnh quang khc hnh Hnh 2. Hnh nh cm bin trn phin silic 4 inch (a); nh
dng ca in cc (2, 3). Tin hnh phn x lp Cr c mt chp cm bin (b); nh SEM mng mng SnO2/NiO
chiu dy 5 nm v lp Pt c chiu dy 300 nm lm sau khi ch to (c); v ph EDS ca mng mng SnO2/NiO
in cc (4). Sau khi phn x ta dng cng ngh liff- (d).
off ty b phn Cr/Pt (5). Tip theo ta tin hnh
Trn Hnh 3 l gin nhiu x tia X ca mng
quang khc mt n th 2 m ca s cho lp nhy
SnO2 c x l ti 400 oC/2 gi. Gin nhiu x
ca vt liu (6, 7). Sau dng bia Sn ( sch ca
tia X cho thy xut hin cc nh nhiu x cng
bia t 99,99%, ng knh ca bia: 5 cm, chiu dy
bia: 5 mm) phn x mng SnO2 dy 40 nm trong mnh nht ti 2 = 26,65o ng vi mt (110) v cc
mi trng kh Ar/O2 vi t l 1:1 (8). S dng cng nh ti gc 2 l 33,7o v 51,7o tng ng vi mt
ngh Liff-off ty b phn SnO2 khng s dng (9). (101) v (211) ca SnO2 cu trc t din (JCPDS, 41-
Sau khi ch to mng SnO2 ta tin hnh quang khc 1445).
mt n th 3 m ca s cho lp xc tc (10). Dng Cc nh nhiu x tri rng chng t kch thc
bia NiO ( sch ca bia t 99,99%, ng knh ca ht tinh th ca mng mng kh nh. Theo cng thc
69
Tp ch Khoa hc v Cng ngh 116 (2017) 068-071
thc nghim ca Scherrer c th tnh c kch thc p ng ca cm bin tng ng vi nng kh H2S
tinh th trung bnh d= k/cos. Trong k ~ 0,9 l ti nng 2,5; 5; v 10 ppm ln lt c cc gi tr l
hng s thc nghim, l bc sng ca tia X (i 2,23; 2,63 v 3,31 ln. Tip tc tng nhit vi cc
vi bc x CuK: = 0,154056 nm), l rng ti gii nhit l 300; 350 v 400 oC ta thy nhit
na cao ln nht (Full Wide at Half Maximum) 400 oC p ng ca linh kin l cc i, ng vi
ca nh ph tnh theo radian, l gc nhiu x ca tt c cc nng kh kho st. Ln lt l 4,02; 6,25
nh ph . Gi tr c tnh kch thc tinh th trung v 8,67. iu cho thy cm bin c mng mng
bnh ca mng mng SnO2 l khong 12 nm. Mc d SnO2/NiO ch to bng phng php phn x lm
vy khng pht hin c s sut hin nh nhiu x vic tt nht gii nhit 400 oC. Qua Hnh 4(b) ta
ca NiO trn gin nhiu x tia X. iu ny c th thy nhy ca mng mng SnO2/NiO c nhy
gii thch do mng NiO qu mng, nn tn hiu ca cao nht 400 oC v nhy tng dn u khi ta tng
NiO b ln t bi tn hiu ca SnO2. Tuy nhin qua nng kh. nhy cao nht t 8,67 ln ng vi
ph tn sc nng lng EDS ca mng mng (Hnh nhit 400 oC vi nng kh l 10 ppm kh H2S.
2(d)) cho thy hp phn ca cc nguyn t c mt 2.5 ppm 5 ppm 10 ppm
trong mu vi cc nguyn t chnh l Sn, O, NiO, Si. 120 (a)
10 o
250 C
400 C
80 o
350 C
o
NiO l cc nguyn t m chng ta ch to. 40
8
o
400 C
105
in tr ()
SnO2 (110)
p ng (Ra/Rg)
Tetragonal SnO2 70
350 C
o
35 6
JCPDS, No. 41 - 1445
C-ng (.v.t.y.)
120
SnO2 (101)
80
300 C
o
SnO2 (211)
4
40
SnO2 (200)
105
250 C
70 2
SnO2 (210)
o
35
70
Tp ch Khoa hc v Cng ngh 116 (2017) 068-071
Nng kh (ppm) Nng kh (ppm) [7] H. Liu, S.P. Gong, Y.X. Hu, J.Q. Liu, D.X. Zhou,
Properties and mechanism study of SnO2 nanocrystals
Hnh 5. Thi gian p ng v hi phc ca cm bin. for H2S thick-film sensors, Sens. Actuators B 140
(2009) 190195. doi:10.1016/j.snb.2009.04.027.
4. Kt lun
[8] D.J. Yoo, J. Tamaki, S.J. Park, N. Miura, N.
Cm bin kh H2S trn c s mng mng Yamazoe, H2S sensing characteristics of SnO2 thin
SnO2/NiO c ch to thnh cng. Cng ngh film prepared from SnO2 sol by spin coating, J.
ny cho php ch to quy m ln cc chp (~400 Mater. Sci. Lett. 14 (1995) 13911393.
chp/1 phin Si 4-inch) cm bin bng s kt hp doi:10.1007/BF00270739.
gia phng php phn x hot ha v quang khc.
