EXPERIMENTAL Various samples of ZnS were obtained for study as detailed in Table 1, including different suppliers of standard CVD ZnS made from hydrogen sulfide gas and zinc vapor, lega
Trang 1Variability in Chemical Vapor Deposited Zinc Sulfide: Assessment of
Legacy and International CVD ZnS Materials
John McCloy,*a Ralph Korensteinb
a Raytheon Missile Systems, 1151 E Hermans Road, Tucson, AZ, USA 85734
b Raytheon Company, 350 Lowell Street, Andover, MA, USA 01810
ABSTRACT
Samples of CVD ZnS from the United States, Germany, Israel, and China were evaluated using x-ray diffraction, transmission and Raman spectroscopy, and biaxial flexure testing Visible and near-infrared scattering, 6 μm absorption, and ultraviolet cut-on edge varied substantially in tested materials Transmission cut-on (ultraviolet edge) blue-shifts with annealing and correlates with visible color but not the 6 μm absorption Raman scattering for CVD ZnS, presented here for the first time, was similar for all ZnS tested Crystallographic hexagonality and texture was determined and correlated qualitatively with optical scattering All CVD ZnS tested with biaxial flexure exhibit similar fracture strength values and Weibull moduli This survey suggests that despite over 30 years of production as an infrared window, the optical properties of CVD ZnS and their variability still defy easy explanation
Keywords: Zinc sulfide, chemical vapor deposition, IR window
1 INTRODUCTION
Chemical vapor deposited (CVD) zinc sulfide has been an indispensable infrared window material since its introduction
in the early 1970s by Raytheon.1 Development of ZnS internationally has been recently documented2 but a comparison
of properties among various producers has not been previously available Samples of CVD ZnS, Hot isostatic pressed CVD ZnS (multispectral), some legacy experimental Raytheon grades (red ZnS and elemental ZnS), legacy hot-pressed ZnS, and single crystal melt-grown ZnS were obtained from various suppliers Transmission was investigated to study scattering, absorption, and color Several samples of red ZnS were annealed at various temperatures to investigate the phenomenon of coloration in ZnS X-ray diffraction (XRD) studies were used to quantitatively measure hexagonality and crystallographic texture and investigate its relation to optical transmission Finally, biaxial flexure testing was performed, generating data sets for red ZnS and elemental ZnS not previously available
2 EXPERIMENTAL
Various samples of ZnS were obtained for study as detailed in Table 1, including different suppliers of standard CVD ZnS (made from hydrogen sulfide gas and zinc vapor), legacy Raytheon elemental ZnS (made from hydrogen gas, sulfur, and zinc vapor3), legacy Raytheon red ZnS (grown ~600 °C with large excess of Zn reactant,4 and multi-spectral ZnS (CVD ZnS which has been hot-isostatic pressed in the presence of platinum metal) Single crystal Bridgeman grown crystals of ZnS and legacy hot-pressed ZnS from powder precursors were also studied
Crystal structure was investigated using a Rigaku Geigerflex II x-ray diffractometer (XRD) fitted with a CuKα x-ray source, a diffracted beam monochrometer, and a sodium iodide scintillation detector Diffracted intensity of polycrystalline samples was recorded for 2θ angles from 20 to 100º in 0.05º increments Some samples were ground in
an agate bowl, and powder patterns were taken of the region between 25 and 35º with 0.02º resolution to further investigate the characteristic region of ZnS polytypes
* Present address: Battelle Pacific Northwest National Laboratory, john.mccloy@pnl.gov
Trang 2Transmission of polished samples was investigated in the ultraviolet through near-infrared (175 – 3300 nm) on a Varian Cary 5000 spectrophotometer, and data was recorded at 1 nm wavelength increments Infrared transmission (2 – 20 μm) was measured using a Fourier transform infrared spectrometer, Bruker Equinox 55 FTIR, with a deuterated triglycine sulfate (DTGS) detector using a spectral resolution of 4 cm-1 and signal averaging over 80 scans
