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Quartz crystal monitoring in the production of dielectric multilayer stacks is compared to optical
monitoring. The stacks are calculated with the aid of an optimizing program. This yields optical
thicknesses of the layers differing from multiples of a quarter of the wavelength. Optical monitoring
is complicated in this case. Using quartz crystal monitoring, planning and execution of the process
is easier and yields stacks with satisfactory reflectance characteristics faster than with
optical monitoring.
The reproducibility of the optical thickness of MgF2 layers is investigated. In general, both
methods turn out to be equivalent in performance.
1. Introduction is fixed to the domed calotte, in a position with the same distance
to the centre of the bell jar and on the same height as the regular
Optical thin dielectric film stacks, fabricated in the Delft
substrates. Using a shutter before the test substrates, we can
University Optical G r o u p (e.g. broad band mirrors, high- and
control the exposition during evaporation independently.
low-pass filters, anti-reflectance coatings, etc.), are usually
The test substrates are used for measurement of the obtained
optimized with the aid of a specially designed computer
refractive indices after the process following the A b e l s method2
program. This optimization is performed by varying the layer
The changer can contain six test substrates.
thicknesses keeping the refractive indices fixed on experiment-
Furthermore, we used a Beckman spectrophotometer DB--GT
ally determined values.
for determination of the reflectance and transmittance of the
This design process yields stacks whose layers, in general,
stack afterwards.
have optical thicknesses differing from exact multiples of a
quarter of the wavelength. F o r monitoring t the evaporation
process of these stacks an optical method or a quartz crystal 3. The evolution o f a thin film stack
monitor can be used. The aim of this paper is to give some
In Figure 1 the evolution of a stack is sketched; our discussions
practical information on the use of quartz crystal monitoring.
will follow this diagram.
After information about the equipment used, we discuss
Figure 1 showing the processes leading to a multilayer stack
satisfying preset specifications. Finally, we consider the repro-
ducibility of the optical thickness of MgF~ layers. Optical and A SpeclflCOtlOnSRa
()~)
quartz crystal monitoring are compared. Toleronces
1
Inltlol stock
2. The equipment used B '{t},{n,(X)~,R,(X}
h. ~ die proidem. We shall consider the problems related C. Optimizing of the stuck. The discussion of the optimizing
to producing broadband anti-reflection coatings, low- and high- program is beyond the scope of this paper. Important is,
pass filters, broadband laser mirrors, etc., all composed of that it leads to stacks consisting of layers with optical thick-
dielectric layers and in general for use at visible wavelength. In nesses that, in general, differ from multiples of a quarter of a
our optimizing program the desired reflectance Rd(,~), where ,~ wavelength. This fact influences the choice of the monitoring
is the wavelength, must be specified as an ideal curve (consisting method. The so-called turning value method a' 1o., t which is in
of a set of straight lines in the various wavelength regions that use for ¼,~stacks, cannot be used in our case.
must be specified by the user) plus bands of constant widths Another optical method, ~ in which deposition is terminated
around it in which deviations of the ideal curve can be tolerated. after (if possible) or before (to avoid) a turning value is reached
The number and positions of the wavelength regions, the place can he applied. However, as will be discussed later, this method
of the straight lines and the width of each of the tolerance re- shows certain disadvantages in comparison with quartz crystal
gions can be freely chosen. An example, relating to a low-pass monitoring.
filter, is given in Figure 3. The computer input in this example Another feature of the program is, that it determines the
derivatives of the reflectanceRo (,~), viz. ~Rslc94, where Rs is the
reflectance in thejth extremum and t~ is the thickness of the kth
Aalustoble fo layer. They are used for finding the layers, for which errors in
stondor(;Iolcallotot: t ] thickness have serious consequences for the total reflectance of
the stack and also for the calculation of deviations in the
- f~-fo IFrequenc¥meter
+
o TJOz Itao~
i~i/ 8 I-0.P98 -0199 0097 -0.0o,2 "0.489
SiO~ F~ tk~0481"t 0142 "O.~f.,)5-0018 0 t94 /
\
0003-0534 -0639 -0115- C.%64//
L\\\\",~IT,\" {3K?'