[9] S.-W. Choi, A. Katoch, J. Zhang, S.S. Kim,
nh hng ca mng mng SnO2/NiO ln tnh nhy Electrospun nanofibers of CuO/SnO2 nanocomposite
kh H2S trong gii nng t 2,5 10 ppm v trong as semiconductor gas sensors for H2S detection, Sens.
gii nhit t 250 400 oC theo thi gian c Actuators B 176 (2013) 585591.
kho st. Cm bin cng c th lm vic c trong doi:10.1016/j.snb.2012.09.035.
iu kin nhit thp l 250 oC vi p ng t
2,23 ln vi nng 2,5 ppm kh H2S. Thi gian p [10] G.J. Fang, Z.L. Liu, C.Q. Liu, K.L. Yao, Room
temperature H2S sensing properties and mechanism of
ng ca cm bin nhanh trong khong t 13-33 giy 2CeOSnO solgel thin films, Sens. Actuators B, 6
ty thuc vo nhit v nng kh o. D trn (2000) 46.
quy trnh cng ngh ch to ny hon ton c th pht
trin ch to c s lng ln cm bin o kh [11] Mukta V. Vaishampayan, Rupali G. Deshmukh,
H2S quy m cng nghip. Pravin Walke, I.S. Mulla, Fe-doped SnO2
nanomaterial: A low temperature hydrogen sulfide
Li cm n. Cng trnh ny c thc hin vi s ti gas sensor, Materials Chemistry and Physics 109
tr ca ti cp Trng m s: T 2015 - 068 (2008) 230234.
doi:10.1016/j.matchemphys.2007.11.024
Ti liu tham kho
[12] D.-L. Tang, S. He, B. Dai, X.-H. Tang, Detection H2S
[1] S.K. Pandey, K.-H. Kim, K.-T. Tang, "A review of mixed with natural gas using hollow-core photonic
sensor-based methods for monitoring hydrogen bandgap fiber, Opt. - Int. J. Light Electron Opt. 125
sulfide", TrAC Trends Anal. Chem. 32 (2012) 8799. (2014) 25472549. doi:10.1016/j.ijleo.2013.10.097.
doi:10.1016/j.trac.2011.08.008.
[13] D.D. Vuong, G. Sakai, K. Shimanoe, N. Yamazoe,
[2] Y. Guan, C. Yin, X. Cheng, X. Liang, Q. Diao, H. Hydrogen sulfide gas sensing properties of thin films
Zhang, et al., Sub-ppm H2S sensor based on YSZ and derived from SnO2 sols different in grain size, Sens.
hollow balls NiMn2O4 sensing electrode, Sens. Actuators B 105 (2005) 437442.
Actuators B 193 (2014) 501508. doi:10.1016/j.snb.2004.06.034.
doi:10.1016/j.snb.2013.11.072.
[14] N. Van Hieu, P. Thi Hong Van, L. Tien Nhan, N. Van
[3] J.-Z. Dong, S.M. DeBusk, GCMS analysis of Duy, N. Duc Hoa, Giant enhancement of H2S gas
hydrogen sulfide, carbonyl sulfide, methanethiol, response by decorating n-type SnO2 nanowires with
carbon disulfide, methyl thiocyanate and methyl p-type NiO nanoparticles, Appl. Phys. Lett. 101
disulfide in mainstream vapor phase cigarette smoke, (2012) 253106. doi:10.1063/1.4772488.
71
Tp ch Khoa hc v Cng ngh 116 (2017) 068-071
72
Tp ch Khoa hc v Cng ngh 116 (2017) 072-076
Tm tt
ng nano ccbon c tng hp bng phng php lng ng nhit ha hc t pha hi vi kh ngun
ccbon l axilen (C2H2), kim loi xc tc l hp kim permalloy (Fe19Ni81). S hnh thnh, kch thc v hnh
thi ca ng nano ccbon ph thuc vo lp kim loi xc tc v nhit . 750 oC, vi mng kim loi xc
tc dy 10 nm, ng nano ccbon thu c c nh hng thng ng, tuy nhin nu b dy mng kim loi
xc tc ln hn 20 nm, ng nano ccbon khng th hnh thnh. Trong vng nhit 650 oC - 850 oC, nhit
kim loi xc tc cng cao, ng knh ca ng nano ccbon thu c cng ln v mt gim.
T kha: ng nano ccbon, c ch VLS, CVD nhit, kim loi xc tc
Abstract
Carbon nanotubes were synthesized by thermal chemical vapor deposition method using acetylene (C 2H2)
as carbon precursor, permalloy (Fe19Ni81) as catalyst. The formation, dimension and morphology of
nanotubes were strongly depended on the parameters of catalyst thin film and sintering temperature. At
750oC, with 10-nm thickness catalyst film, carbon nanotubes were aligned vertically, but when catalyst film
was thicker than 20 nm, no CNT was observed. In the range from 650 oC to 850 oC, at higher sintering
temperature, the obtained carbon nanotubes had larger diameter.
Keywords: carbon nanotubes, VLS mechanism, thermal CVD, catalyst metal.
73
Tp ch Khoa hc v Cng ngh 116 (2017) 072-076
hay cc ht kim loi. cng mt nhit x l, kch [13]. Tnh nh hng ca cc CNT l do tng tc
thc cc ht kim loi xc tc tng tuyn tnh vi b vt l gia cc CNT lc Van der Waals [11]. Khi
dy mng [16,20]. V vy khi b dy ln, cc ht cc CNT cng ng u v cng st nhau (mng kim
kim loi xc tc c kch thc ln hn di khuch loi xc tc mng ~ 10 nm) mt CNT cao lc
tn ca ccbon v do n khng h tr cho s hnh tng tc cng ln, v trong qu trnh mc cc CNT
thnh ca CNT [6,19]. ta vo nhau mc thng ng (Hnh 3.a).
Vi mng kim loi xc tc c b dy ln, cc
ht kim loi xc tc to ra c kch thc trung bnh
ln hn. Tuy nhin cc ht to ra c kch thc
khng ng u, n gm cc ht to nm xen k vi
cc ht nh. Cc ht c kch thc ln hn chiu di
khuch tn ca ccbon s khng h tr CNT hnh
thnh, ch cc ht c kch thc nh hn chiu di
khuch tn ca ccbon mi ph hp lm mm cho s
hnh thnh ca CNT. Cc CNT hnh thnh t cc ht
kim loi xc tc nm xen k gia cc o kim loi
ln, v cch xa nhau, do chng gn nh khng
tng tc vi nhau mc nh hng (Hnh 3.b).
