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J Braz. Soc. Mech. Sci. Eng.

DOI 10.1007/s40430-016-0617-4

TECHNICAL PAPER

Fabrication and thermomechanical characterization of a new


Cu–Al–Ni–Mn–Ti shape memory alloy bolt
G. D. Travassos1 · L. F. A. Rodrigues1 · C. J. de Araújo1   

Received: 1 March 2016 / Accepted: 27 July 2016


© The Brazilian Society of Mechanical Sciences and Engineering 2016

Abstract Industry experts in product innovation are properties, demonstrating a great capacity for strain recov-
always developing proposals and more effective solutions ery and energy dissipation by mechanical hysteresis.
appropriate to the needs of some high-tech industrial areas,
creating advanced technologies that increase the reliability Keywords  Superelasticity · Superelastic bolt · SMA
of systems used in these areas. In this context, advanced actuators · Smart materials
materials are frequently studied to obtain more reliability
in bolted joints, avoiding problems, such as leaks in pipe-
lines or constant maintenance. In this work, a novel super- 1 Introduction
elastic bolt was developed from a Cu–Al–Mn–Ni–Ti shape
memory alloy (SMA) to increase reliability in bolted con- Conventional bolts are largely used in many types of indus-
nections. The superelastic phenomenon presented by SMA trial structures and equipments. These mechanical compo-
allows full or partial recovery of large strains, between 4 nents may be submitted to cyclical or variable mechanical
and 8 % in tensile mode. This capability can be useful for loads (forces and torques) which can cause large plastic
the development of various industrial applications, espe- strains when its elastic limit is exceeded [1]. In addition,
cially in areas that require new high-technologies such the assembly and disassembly operations can lead to pre-
as aerospace, automotive, energy and oil and gas sectors. mature failure of bolts manufactured with conventional
Thus, this paper describes the fabrication and thermome- metallic materials. An alternative for this problem may be
chanical characterization of a superelastic bolt from a cop- the manufacture of new bolts from shape memory alloys
per based SMA. The selected Cu–Al–Mn–Ni–Ti superelas- (SMA), classified as smart material. These advanced met-
tic SMA was processed using plasma melting followed by als exhibit the superelasticity phenomenon and can recover
metal injection molding for minimizing bolt manufactur- large strains after loading and unloading [2–4]. Alterna-
ing machining steps. After the manufacture of the SMA tively, when its strain recover is blocked, these materials
bolt, it was carried out thermomechanical characterization can generate high forces by increasing temperature [5].
using DSC thermal analysis and reversible tensile test- Nowadays, there are two major classes of SMA: the Ni–
ing at increasing temperatures between 35 and 90 °C. The Ti alloy and its variants (Ni–Ti–Cu, Ni–Ti–Mo, Ni–Ti–Nb,
results show that the superelastic bolt has good mechanical etc.), and copper based alloys (Cu–Zn–Al, Cu–Al–Ni, Cu–
Al–Mn, Cu–Al–Be, etc.) [3, 6]. The Ni–Ti based SMA are
more expensive, but have the advantage of being biocom-
Technical Editor: Marcelo A. Savi.
patible, increasing applications in medicine and dentistry,
as well as general industrial applications (aerospace, auto-
* C. J. de Araújo motive, oil and gas, etc.) [7]. On the other hand, the copper
carlos.araujo@ufcg.edu.br based SMA are low cost, but can be fragile and thus dif-
1 ficult in applications.
Department of Mechanical Engineering, Universidade
Federal de Campina Grande, Rua Aprígio Veloso, 882, Among the copper based SMA, Cu–Al–Ni and Cu–Zn–Al
Campina Grande, PB 58429‑140, Brazil alloys are the most studied. In the polycrystalline state, the

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J Braz. Soc. Mech. Sci. Eng.