Raman spectroscopy was performed using a Thermo-Nicolet Almega XR single beam dispersive spectrometer with a holographic notch filter to block the 532 nm laser excitation beam Samples were placed under the 10x objective of the confocal microscope Spectral resolution was 2.2 – 2.5 cm-1 with the high resolution grating, 25 μm slit, and 79 to 1290
cm-1 spectral range Laser power was 13% and spectra were averaged over 32 scans A few ZnS samples were also surveyed with the low resolution grating out to 4248 cm-1, with spectral resolution 6.4 – 10.5 cm-1
Biaxial flexure strength testing was performed in accordance with ASTM C1499.5 The characteristic diameters were as follows: 10.67 mm (load ring), 20.32 mm (support ring), and 25.4 mm (sample) Sample thickness was 1.9 to 2.0 mm All samples had the CVD growth axis perpendicular to the plane of the large area of the sample which was placed under stress Various samples were tested, with some datasets having more data points than others due to sample availability All sample surfaces were polished using a controlled grind procedure to minimize the effects of the surface flaw population differences, using successive steps of grinding and polishing with smaller grits
Nomenclature Material type Supplier Country of
Origin Notes
PS Standard CVD Princeton Scientific
very Zn rich reactant;
eZnS CVD
Chinese CVD
(H2 + S + Zn) Research institute synthetic crystals China See Reference
6
PS msZnS CVD + (Pt?) HIP Princeton Scientific
(US) importer Germany “multispectral ZnS”
PS HH CVD + (Pt?) HIP Princeton Scientific
(US) importer
Germany special short HIP
(unknown details)
Vitron HH CVD + HIP (no Pt) Vitron Germany “special clear grade”
Rafael msZnS CVD + HIP (no Pt) Rafael Israel “multispectral ZnS”
3 RESULTS
3.1 Atomic structure
Diffraction patterns of polycrystalline samples were taken from 2θ angles 20 – 100° Some of these are shown normalized to their maximum peak in Figure 1a Generally, the texture of as-deposited CVD samples including eZnS is
Table 1: ZnS samples investigated; all polycrystalline unless otherwise noted
Trang 34O
msZnS
IRTRAN
'isotropic' (randomly oriented)
Various CVD ZnS eZnS
(100) texture (°)
30 S x
0
20
10%
o
0.06-0
E
0 z
0.1
0.08
0.04
0.02
-0
20
066)
00
0
6
H
1
9
1
Sd
S
6 9-i
/
(0)
9
S
8
-
H ((9)
660)
06t6)
(000) 666) ((C)
:6
(006)
OOI
06
06
OL
09
09
06
06
IRTRArJ2 26% 6
predominantly {100} while that of HIPped samples is predominantly{111}, presumably due to plastic deformation and recrystallization Nucleation and growth rates are highest on “atomically rough” planes which have higher densities of kinks and steps, like{ 100 }planes, and would be expected to dominate as-deposited materials,7 though it should be noted that RedZnS had a significantly higher fraction of {111} A quantitative analysis of the texture was performed using the scattered intensities for textured planes (hkl) in the polycrystalline sample (txt superscript), calculated as8
( txt / txt) ( / iso/ iso)
In an isotropic polycrystalline sample fhkl=1 for all (hkl) planes The larger the value, the larger the volume fraction
of{hkl }planes orientated in the Bragg diffraction position The powder pattern for cubic ZnS #05-0566 was used as the “isotropic” sample (iso superscript) Furthermore, the %{111} and %{100} was calculated as follows (Figure 1b):
,
1.60 1.46
6.18
msZnS
hkl msZnS
f
Lattice parameter measurements were made, using a NIST traceable alumina standard internal to the instrument, using the alumina (0.2.10) plane reflection (expected at 2θ = 88.995° and measured at 89.02°) to perform the angular correction Diffracted intensity was measured from 87.7 to 89.3° for ZnS at 0.02° intervals with 5 second integration time The sphalerite (422) reflection, measured at 2θ = 88.4 to 88.6°, was corrected by the standard, then used to calculate the interplanar spacing (dhkl) and the cubic lattice parameter.9 The estimated accuracy of lattice constant measurements is better than ±0.001 Å Measured lattice parameters are shown in Figure 1c