(a) (b)
74
Tp ch Khoa hc v Cng ngh 116 (2017) 072-076
cho thy xu hng gim nghing hay s tng ca khi tng nhit x l mng kim loi xc tc, chng
nh hng thng ng ca cc CNT khi i t mp ti thu c CNT c ng knh ln hn, v mt
ca mng CNT (pha bn phi) vo trong mng CNT xp kht thp hn. trn 900 oC, chng ti ch thu
(pha bn tri). Hirose v cc cng s s dng s c si ccbon c kch thc ln. Hnh 4 l nh
thay i lc tng tc Van der Waals theo v tr ny SEM chp ct lp ca CNTs mc 750 oC (Hnh 4.a)
iu khin nh hng ca mng CNT [21]. v 850 oC (Hnh 4.b). T nh SEM c th cho thy
rng nhit 750 oC, ng CNT hnh thnh c
ng knh nh hn v mt xp kht cao hn so
vi CNT nhn c nhit 850 oC. Nh vy, khi
tng nhit , ng knh ca CNT tng v xp
kht ca cc CNT thng ng gim. Kt qu ny ca
chng ti ph hp vi kt qu m Siegel v cng s
thu c [8].
S tng kch thc theo nhit c l gii
l do, khi tng nhit , kch thc trung bnh ca
ht kim loi xc tc tng dn, khi tng n kch thc
ti hn (ln hn chiu di khuch tn tng ng ca
ccbon) th cc si ccbon hnh thnh thay cho CNT.
Nu tip tc tng nhit , kch thc trung bnh
tip tc tng, nhng lc ny xut hin ng thi cc
ht kim loi xc tc rt nh (Rmin ~ mt vi nano mt)
nm xen k gia cc ht kim loi rt ln, cc ht ny
c kch thc nh h tr s hnh thnh ca
CNT n vch [14,15,18]. V vy tng hp CNT
n vch t cc mng kim loi xc tc, cc nhm
thng tng hp nhit cao.
4. Kt lun
Chng ti trnh by cc kt qu nghin cu
v nh hng ca mng kim loi xc tc ti qu trnh
tng hp CNT bng phng php CVD nhit. B
dy ti hn ca mng xc tc permalloy trn
SiO2/Si mc CNT 750 oC l 20 nm. Vi b dy
trong khong t 5 10 nm, CNT c c nh hng
thng ng. Nhit nh hng phc tp ti s
Hnh 4. nh SEM chp ct ngang ca rng CNT hnh thnh CNT. Trong di nhit t 650 oC n
mc nh hng thng ng vi mng kim loi xc 850 oC, khi tng nhit , ng knh ca CNT tng
tc permalloy dy 10 nm, tng hp nhit 750 oC v mt CNT gim.
(a) v 850 oC (b). Li cm n
3.2 nh hng ca nhit Nghin cu ny c ti tr bi Qy Pht trin
nh hng ca nhit l rt phc tp, c hai Khoa hc v Cng ngh Quc gia (NAFOSTED)
thng s nhit nh hng ti qu trnh mc CNT trong ti m s 103.02-2015.05.
l: nhit phn ng hay nhit mc CNT v nhit Ti liu tham kho
hnh thnh ht kim loi xc tc. Khi nghin cu
tch bit nh hng ca nhit phn ng v nhit [1] E. Shawat, V. Mor, L. Oakes, Y. Fleger, C.L. Pint, G.
ti vic hnh thnh CNT, cc nhm nghin cu D. Nessim, Nanoscale, 6 (2014) 1545-1551.
trn th gii cho thy nhit phn ng khng nh [2] Haider Almkhelfe, Jennifer Carpena-Nez, Tyson C.
hng nhiu ti kch thc ca CNT. Kch thc ca Back and Placidus B. Amama, Nanoscale, 8 (2016)
CNT ch b nh hng bi nhit x l mng kim 13476-13487.
loi xc tc hay nhit [19,20]. Trong bi bo [3] J. Lee, I.Y. Stein, S.S. Kessler, B.L. Wardle, Applied
ny, chng ti trnh by nh hng ca nhit ti Materials and Interfaces, 7(16), (2015) 8900-8905.
kch thc ca CNT. T cng thc (1) ta thy rng
khi tng nhit cng cao, kch thc nh nht [4] J.P. Giraldo, M. P. Landry, S.M. Faltermeier, T.P. Mc
Nicholas, N.M. Iverson, A.A. Boghossian, N.F.
ca ht kim loi xc tc cng gim. Tuy nhin, trong
Reuel, A.J. Hilmer, F. Sen, J.A. Brew , M.S. Strano,
gii nhit t 650 oC n 850 oC c nghin cu, Nature Materials, 13 (2014) 400-408.
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[5] A. Lenert, D.M. Bierman, Y. Nam, W.R. Chan, I. nanostructures for optoelectronic devices processing
Celanovic, M. Soljacic, E. N. Wang, Nature characterixation and applications, Yi Guy-Chun
Nanotechnology, 9 (2014) 400-408. (Editor), ISBN: 978-3-642-22479-9 (2012) 9.
[6] Y. Y. Wei, G. Eres, V. I Merkulov, D. H. Lowndes, [14] H. U. Rashid, K. Yu, M. N. Umar, M. N. Anjum, K.
Applied Physics Letters, 78(2001) 1394-1396. Khan, N. Ahmar, M. T. Jan, Reviews on Advanced
Materials Science, 40 (2015) 235-248.
[7] S. Fan, M. G. Chapline, N. R. Franklin, T. W.
Tombler, A. M. Cassell, H. Dai, Science, 283 (1999) [15] V.L. Kuznetsov, A.N. Usoltseva, A.L. Chuvilin, E.D.
512-514. Obraztsova, J-M Bonard, Physical review B, 64
(2001) 235401-235407.
[8] M. P. Siegel, D. L. Overmyer, P. P. Provencio,
Applied Physics Letters, 80 (2002) 2171. [16] Q.A. Nerushev, S. Dittmar, R.E. Morjan, F.
Rohmund, E. E.B. Campbell, Journal of Applied
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Letters, 82 (2003) 448.