Fig. 1  Methodological
sequence used in the present Selection of the Superelastic
work Cu-based SMA

Design and Manufacture of


the Metallic Mold

Fabrication of the
Superelastic Bolt by PSPP

Mechanical Stabilization

Thermal Analysis Heat Treatment

Isothermal Uniaxial Tensile


Tests

Cu–Al–Ni SMA can be quite fragile, due to intergranular near room temperature (30 °C). Another important charac-
cracking (IGC) problems [6]. According to Gui et al. [8], IGC teristic for the choice of the SMA is that its production cost
problem can be circumvented by modifying the Cu–Al–Ni must be economically viable. Thus, a copper based SMA was
SMA, suggesting that the Cu–Al–Ni–Mn–Ti alloy can have selected, with nominal composition shown in Table 1. This
higher strength due to reduction in the grain size. Based on SMA was successfully used by Da Silva et al. [10] for manu-
this, Da Silva et al. [9] successfully tested a cylindrical con- facturing a cylindrical electrical connector. Compared to ter-
nector manufactured with the 79.4Cu–12.6Al–5.0Ni–2.0Mn– nary Cu–Al–Ni SMA, the addition of Mn and Ti reduces brit-
1.0Ti (wt%) SMA. This component was thermomechanically tleness and others problems related to intergranular cracking
cycled without presenting any problem of premature failure. commonly observed in these alloys [6, 8].
Mainly due to the property of superelasticity, SMA have
been considered for applications in bolted connections for 2.2 Fabrication of the SMA copper based superelastic
applications in civil engineering [10]. However, there are bolt
few experimental studies evaluating the development of
mechanical components such as bolts, nuts and washers, A stainless steel mold was designed taking as reference
particularly of copper based SMA [11–14]. from commercially available M6 bolt dimensions, with
In this context of technological advance based on the 40 mm in length (M6-1.0 × 40 DIN 931 CLASS 8.8, from
potential of SMA materials, this paper proposes the devel- Ciser Inc., Brazil). This is necessary because the Plasma
opment of a novel smart bolt, manufactured from a low Skull Push Pull (PSPP) process employed for manufactur-
cost ductile copper based SMA, allowing large recoverable ing the Cu–Al–Ni–Mn–Ti SMA superelastic bolt consist
strains. The Cu–Al–Ni–Mn–Ti SMA superelastic bolt was of melting by a rotating plasma arc torch followed by the
obtained by the Plasma Skull Push Pull (PSPP) process, injection of the melt into a mold [15]. Figure 2 show the
previously validated by De Araujo et al. [15] for the manu- sequence of PSPP process for this specific application.
facture of Cu–Al and Ni–Ti based SMA. Characterization For the manufacture of M6 superelastic bolt it was calcu-
by thermal analysis and stress–strain isothermal tests has lated that the mass of material needed to completely fill the
demonstrated the effectiveness of this new concept. mold, using the volume of the internal cavity of the mold
and the bulk density of the selected SMA.
Figure  2 summarizes all steps for obtaining the final
2 Experimental procedure product, from pure metals to the bolt from machining oper-
ations. The commercial pure constituents were cut (Fig. 2a)
The methodology used to develop the present work follows
the flowchart of Fig. 1.
Table 1  Nominal chemical composition of the selected copper based
SMA (wt%)
2.1 Selection of the superelastic SMA
Cu (%) Al (%) Ni (%) Mn (%) Ti (%)
The selection of the SMA was based on a suitable material for
79.4 12.6 5.0 2.0 1.0
manufacturing bolts with superelasticity effect at temperatures

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J Braz. Soc. Mech. Sci. Eng.

Fig. 2  Steps for obtaining the Cu–Al–Ni–Mn–Ti SMA superelastic bolt by the PSPP process

in proportions of Table 1. As previously described, to man- The phase transformation temperatures of the super-
ufacture the superelastic bolt it was chosen a plasma melt- elastic bolt were determined using a DSC apparatus from
ing process followed by injection into the metallic mold, as TA Instruments, model Q20. The sample was cut to about
shown in Fig. 2b–e. From this PSPP process is obtained a 47 mg and tested in the temperature range from −20 to
final product with the shape close to a M6 bolt, i.e., in the 80 °C, starting first from high to low temperature (cooling)
top a cylinder with diameter close to the head bolt and a followed by reversion (heating). The rate of heating and
lower cylinder with diameter and length corresponding to cooling was 5 °C/min.
the body of the bolt (Fig. 2e).
After the PSPP process (Fig. 2e), it is necessary to per- 2.4 Mechanical stabilization and isothermal uniaxial
form two machining operations. The first uses a hand tool tensile tests
to obtain the M6 threads of the bolt in the body part and
subsequently makes the head of the bolt, thus taking the The mechanical stabilization procedure consists of load-
hexagonal shape (Fig. 2f, g). These machining operations ing and unloading the superelastic M6 bolt for 50 times
do not affect the general characteristics of the phase trans- at a temperature in which the SMA is fully in austenitic
formation observed in this bolt. phase (90 °C). Figure 3 show the assembly employed for
that stabilization process and isothermal uniaxial tensile
2.3 Heat treatment and thermal analysis tests.
After mechanical stabilization with the structure shown
After the PSPP process and machining, the product was in Fig. 3a, isothermal stress–strain tests were carried out,
heat treated at a temperature of 850 °C for 15 min with starting from 35 °C with increments of 5 °C until a final
subsequent quenching in water. Then, some specimens temperature of 90 °C. For all tensile tests the maximum
from the bolt showed in Fig. 2f were taken to determine the strain was limited at 5 % with a strain rate of 1 %/min
transformation temperatures using Differential Scanning (corresponding to 1667 × 10−4 s−1) during loading and
Calorimetry (DSC). unloading.