Figure 1 X-ray diffraction data for ZnS samples; (a, UL) normalized polycrystalline diffraction data; (b, UR) quantification of textures, with various CVD ZnS samples in dotted box; (c, LL) hexagonality, calculated
extinction, and lattice parameter; (d, LR) XRD powder pattern from which hexagonality data was calculated
a)
d) c)
b)
Trang 4A simple measure of the hexagonality in polycrystalline ZnS powders and hot-pressed compacts has been proposed using the ratios of characteristic peaks in the wurtzite and sphalerite XRD spectra.10-12 The atomic fraction of hexagonal stacking (hexagonality) can be calculated as
(0002) (111) 28.53
(0002) (111) (10 10)
1.84 1
I
+
where w is the 2H hexagonal phase (wurtzite), s is the 3C cubic phase (sphalerite), the subscripts are 2θ angles, and the superscripts are the characteristic planes, since the 2H(0002) and the 3C(111) overlap at 2θ=28.53° Intensity values were obtained using the peak height of the higher resolution, smaller angular range data Representative data is shown
in Figure 1c and 1d for HIPped ZnS (msZnS, similar spectra for all HIPped samples in this study), eZnS (similar spectra for Chinese and red), CVD ZnS (Raytran, similar for all standard CVD samples in this study), and Bridgeman melt-grown crystal Note the extra peaks (~29.6˚ and 30.1˚) for the Bridgeman crystal, which can be most closely indexed by assuming a 72R polytype structure (even though the crystals were sold as 3C pure cubic crystals)
3.2 Optical properties
Composite spectra of FTIR and UV-VIS transmission measurements for various samples are shown in Figure 2 Sample thicknesses, UV edge (defined as the last spectrometer data point on the short wavelength edge of the transparency window before a negative transmission value was recorded), and transmission and calculated extinction for various wavelengths and samples are shown in Table 2 Extinction is calculated from measured transmission as:
(1/ )*ln (1 ) / 22 2 (1 ) / 44 2
where β is the extinction coefficient (in cm-1), L is the sample thickness, T is the measured transmittance, and R is the single surface reflectivity in air calculated from the index of refraction (from the Sellmeier equation for CVD ZnS3)
Thickness
(mm) UV edge (nm) T1.064/ α1.064 T3.39/ α3.39 T6.0/ α6.0 T10.6/ α10.6
n = 2.288 n = 2.255 n = 2.240 n = 2.192 Theoretical (no
Raytheon Elemental 4.64 386 55.3% / 0.59 72.9% / 0.03 59.6% / 0.46 68.7% / 0.14 Raytheon Red 3.18 400 67.0% / 0.27 72.2% / 0.08 48.1% / 1.33 67.9% / 0.32 Chinese 4.62 386 62.1% / 0.35 71.8% / 0.07 73.1% / 0.04 68.4% / 0.21 Vitron FLIR 2.00 380 28.7% / 4.59 68.5% / 0.38 62.8% / 0.82 72.5% / 0.20 Rohm & Haas 4.64 382 16.9% / 3.11 56.9% / 0.55 60.8% / 0.42 68.4% / 0.21 Rafael CVD 2.49 361 50.9% / 1.42 65.9% / 0.45 70.4% / 0.22 70.8% / 0.25 II-VI Infrared 4.89 383 26.8% / 2.02 61.0% / 0.38 60.9% / 0.40 64.8% / 0.30 Princeton Scientific
FLIR
5.13 390 8.4% / 4.18 54.3% / 0.59 50.9% / 0.72 64.7% / 0.29 Kodak IRTRAN2 6.39 445 1.1% / 6.54 63.3% / 0.24 71.3% / 0.06 60.5% / 0.34 Raytheon
Multispectral 4.64 344 72.0% / 0.04 73.6% / 0.01 74.4% / <0.01 69.2% / 0.18 Bridgeman single
crystal 1.00 340 73.1% / 0.04 72.8% / 0.17 73.2% / 0.16 73.3% / 0.29
Table 2: Measured transmittance, UV edge, and calculated extinction (cm -1 ) at key wavelengths; 1.064,
3.39, and 10.6 μm are laser wavelengths and 6 μm gives an indication of the zinc hydride absorption
Errors on the calculated extinction are larger for thinner samples
Trang 56 6 10 12 14 16
WaveIegth (icro)
60
60
C
0
.8 40
E
=
20
60
WaveIegth (ioror)
60
C
0
E
=
20
650C24h 650C2h treatmentNo /
I if i,'