[17] Wei-Wen Liu, Azizan Aziz, Sian-Piao Chai, Abdul
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Thang, N N Trung, N H Lam, Synthesis of multi- Nanomaterials, 2013 (2013) ID 592464.
walled and single-walled carbon nanotubes by
thermal CVD method, Proceedings of the Eleventh [18] S. B. Sinnott, R. Andrews, D. quian, A. M. Rao, Z.
Vietnamese-German Seminar on Physics and Mao, E. C. Dickey, F. Derbyshire, Chemical Physics
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April 5th (2008) 85-88.
[19] O. A. Nerushev, R. E. Morjan, D. I. Ostrovskii, M.
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(2), (2009) 215-218.
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76
Tp ch Khoa hc v Cng ngh 116 (2017) 072-075
Tm tt
Trong nghin cu ny xc nh kh nng khng vi khun ca tinh du v qu chanh (TDA), tinh du v
qu cam (TDB) v hn hp hai loi tinh du ny trn hai nhm vi khun Gram m Escherichia coli v Gram
dng Staphylococcus aureus. C hai loi tinh du u th hin tc dng c ch s pht trin ca chng
Escherichia coli vi ng knh vng trn khng khun l 39 2,8 mm (tinh du v qu chanh) v 32 1,5
mm (tinh du v qu cam). Vi chng Staphylococcus aureus, ng knh vng trn khng khun 43 3,5
mm (tinh du v qu chanh) v 37 1,4 mm (tinh du v qu cam). Nng c ch ti thiu (MIC) ca tinh
du v qu chanh trn c hai chng l 6,25 l/ml; tinh du v qu cam trn chng Escherichia coli: 6,25
l/ml v chng Staphylococcus aureus: 3,35 l/ml. Vi th tch tinh du v qu chanh s dng (0,1- 0,2
l/ml) v tinh du v qu cam (0,8-1,6 l/ml) cho kt qu cng hng mnh nht (FIC 0,5) trn c hai
chng vi khun Staphylococcus aureus v Escherichia coli. Bng phng php DPPH xc nh c kh
nng chng oxy ha ca hn hp tinh du v qu chanh v cam l 45,56 0,25%.
T kha: Hot tnh sinh hc, Hn hp, Tinh du v qu chanh, Tinh du v qu cam
Abstract
The aim of this study was to evaluate the antimicrobial activity of oils against food-related bacteria gram
negtive Escherichia coli and gram positive Staphylococcus aureus by using lime, orange peel oils in
individual and in mixture. Both tested oils showed effective inhibition against Escherichia coli with inhibition
zones of 39 2.8 mm (lime peel oil) and of 32 1.5 mm (orange peel oil). They also inhibited
Staphylococcus aureus with inhibition zones of 43 3.5 mm (lime peel oil) and of 37 1.4 mm (orange peel
oil). The minimum inhibitory concentrations (MIC) of lime peel oil against both tested strains were 6.25 l/ml;
orange peel oil on a strains of Escherichia coli: 6.25 l / ml and Staphylococcus aureus: 3.35 l / ml. With
volume of lime peel oil used (0.1- 0.2 l/ml) and orange peel oil (0.8-1.6 l/ml) for maximum resonance
results (FIC 0.5) on both strains of Staphylococcus aureus and of Escherichia coli. The antioxidant
activity was determined by using DPPH and it was 45.56 0.25%.
Keywords: Biological activity, Mixtures, Lime peel oil, Orange peel oil.
73
Tp ch Khoa hc v Cng ngh 116 (2017) 072-075
kim chng. Kh nng khng khun ca tinh du v du s dng (0,10- 0,20 l/ml vi tinh du v qu
qu chanh, vi ng knh vng trn khng khun chanh v t 0,80-1,60 l/ml vi tinh du v qu cam)
ca chng Escherichia coli l 39 2,8mm v chng s cho kt qu cng hng mnh nht (FIC 0,5).
Staphylococcus aureus l 43 3,5mm. Nng c Nh vy vic s dng hn hp tinh du v qu chanh
ch ti thiu ca tinh du v qu chanh trn c hai v cam c kh nng khng khun mnh trn chng vi
chng vi khun ny l 6,25l/ml. Kh nng khng khun Escherichia coli v Staphylococcus aureus hn
khun ca tinh du v qu cam, vi ng knh vng l khi s dng ring r tng loi tinh du. iu c
trn khng khun ca chng Escherichia coli l 32 ngha quan trng trong vic b sung hn hp tinh
1,5mm, nng c ch ti thiu 6,25l/ml, chng du ny vo thc phm; va c tc dng to mi
Staphylococcus aureus l 37 1,4 mm v nng c thm cho thc phm, c tc dng khng khun v bo
ch ti thiu 3,35l/ml. qun thc phm.
Bng 1. Kh nng khng khun ca tinh du v qu Bng 3. Nng c ch ring phn ca tinh du v
chanh v cam qu chanh v cam vi chng Staphylococcus aureus.
Tinh ng knh vng trn Nng c ch ti 1MICTDB 1/2MICTDB 1/4MICTDB 1/8MICTDB
du khng khun* (mm) thiu (MIC) ** (l/ml) **(6,25 (3,13l/ml) (1,6l/ml) (0,8l/ml)
Staphylococcus Escherichia Staphylococcus Cc gi tr l/ml) )
Escherichia coli aureus coli aureus
1MICTDA
TDA 39 2,8 43 3,5 6,25 6,25 2,51 1,54 1,34 1,16
(0,8l/ml)
TDB 32 1,5 37 1,4 6,25 3,35
1/2MICTDA
1,64 1,15 0,83 0,65
TDA: Tinh du v qu chanh, TDB: Tinh du v qu cam (0,39l/ml)
*ng knh vng trn khng khun th hin kh nng c 1/4MICTDA
1,46 0,92 0,64 0,58
ch vi khun ( 6mm: c kh nng khng khun). (0,2l/ml)
**Nng c ch ti thiu l gi tr trung bnh ca t nht 1/8MICTDA
ba ln th nghim lp li. 1,15 0,71 0,45 0,36
(0,1l/ml)
Bng 2. Nng c ch ring phn ca tinh du v **MIC: nng c ch ti thiu, FIC 0,5: Cng hng,
qu chanh v cam vi chng Escherichia coli 0,5 <FIC 1,0: cng hp, 1,0< FIC 4,0: khng tng
tc, 4,0 < FIC: i khng.