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J Braz. Soc. Mech. Sci. Eng.

Fig. 3  Structure employed for mechanical stabilization and tensile tests at different temperatures. a Universal testing machine, Instron 5582. b
Detail of the assembly of M6 superelastic bolt in the heating chamber

3 Results and discussion

3.1 Transformation temperatures of the SMA bolt

The reversible phase transformation observed in SMA is


characterized by four characteristic temperatures: starting
temperature of martensite formation from austenite during
cooling (Ms) and finish temperature of this martensite for-
mation (Mf), and the starting temperature of austenite rever-
sion from martensite during heating (As) and the temperature
associated with the end of austenite reversion (Af) [2, 6].
The temperatures of the start and end of the phase trans-
formations during cooling and heating of the copper based
SMA were obtained by the tangent intersections in the
DSC peaks [2], as pointed out in Fig. 4.
As can be observed in Fig. 4, the SMA bolt becomes
fully in the austenite state, and consequently superelastic,
Fig. 4  Transformation temperatures of the Cu–Al–Ni–Mn–Ti SMA
after about 60 °C (above Af = 52.6 °C). From this tempera- used to manufacture the superelastic bolt
ture, the mechanical load applied to the bolt should induce
martensite by stress from austenite, leading to large revers-
ible strains during loading and unloading [2]. which present superelasticity as a well-defined plateau
stress in both, the loading and unloading path [2, 6]. From
3.2 Mechanical stabilization Fig.  5 it is observed that after about 10 cycles of loading
and unloading, the stress–strain behavior of the bolt tends
The cyclic stress–strain behavior of the SMA bolt in super- to stabilize due to accumulation of residual strain, which is
elastic regime (90 °C) is shown in Fig. 5. This behavior is approximately 0.7 % after 50 cycles. There is also a slight
approximately bi-linear during loading and almost linear decrease in maximum stress (at 5 % of strain), which also
during unloading, unlike is observed for most of the SMA, tends to stabilize at approximately 212 MPa with the cycles.

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J Braz. Soc. Mech. Sci. Eng.

220
Maximum Stress
200
180
160
140 Critical Stress

Stress (MPa)
120
100
80
60 in T = 90 °C
Stra T = 75 °C
40 u al
sid T = 60 °C
20 Re
T = 45 °C
0 T = 35 °C
0 1 2 3 4 5
Strain (%)

Fig. 6  Evolution of the stress–strain behavior of the superelastic


Fig. 5  Stress–strain behavior during 50 cycles of mechanical stabi- SMA bolt with increasing temperature
lization of the Cu–Al–Ni–Mn–Ti SMA bolt in superelastic regime
(T = 90 °C)

250
3.3 Isothermal uniaxial tensile behavior
200
Figure 6 shows the obtained stress–strain behaviors of the
Stress (MPa)

M6 SMA bolt for different test temperatures. In this figure 150


the main bolt thermomechanical parameters are defined:
critical stress to induce martensite from austenite, maxi- 100
mum stress during loading (at 5 %) and residual strain after
mechanical unloading. Qualitatively, it can be observed, a 50
gradual increase in the maximum stress and elastic mod-
ulus of the bolt with temperature. As expected, the super- 0
90
elastic recovery of the bolt increases gradually with tem- 80
Te

70 6
m

perature, tending to stabilize at about 5 % for temperatures 5


pe

60 4
higher than 60 °C. 3
ra

50 2
(%)
tu

Figure  7 shows a three-dimensional plot of the stress– 40 1 in


re

strain graphs for all temperatures at which the tests were 0 Stra
(°C

performed with the SMA superelastic bolt.