Wavelength (nanometers)
0.8
-0.6
(0
E
0.4
-C,
I0.2
Wavelength (microns)
A series of samples of red ZnS were subjected to vacuum anneal treatments from 650 to 850 °C in a Seco/Warwick furnace It was initially assumed that annealing would enable hydrogen release13 and show a change in the characteristic 6 μm absorption Since red ZnS had the strongest and most well-defined absorption here, it seemed the right candidate to explore Secondly, there was some anecdotal evidence that red ZnS visible transmission changed differently under annealing conditions than CVD ZnS did There was a desire to explore this aspect as well, since red ZnS had the longest wavelength ultraviolet edge of any of the samples tested
Typical thicknesses of untreated standard yellow CVD ZnS had a UV edge of 382 nm which blue-shifted to 343-344 nm when annealed (in vacuum at 850 °C for 24 hours) or HIPped In contrast to HIPing, annealing of CVD ZnS in general produced markedly more scattering in the visible and near-infrared, despite blue-shifting band edge This ultraviolet transmission improvement with heat treatment is believed to be due to the removal of band gap electronic defects involving impurities of oxygen14 and/ or hydrogen.13
Figure 3 shows a summary of the transmission measurements for these annealing experiments along with photographs
of some of the samples before and after the heat treatment Starting samples were all approximately 3.175 mm thick One sample was subjected to a 650 °C anneal for successively small amounts of time, first 2 hours, and then an additional 4 hours for a total of 6 hours After the first 2 hours, very little if any change was evident in the infrared but the UV band edge blue-shifted slightly The apparently slightly higher long-wave transmission in this sample is due to
Figure 3: (a,L) UV-VIS edge of Red ZnS annealing experiments; (b,R) IR transmission of annealed Red
Figure 2: Transmission graphs for some of the measured ZnS samples, thicknesses as in Table 1 (1)
Ray msZnS, (2) RedZnS, (3) eZnS, (4) Rohm & Haas, (5) IRTRAN, (6) Chinese, (7) T max , which is the
calculated transmission (from refractive index) with only reflection losses (Ref 3)
a) b)
Trang 600 0 0 -J 0 0) (0 0 0 0 (0 a 0, 0 0
61: 2 LqQ() 642 LO(L)4-TO(L) 619 210(X) 446: L0(L)TA(L)
425: L(X)TQ() 400: T0(X)-C-TAQ()
-181: 2TAQ() 145: 2TA(L) 97: aflidentifled
Figure 4: Raman scattering data in CVD ZnS
slight tilt or wedge After the next 4 hours of annealing, again there was very little change in the infrared with the 6 μm absorption remaining deep, sharp, and two pronged, with no significant spectral or intensity change Visible transmission degraded and the band edge further blue-shifted Another red sample was subjected to high temperature for a short time, 850 °C for 2 hours, resulting in a complete elimination of the 6 μm absorption, a large scattering from the visible through the infrared, and a band edge blue-shift despite strong scattering
The most striking change in these samples was their change in visual appearance (color and transparency) Samples with a reddish hue have band edges around 400 to 420 nm, absorbing the violet most strongly and hence appearing red
By way of comparison, standard ZnS which is yellowish typically has a band edge of around 375 nm which transmits all the visible to some extent but transmission in the violet is low In the latter case described (850 °C anneal), the reddish-yellow color was eliminated and the sample became whitish yellow and highly scattering In the other case (650 °C anneal), the first 2 hour anneal changed the sample from reddish to orangish, with the edges of the disk being more effected than the bulk The subsequent 4 hour anneal changed the sample to a colorless material which was still fairly low scatter despite the reduced transmission from the band edge to about 3 μm This is interesting since the color