1MICTDB 1/2MICTDB 1/4MICTDB 1/8MICTDB
**(6,25 (3,13l/ml) (1,6l/ml) (0,8l/ml) Bng 4. Kh nng chng oxy ha ca hn hp tinh
Cc gi tr l/ml) du v qu chanh v cam
1MICTDA Mu th nghim Th tch (ml) % qut gc t
2,30 1,50 1,35 1,15
(6,25l/ml) do DPPH
1/2MICTDA TDA 0,10 41,25 0,12
1,60 1,10 0,85 0,68
(3,13l/ml) TDB 0,10 38,17 0,24
1/4MICTDA
1,35 0,85 0,80 0,41 Hn hp TDA v TDB 0,10 45,56 0,25
(1,6l/ml)
Vitamin E 0,10 43,38 0,17
1/8MICTDA
1,15 0,65 0,41 0,35
(0,8l/ml) 3.3. Kh nng chng oxy ha ca hn hp tinh
du v qu chanh v cam
3.2. Kh nng khng khun khi s dng hn hp Kh nng chng oxy ha ca hn hp tinh du
tinh du v qu chanh v cam v qu chanh v cam c xc nh theo phng
php qut gc t do DPPH, th nghim c tin
Tc dng cng hng, khi s dng hn hp hai hnh ti Trng i hc Cng nghip H Ni. Kt
loi tinh du v qu chanh v cam cc nng qu c trnh by bng 4.
khc nhau c nh gi bi ch s FIC, nng c
ch ring phn c xc nh bng phng php pha Kt qu nghin cu trong bng 4 cho thy hn
long lin tc hn hp hai loi tinh du ny trong mi hp tinh du v qu chanh v cam c kh nng
trng lng s dng phn 96 ging. Kt qu c chng oxy ha ln hn tinh du v qu chanh v
thnh by bng 2 v bng 3. cam khi s dng ring r. Tinh du v qu chanh v
cam khi s dng ring r, kh nng chng oxy ha
Kt qu nghin cu trong bng 2 v bng 3 cho nh hn vitamin E, nhng khi s dng kt hp hai
thy, nng 1/8 n 1/4 MIC vi mi loi tinh
74
Tp ch Khoa hc v Cng ngh 116 (2017) 072-075
loi tinh du ny th kh nng chng oxy ha li ln [3]. V Thu Trang, Lm Xun Thanh, Samira Sarter.
hn so vi vtamin E. Nghin cu hot tnh khng vi khun khi s dng kt
hp tinh du qu v mng tang. Tp ch Khoa hc v
4. Kt lun Cng ngh, tp 52 (5B) (2014) 417-422.
Kh nng khng khun ca tinh du v qu [4]. Gutierrez J., Barry-Ryan C., and Bourke P. The
chanh, vi ng knh vng trn khng khun ca antimicrobial efficacy of plant essential oil
chng Escherichia coli l 39 2,8mm v chng combinations and interactions with food ingredients.
Staphylococcus aureus l 43 3,5mm. Nng c International Journal of Food Microbiology, 124
(2008) 91-97.
ch ti thiu ca tinh du v qu chanh trn c hai
chng vi khun ny l 6,25l/ml. Kh nng khng [5]. Fei L., Liang H., Yuan Q. and Li C. In vitro
khun ca tinh du v qu cam, vi ng knh vng antimicrobial effects and mechanism of action of
trn khng khun ca chng Escherichia coli l 32 selected plant essential oil combinations against four
food-related microorganisms. Food Research
1,5mm, nng c ch ti thiu 6,25l/ml, chng
International 44 (2011) 3057-3064.
Staphylococcus aureus l 37 1,4 mm v nng c
ch ti thiu 3,35l/ml. Vi th tch tinh du v qu [6]. Molyneux P. The use of the stable free radical
chanh s dng (0,1- 0,2l/ml) v tinh du v qu cam diphenylpicryl-hydrazyl (DPPH) for estimating
(0,8-1,6l/ml) cho kt qu cng hng mnh nht antioxidant activity. Songklanakaric Journal of
Science Technology 26, (2004) 211- 219.
(FIC0,5) trn c hai chng vi khun
Staphylococcus aureus v Escherichia coli. Bng [7]. Matook S.M and Fumio H. Evaluation of the
phng php DPPH xc nh c kh nng antioxidant activity of extracts from buntan (Citrus
chng oxy ha ca hn hp tinh du v qu chanh v grandis Osbeck) fruit tissues. Food Chemistry 94
cam l 45,56 0,25%. (2006) 529-534.
75
Tp ch Khoa hc v Cng ngh 116 (2017) 076-081
Trng Hu Tr
Trng i hc Bch khoa - i hc Nng - 54 Nguyn Lng Bng - Lin Chiu - Nng
n Ta son: 25-4-2016; chp nhn ng: 20-12-2016
Tm tt
Vt liu graphene a lp (FLG) c nghin cu s dng trong nhiu lnh vc khc nhau trong hn thp
nin va qua nh vo nhng tnh cht u vit ca chng. nghin cu ny FLG c ch to t rut
bt ch bng phng php bc tch c hc v c ng dng lm cht mang cho ht nano palladium (Pd).
Xc tc Pd/FLG c nh gi cc c trng bng mt s phng php phn tch ha l hin i nh hp
ph - gii hp ph ng nhit nit v x l s liu theo l thuyt BET, knh hin vi in t qut (SEM), knh
hin vi in t truyn qua (TEM) v quang ph Raman. Kt qu ng dng xc tc cho phn ng hydro ha
cinnamaldehyde (CAL) thu c hydrocinnamaldehyde (HCAL) vi chn lc cao trn 94% khi
chuyn ha bng 80%. chn lc cao nghin cu ny c th n t hai l do khc nhau, trc ht l do
graphite ha cao ca cht mang FLG (IG/ID = 5,7), th hai c th do kch thc ca ht nano Pd mang
li.