I l
Figure 4. Example of the matrix of derivatives ~Rs/~tk (dimension
Wav2lenoth ~,m - t) of an anti-reflectance coating. The refractive indices of TiO2
3. Example of the specification of the reflectan~ ,%. and SiO, are given in Figure 10. The thicknesses of the layers
tt . . . t., are 94.7, 107.1, 22.7 and 15.2 nm, respectively.
where
B. The initial stack. Our program optimizes by varying the
layer thickness (starting from an initial stack) until the reflec- Cs is the frequency factor, depending only on the oscillating
tance of the stack is brought completely (if possible) within the frequency f~ of the crystal,
given tolerance bands. The used initial stack is often derived Cp is the position factor, depending only on the relative
from systems d.,~.ocrihed in the literature. The initial stack is positions of the crystal to vapour source and substrate and
supplied to the program by giving the refractive indices {n~(,~)} C,, is the material factor, depending only on the material of
of the layers and their starting thicknesses {4 :. Dispersion is
the layer.
taken into account. The refractive indices are obtained from
previous experiments by which layers, with optical thickn~ses The factor C / i s introduced since, afte: use in several measure-
of about ¼k, are deposited on test substrates. The conditions merits, the mass loading of the crystal is increased considerably,
(such as: the composition of residual gas, the bell jar pressure, and then the assumption of a linear relationship between mass
the substrat¢ temperature and the rate of evaporation) under and frequency is no longer valid for the total range in which the
which the layer is deposited, have to be accurately described to frequency is decreased. For a single layer, however, we still can
make reproduction possible. use this relationship provided that C s is related to the total
392
C J vd Laan and H J Frankena: Monitoring of optical thin films using a quartz crystal monitor
,,00 ,/
,050
C, Source
Figure 6. Position of crystal, rotating substrate and directed surface
source. For the BA 510 equipment, we have hc = 514 nm, Re = 188
,000
ram, h = 464 mm, R = 165 mm and p = 91 mm which gives Cp =
"i
0.842.
1 , I , I , l , . I ,
0 2C "~0 60 80 tOO
393
C J vd Laan and H J Frankana: Monitoring of optical thin films using a quartz crystal monitor
!-
~l !2_0 I L I [
tor glass, which interference filters must be used and what i I
refractive indices the materials used will have in vacuum. gJ I I
I I
Much skill is necessary in meeting these problems, since the I !
I
performance of the resulting stack will strongly depend on the t t, t,; L, t5 t6 t~
way in which the process is planned. If we compare this with
t3
the plan using quartz crystal monitoring, the simplicity of the T~me
latter method is obvious; the calculations can be carried out
Figure 7. Recorder sheet obtained from deposition of a quartz crystal
with the aid of a pocket calculator and not much experience is monitored layer (Xf = 800 Hz). The slope of the lines a is calculated
required. and the lines are drawn on the sheet before deposition of the layer.
394
C J vd Laan and H J Frankena: Monitoring of optical thin films using a quartz crystal monitor
In the latter case, the new refractive indices are supplied to the I O~J
program and the cycle restarts (Figure 1). If the refractive
indices are correct, the thicknesses o f the layers must differ from
the calculated values. Supposing that the deviations of the
reflectance are known accurately enough, the differing layers
can be detected from the matrix ~Rj/~t,. F o r small deviations,
however, the (unavoidable) absorbtions and inhomogenities
become important and the previous method is not applicable. T 050
In general, for incorrect layers ORj]~& is relatively high;
assuming this, a trial-and-error method can be used. If the
source of the failure cannot be found in this way, the previous
process is repeated; in many cases this second run leads to a
more satisfactory result.