)

The thermomechanical parameters determined from


Fig. 7  Three-dimensional stress–strain graphs of the SMA superelas-
Fig. 6, as the residual strain, the maximum stress (at 5 % of
tic bolt with increasing test temperature
strain) and the critical stress to induce martensite at differ-
ent temperatures [16], are shown in Figs. 8 and 9.
Figure  8 confirms that for temperatures higher than where the stress increase slightly with temperature (about
55 °C the Cu–Al–Ni–Mn–Ti SMA bolt become fully super- 20 MPa from 55 to 90 °C).
elastic, with a residual strain tending to zero. Figure 10 shows the results of another important param-
From Fig. 9 it is possible to identify two regions of eter, the dissipated energy (in MJ/m3) that can be obtained
critical stress with different dσ/dT slopes. The first region, from internal area of the superelastic loops [2, 17] of Fig. 7.
between 35 and 50 °C allows extrapolate the Ms tempera- For an almost complete superelastic behavior, between 55
ture at zero stress. Comparing the extrapolated Ms (31.9 °C) and 90 °C, the dissipated energy are in the range of 1.45–
from Fig. 9 with the value obtained by DSC (34.3 °C) in 1.80 MJ/m3. These values are compatible with others pre-
Fig. 4, we can note a good agreement. Upon heating to the sented in the literature for copper based SMA [18, 19].
austenitic phase, for temperatures higher than 55 °C, the This hysteretic behavior associated with dissipation of
SMA bolt becomes more and more superelastic and the mechanical energy (Figs. 6, 10) may be used to mitigate
dσ/dT slope is strongly reduced, defining a second region mechanical vibrations [20], making the use of this type of

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J Braz. Soc. Mech. Sci. Eng.

1,6 2,2
Dissipated Energy
1,4 2,1

Dissipated Energy (MJ/m3)


2,0
Residual Strain (%)

1,2
1,9
1,0
1,8
0,8
1,7
0,6
1,6
0,4
1,5
0,2
1,4
0,0 30 40 50 60 70 80 90
30 40 50 60 70 80 90 Temperature (ºC)
Temperature (°C)
Fig. 10  Dissipated energy in the Cu–Al–Ni–Mn–Ti superelastic
Fig. 8  Residual strain as a function of test temperature after unload- SMA bolt as a function of test temperature
ing the Cu–Al–Ni–Mn–Ti superelastic bolt

for future commercial production due to its low cost and


220 easy manufacturing processes such as forging, machining
200 and rolling. Thus, it is possible to estimate that for large
180 scale production major changes are not required to existing
160 manufacturing lines in the industries of brass bolts.
The stress–strain hysteretic loops presented in this work
140
Stress (MPa)

show that the designed superelastic bolt has good mechani-


120
cal properties when compared with conventional bolts of
100 other metallic alloys, as yellow brass and bronzes. The
80 great advantage of this concept is demonstrated by the
60 Critical Stress recovery of large strains, of the order of 5 %, and dissipated
40 Maximum Stress energy as higher as 1.6 MJ/m3 at temperatures around
20 Ms=31,9 °C 60 °C.
0 There is a commercial feasibility of manufacturing the
30 40 50 60 70 80 90 superelastic bolt developed in this study, both for use in
Temperature (°C) specific applications of high technology but also by replac-
ing traditional bolts in many structures for dynamic appli-
cations, which can require these types of energy absorbing
Fig. 9  Maximum stress and critical stress as a function of tempera-
ture for loading the Cu–Al–Ni–Mn–Ti superelastic bolt elements.

Acknowledgments The authors thank the National Council for


Scientific and Technological Development (CNPq) Brazilian office
bolt can improve the dynamic performance of pipes sub-
for sponsoring the National Institute of Science and Technology
jected to temperature and variable mechanical loads. for Smart Structures in Engineering (INCT-EIE, Grant Number
574001/2008-5), UFCG-UFRJ-ITA Casadinho project (Grant Number
552199/2011-7), Universal 14/2012 (Grant Number 474524/2012-4),
CNPq-Petrobras Doctoral Scholarship (Grant Number 503082/2011-
4 Conclusions 2) and PQ 1D (Grant Number 304658/2014-6).

In this work a Cu–Al–Ni–Mn–Ti SMA was studied for


the development of smart fasteners, such as new bolts, due
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