T kha: FLG; Pd/FLG; Raman; SEM; TEM; hydro ha CAL.
Abstract
Few layer graphene (FLG) materials have been applied in different areas for over last decade thanks to their
novel properties. In this work, FLG was produced from pencil lead by mechemical exfoliation method, this
material was used as catalyst support for palladium (Pd) nanoparticles. Pd/FLG catalyst was characterised
by several techniques including nitrogen adsorption - desorption isotherms (BET), scanning electron
microscopy (SEM), transmission electron microscopy (TEM) and Raman spectrum. The catalyst was tested
for the selective hydrogenation of cinnamaldehyde (CAL) and the result showed a high selectivity towards
the C=C bond, over 94% of hydrocinnamaldehyde (HCAL) obtained at 80% of CAL conversion. The high
selectivity to HCAL in this work would be related to two different aspects, the first is the high graphitization
degrees of FLG (IG/ID = 5,7), the second is the particle size of Pd.
Keywords: FLG; Pd/FLG; Raman; SEM; TEM; Cinnamaldehyde hydrogenation.
76
Tp ch Khoa hc v Cng ngh 116 (2017) 076-081
ng ny thng c thc hin trn xc tc d th vi nhm Arai v cc cng s [13] cho thy chn lc
pha hot tnh l cc kim loi qu nh palladium (Pd), ca phn ng hydro ha CAL cn ph thuc vo
platinum (Pt), ruthenium (Ru) c phn tn trn cc dung mi s dng.
cht mang khc nhau [4-7], chn lc i vi
Qua phn tch kt qu ca nhng cng trnh
HCAL khi pha hot tnh l cc kim loi qu gim dn
c cng b cho thy chn lc i vi HCAL
theo th t Pd > Ru > Pt [8]. Nh vy Pd l pha hot
trong qu trnh hydro ha CAL ph thuc vo rt
tnh hiu qu nht c s dng khi mun thu nhn
nhiu yu t, trong cht mang cho xc tc c mt
HCAL vi chn lc cao. Trong thc t, vic s
vai tr rt quan trng. V vy, bi bo ny phn
dng Pd lm pha hot tnh cho phn ng hydro ha
tch v la chn vt liu graphene a lp (few layer
chn lc CAL nhm thu nhn HCAL c nghin
graphene: FLG) lm cht mang cho pha hot tnh l
cu bi nhiu nhm khc nhau, kt qu thu c cho
ht nano Pd trong phn ng hydro ha CAL nhm thu
thy chn lc i vi HCAL thay i trong mt
c HCAL c chn lc cao. Graphene a lp l
phm vi rt rng, t 20 n trn 90 % [1-2,7,9-12] ty
vt liu mi c nghin cu sn xut v ng dng
thuc vo xc tc s dng v iu kin tin hnh
trong hn mt thp nin qua nh vo nhng tnh cht
phn ng. Bng 1 trnh by kt qu ca cc nhm
u vit ca n nh dn in, dn nhit, bn c
nghin cu khc nhau cng b.
cao [14]. FLG l vt liu carbon nn chng kh tr v
So snh kt qu ca Li v cc cng s [9] vi mt ha hc do c th s dng lm cht mang cho
kt qu ca Liu v cc cng s [11] bng 1 cho xc tc trong mi trng acid hoc kim. Ngoi ra,
thy, khi s dng cng loi xc tc (Pd/CNTs) nhng y l vt liu khng c cc vi mao qun nn trnh
dung mi v iu kin tin hnh khng ging nhau c cc phn ng chuyn ha su to ra nhng sn
dn n chn lc i vi HCAL rt khc nhau, gi phm khng mong mun.
tr ny l 20% nghin cu ca Li so vi 90%
2. Thc nghim
nghin cu ca Liu. Trn cng loi xc tc l
Pd/SiO2, kt qu ca nhm Liu [1] thu c 81,6% 2.1. Graphene a lp - cht mang cho xc tc
HCAL trong khi nhm ca Mahmoud [7] ch thu
c 75% loi sn phm ny. Nghin cu v vi tr Cht mang cho pha hot tnh l FLG, nghin
ca cht mang xc tc trong phn ng hydro ha cu ny FLG c sn xut t rut bt ch (loi 9B)
bng phng php bc tch c hc, phng php ny
CAL, nhm nghin cu ca Liu [1] cho thy, trong
c xut bi C. Pham Huu [15]. Trc ht rut
cng iu kin tin hnh phn ng, dung mi v pha
bt ch c mi ln b mt tm thy tinh (c lm
hot tnh, th cht mang s c nh hng khng
t vt liu borosilicate) c b mt nhm nhm thu
nhng n hot tnh ca xc tc m cn nh hng c
n chn lc i vi HCAL. Ngoi ra kt qu ca c graphite vi s tm graphene t hn.
nhm Liu [1] cng nh kt qu nhm nghin cu ca
Bng 1. Kt qu nghin cu v chn lc i vi sn phm HCAL trong phn ng hydro ha CAL s dng Pd
lm pha hot tnh trn cc cht mang v dung mi khc nhau.