ooo ~, v I I I
Comparingoptical monitoring with quartz crystal monitoring. 4oo 5oo 6oo 7oo 8oo
Not much difference exists in the error detection using optical ~j Ilm
or quartz crystal monitoring. However, there is a difference in Figure 9. Transmittance curve of a high-pass filter. The dotted line
the way in which errors in previous layers influence the errors gives the calculated transmittance, the solid line the measured
in later layers. In the case of optical monitoring, normally transmittance after the first process.
more than one layer is put on the same monitor glass in order to
avoid influences of the difference in sticking properties between The materials and the calculated thicknesses are given in
the substrate and the monitor glass. Now, an error in the Table 2. The refractive indices of the used materials as a func-
terminating point of a foregoing layer also changes the reflec- tion of the wavelength are depicted in Figure 10.
tance at the point where the calculated thickness of the next
layer is reached (Figure 8). It is not possible to correct this
Table 2. Materials and calculated thicknesses of the high-pass filter
Colculatecl
of Figure 9.
i 1
1_ ( n. t r)co, (n2t2}col _ I Thickness
_ iL _
Material nm
l
=-~ (n! "~l)ob, f= Obto,nea
BK7
TiO2
SiO2
TiO2
SiOz
36.3
70.8
48.3
82.2
TiO2 46.0
SiO2 76.3
TiOz 46.8
SiO, 83.3
TiO2 46.8
SiO2 64.3
TiO2 36.7
"SiO2 84.1
~V~L...I_ Air
KePt c o n s t o n * l
395
C J vd Laan and H J Frankena: Monitoring of optical thin films using a quartz crystal monitor
2 7,:: m
monitoring, the terminating point was chosen such that the best
accuracy was obtained. Now we, calculate the relative deviation
as a function of the optical thickness, assuming that in both
2 5C
methods the absolute error in the terminating point of the
monitoring signals will remain constant. The optical monitoring
2 30 signal is approximated by
R = a cos(4~) + b, (7)
q~ = n x = c o n s t a n t x nt, (8)
~?/<nt>
with 10 comparable optically monitored layers. The used
material was MgF2 and the optical thickness of all layers w a s
= + ''= (lO)
about 430 nm. Optical monitoring was performed at such a where
wavelength ,X,. that the evaporation process terminated at P = 2AR/(na). (11)
5A,,,/8 (Figure 11). The frequency shift Af using quartz crystal
The absolute values in equation 10 originate from the fact
that AR must be positive in the minima and negative in the
(0) ~.m/2 (b)
maxima. From the experimentally determined point x = 5/2,
Z\
I
ffT/<nt> = 0.0050 follows P = 0.025, after which the curve can
5hm/8 be computed to other values o f x and nt (see equation 8).
Xm/4 In the case of quartz crystal monitoring the relation
~ t / ( n t ) = 0.0054 x 430/(nt) (12)
I holds (Table 3).
Time .... -~ T~me -. ~
R point
monitoring was 3700 Hz. In both cases the deposition con-
ditions were carefully controlled by skilled operators. After the
processes the transmittances were measured. From the mutual
, Ill I ,
I l X, I I I I
shift of their curves the mean optical thickness nt~ and the 0 I0(, pQ.(, ~,"' 4~." ~} 500 600
standard deviation ~ defined as AI, IR;n
monitoring.
396
C J vd Laan and H J Frankena: Monitoring of optical thin films using a quartz crystal monitor
For both cases, the graphs are given in Figure 12b. From reflectance characteristic from the calculated curve, and
that, we conclude, that in the case of MgF2 layers, quartz consequently, quartz crystal monitoring yields stacks with
crystal monitoring is in general as good as optical monitoring satisfactory performance faster than optical monitoring.
and for layers with optical thicknesses smaller than A~,/8, quartz Concerning the reproducibility of the optical thickness of
crystal monitoring is more accurate than optical monitoring. M g F , layers, the performance is comparable to that of
Experiments with materials of higher refractive index (ZnS and optical monitoring. For layers with optical thickness smaller
TiO2) will be carried out in the near future. than ,~m/8, quartz crystal monitoring is more accurate.
397