iu kin tin hnh phn ng chn lc
i vi Ti liu tham
Xc tc p sut H2
Dung mi Nhit ( C)
o
HCAL (%) kho
(MPa)
94 kt qu nghin
Pd/FLG dioxane 80 0,1 cu ny
Pd/SiC paraxylene 80 2 84 [1]
Pd/AC paraxylene 80 2 87 [1]
Pd/GO paraxylene 80 2 79,8 [1]
Pd/SiO2 paraxylene 80 2 81,6 [1]
Pd/-Al2O3 paraxylene 80 2 92,2 [1]
Pd/C(XC72) toluene 22 0,1 65 [2]
Pd/SiO2 - 25 0,3 75 [7]
Pd/CNTs ethanol 120 5 20 [9]
Pd/CNS isopropanol 60 1 36,4-65,3 [10]
Pd/CNTs trifluoroethanol+CO2 60 4 90 [11]
Pd/PPh3 ethanol 65 0,1 36-90 [12]
77
Tp ch Khoa hc v Cng ngh 116 (2017) 076-081
Qu trnh loi b cht kt dnh trong graphite bng nh chp knh hin vi in t truyn qua (TEM)
thu c sau giai on mi c thc hin theo trn my TOPCON 022-B UHR vi phn gii cao.
hai giai on, th nht l qu trnh x l bng acid
2.4. Hydro ha chn lc cinnamaldehyde
HCl (5M), nhm mc ch tch loi Al2O3, cn giai
on th hai l qu trnh x l bng NaOH (nng Thit b phn ng c s dng cho qu trnh
20%) tch loi SiO2. Phn thu c sau qu trnh hydro ha CAL l bnh cu 3 c c th tch 250 ml,
tch loi cht kt dnh c phn tn trong ethanol v mt c c s dng sc kh hydro vo trong mi
thc hin qu trnh bc tch bng sng siu m nhm trng phn ng, c th hai cho php thot kh hydro
gim s tm graphene trong graphite, sn phm thu khng tham gia phn ng ra ngoi, c th ba c s
c chnh l graphene a lp. dng ly mu ra ngoi phn tch thnh phn cc
cht trong hn hp. Thit b phn ng c gn vi
2.2. Tng hp xc tc Pd/FLG
thit b iu khin lu lng nhm iu khin lng
Tin cht ca pha hot tnh l mui palladium kh hydro a vo mi trng phn ng. Ngoi ra h
nitrate (Pd(NO3)2.6H2O) (Strem Chemicals), xc tc thng phn ng ny cn s dng thm h thng
Pd/FLG c tng hp bng phng php tm t v khuy t nhm mc ch lm tng kh nng khuch
hm lng pha hot tnh c c nh bng 5% khi tn kh hydro vo trong mi trng phn ng.
lng ca xc tc thu c. C th qu trnh tng hp
Mi th nghim c tin hnh vi 5 ml CAL
xc tc c tin hnh theo bn giai on nh sau:
(Sigma-Aldrich) c pha long vo trong 100 ml
- a pha hot tnh ln b mt cht mang: trc dioxane (Sigma-Aldrich), lng xc tc c c nh
ht mui palladium nitrate c ha tan trong dung 50 mg, kh hydro (Air Liquide) c sc vo mi
mi (nc), sau dng pipet a dung dch mui trng phn ng vi lu lng 60 ml/pht v qu
tm ln b mt cht mang, tip theo cht mang trnh c tin hnh nhit 80oC, vi tc
c tm dung dch mui c sy kh. Qu trnh khuy trn c duy tr bng 400 vng/pht. xc
ny c lp li hai ln bo m ton b b mt nh s thay i nng cc cht trong hn hp phn
cht mang c ph ng u tin cht ca pha hot ng theo thi gian, mu c ly ra nh k. Lng
tnh; mu c ly ra cho mi ln phn tch l 0,1ml v
c pha long trong 2 ml dioxane sau s dng
- Sy kh: sau giai on th nht, cht mang
micro pipet ly 1 l v np vo my phn tch sc
c tm mui c n nh trong khng kh 2 gi
k kh (loi Varian 3800) c trang b h thng
trc khi a vo sy kh 110C trong thi gian 2
detector ion ha ngn la.
gi;
Thnh phn cht phn ng, sn phm to thnh
- Nung: giai on ny c thc hin 250C
c xc nh da vo kt qu phn tch nng ca
trong 2 gi trong khng kh nhm chuyn mui sang
chng trong mi trng phn ng v tnh theo cng
dng oxide tng ng;
thc sau:
- Kh: giai on ny c thc hin 300C
A %
A 100 (1)
trong thi gian 2 gi trong dng kh H2 nhm chuyn CAL HCAL COL HCOL
oxide sang Pd kim loi.
Trong :
2.3. Phng php nh gi c tnh ca sn phm
A: nng ca cht phn ng [CAL], sn phm
Cht mang FLG cng nh xc tc Pd/FLG tng
[HCAL], [COL], [HCOL] (mmol/lt).
hp c nh gi cc c trng bng mt s
phng php phn tch ha l hin i nhm hiu r chn lc i vi mi loi sn phm s c
hn v bn cht ca cht mang v s phn tn cng nh ngha theo cng thc sau:
nh kch thc ca ht nano Pd. Cht mang FLG
c phn tch quang ph Raman trn my SelX %
X 100 (2)
RENISHAW nhm xc nh c trng v mc HCAL COL HCOL
graphite ha (mc ny c tnh bng t s IG/ID,
vi IG v ID l cng pic ti nh G v nh D) v Trong :
c trng v s lp graphene. B mt ring c xc Selx: chn lc i vi mt loi sn phm to
nh bng phng php hp ph - gii hp ph ng thnh (%);
nhit nit trn my Tristar 3000 v x l s liu bng
l thuyt Brunauer-Emmett-Teller (BET). Hnh thi [X]: nng ca sn phm [HCAL], [COL],
b mt xc tc c chp nh bng knh hin vi in [HCOL] to thnh (mmol/lt).
t qut (SEM) trn my JEOL 6700-FEG, cui cng chuyn ha c xc nh theo cng thc
kch thc pha hot tnh xc tc c nghin cu sau:
78
Tp ch Khoa hc v Cng ngh 116 (2017) 076-081
79
Tp ch Khoa hc v Cng ngh 116 (2017) 076-081
T th trn hnh 5 cho thy thnh phn ca oxide (GO) [1] cho thy cc cht mang ny c cha
cht phn ng CAL gim tuyn tnh theo thi gian. lin kt - trong mng li tinh th ca chng, khi
i vi cc sn phm to thnh th hm lng ca cc electron lin kt ny s chuyn dch n cc
chng tng dn theo thi gian, trong sn phm tm xc tc kim loi (metal particles) nn mt
hydro ha vo ni i C=C to HCAL chim phn electron s tng ln, kt qu lm tng kh nng
ch yu, (trn 94%); sn phm hydro ha vo ni i hp ph nhm chc aldehyde ln b mt xc tc, do
C=O to sn phm COL c thnh phn rt thp (di lm tng kh nng hydro ha ln ni i C=O
0,5%); sn phm hydro ha hon ton c hai ni i to COL, ni cch khc l cc cht mang va nu
to sn phm HCOL c thnh phn vo khong lm gim kh nng hydro ha ln ni i C=C to
6%. HCAL. Khc vi kt qu cc nhm va nu, nhm
ca Zhu v cc cng s [10] tin hnh nghin cu
nh hng ca xc tc l Pd c phn tn trn cc
cht mang l carbon nano tm (CNS) vi mc
graphite ha khc nhau. Kt qu nghin cu ca
nhm ny cho thy, khi mc graphite ha tng, gi
tr IG/ID thay i t 1,9 n 6,7 th chn lc i vi
HCAL cng tng ln tng ng t 36,4% n 65,3%.
FLG s dng nghin cu ny c mc graphite
ha cao (IG/ID = 5,7), y c th l l do dn n
Hnh 5. Thay i nng cc cht trong mi trng chn lc cao i vi sn phm HCAL trong phn ng
phn ng theo thi gian. hydro ha CAL nghin cu ny.
Da vo kt qu phn tch, chn lc i vi Ngoi l do va nu trn th kch thc ht xc
mi loi sn phm theo chuyn ha c tnh theo tc cng c th l l do quan trng khc nh hng
cng thc 2. Hnh 6 trnh by s thay i chn lc ln chn lc nh kt qu c cng b ca nhm
i vi cc sn phm theo chuyn ha. T th nghin cu Fu v cc cng s [19]. C th nhm tc
c th thy chn lc ca cc loi sn phm thay gi ny nghin cu chn lc i vi HCAL trn
i rt t theo chuyn ha. xc tc ca 1,5%Pd-WN/SBA-15. Kt qu cho thy
khi a thm wolfram nitride (tungsten nitride) vo
xc tc th kch thc trung bnh ca ht nano Pd thu
c nm khong 16,8 nm (kch thc ca ht nano
Pd thu c nghin cu ny cng gn tng t vi
gi tr va nu nh c nhn thy trn hnh 4 B), vi
kch thc ny th c hai lin kt C=C v C=O trong
phn t CAL s b hp ph ln trn b mt pha hot
tnh, trong trng hp qu trnh hydro ha vo ni
i C=C s xy ra d dng hn nn sn phm thu
c c chn lc i vi HCAL cao hn, kt qu
Hnh 6. Thay i chn lc cc cht trong mi
ny c trong cng b ca Bond [3] v Fu [19].
trng phn ng theo chuyn ha ca CAL.
4. Kt lun
Nh vy, so vi cc kt qu cng b c
cp n trong bng 1 th kt qu thu c nghin nghin cu ny ht nano Pd c phn tn
cu ny c chn lc i vi HCAL rt cao, c ng u ln b mt cht mang FLG bng phng
bit khi so snh vi cc kt qu ca cc nhm s php tm t. B mt ring BET ca xc tc Pd/FLG
dng cht mang trn c s ca vt liu carbon [1,9- tng ln gn 3,5 ln so vi cht mang FLG ban u.
12]. Khi s dng xc tc thu c cho phn ng hydro
ha CAL thu c HCAL vi chn lc cao,
Nh phn tch phn m u, trong phn
trn 94%. Kt qu nghin cu ny cng cho thy
ng hydro ha CAL th chn lc ln ni i C=C
mc graphite ha ca cht mang lm t vt liu
hay C=O ph thuc vo nhiu yu t khc nhau.
carbon hay kch thc ca ht xc tc l nhng yu t
Trc ht kt qu cng b ca Liu [1] cho thy loi
c th lm tng chn lc ny.
dung mi c cha nguyn t oxy (tetrahydrofuran)
khng lm tng chn lc i vi HCAL m ngc Ti liu tham kho
li cn lm gim nh chn lc ny. Cc nghin
[1]. Feng Jiang, Jian Cai, Bing Liu, Yuebing Xu and
cu v nh hng ca cht mang, c bit l cc cht Xiaohao Liu, Particle Size Effects in the Selective
mang n t vt liu carbon nh Hydrogenation of Cinnamaldehyde over Supported
triphenylphosphorine (PPh3) [12], carbon nano ng Palladium Catalysts, RSC Advances, Vol.6, (2016)
(CNTs) [9,11], than hot tnh (AC) [1] hay graphene p.75541-75551.
80
Tp ch Khoa hc v Cng ngh 116 (2017) 076-081
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Gurgul, Hydrogenation of cinnamaldehyde in the Wen Liu, Zhengping Hao, Jianliang Xiao, and Zhao-
presence of PdAu/C catalysts prepared by the reverse Tie Liu, Selective Hydrogenation of
water-in-oil microemulsion method, Applied Cinnamaldehyde over Pt and Pd Supported on
Catalysis A: General 487, (2014) p.1-15 Multiwalled Carbon Nanotubes in a CO2-Expanded
Alcoholic Medium, Ind. Eng. Chem.
[3]. G.C. Bond, Catalysis of Metals, Academic Press, Res.,Vol.51(34), (2012) p.11112-11121.
London, 1962.
[12]. Yuankui Zhang, Shijian Liao, Yun Xu, Daorong Yu,
[4]. Marjolein L. Toebes, T. Alexander Nijhuis, Jan Catalytic selective hydrogenation of cinnamaldehyde
Hjek, Johannes H. Bitter, A. Jos van Dillen,Dmitry to hydrocinnamaldehyde, Applied Catalysis A:
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