in the sample is gone but the 6 μm absorption generally associated with zinc hydride remains Most authors have
claimed an intimate relationship between the hydride absorption and the color of ZnS (e.g Lewis et al.13) An etched microstructure was taken of the 650 °C sample after 6 hours annealing which revealed no recrystallization and minimal
if any grain size coarsening
Raman scattering was also performed on the samples
as no data was available in the literature on Raman of CVD ZnS Almost all the samples were indistinguishable in the Raman spectrum from 85 to
1290 cm-1 The main peaks were indexed using a combination of sources.15, 16 Given the similarity of most of the Raman spectra, only a few representative ones are shown in Figure 4 A few minor differences among ZnS samples were noted Red ZnS showed an unidentified peak at 97 cm-1 which was present in no other samples except possibly one of spectra taken of the Bridgman crystal The annealed red ZnS sample
no longer showed this peak and looked more like the other ZnS samples at the low wave number shifts Raytheon multispectral ZnS had a weak broad band centered at 1098 cm-1 which was not evident in other ZnS samples
3.3 Biaxial flexure testing
Seven sets of samples were tested and Weibull analysis was performed as described in previous publications.17 A simple T-test was used to see if the mean fracture strengths were alike or different The results are shown in Table 3 where the samples, their designations, and the number of samples is as follows: Rohm & Haas CVD ZnS (RH, 20); RedZnS (Red, 23); elemental ZnS (E, 26); Raytheon multispectral HIPped ZnS (MS, 7); Princeton Scientific multispectral HIPped ZnS (PS HH, 6); Princeton Scientific CVD FLIR grade (PS, 6); and II-VI CVD ZnS (II-VI, 26) Boxes with a red “x” indicate that the row versus column T-test (two-tailed distribution, two-sample unequal variance) are statistically different The matrix is symmetric, so the other half of the matrix shows the actual calculated values This analysis basically shows that the samples can be grouped into three categories based on the mean strength (values shown in Table 4) The strongest samples were the II-VI standard CVD ZnS samples (group 1) Statistically lower strength as-deposited CVD samples (group 2) included the yellow standard commercial CVD grades produced by Rohm
& Haas (RH) and Princeton Scientific (PS), as well as elemental ZnS (E) and Red ZnS (Red) Lowest in strength (group 3) were the HIPped samples processed using the normal high temperature HIP process of commercial multispectral ZnS (MS and PS HH datasets)
Trang 7RH AS F HH Il-vi
Group Designation Sample Description
Avg grain size (microns
N
effective tensile
stressed
area
iii m2
Mean Strength
(FiPo
SD (MPa)
Weibull rIodulus (unbiased
Weibull Modulus biased)
deubull
scale factor ripa)
Weibull scale factor
psi)
A Weibull analysis was performed using the maximum likelihood estimate (MLE) method as described in ASTM C1239.18 A summary of the parameters determined from this analysis are also shown in Table 4 The strengths were normalized to 1 cm2 stressed area based on the effective tensile stressed area (ASTM C1499 eq X1.3) For this analysis, the Poisson’s ratio for the HIPped samples was assumed to be 0.32 and that of the CVD samples was assumed
to be 0.29 per Klein and Willingham19 The biased Weibull modulus does not take into account the number of specimens while the unbiased one does and is therefore more conservative These values agree well with previous published Weibull numbers,20 when all the data is normalized correctly
The CVD materials all have a moderate Weibull modulus and higher scale factor than the heat treated samples All tests were done on the same apparatus with the same surface preparation by the same optical shop, so surface flaws should be similar for all samples However, the different Young’s modulus between as-deposited and HIPped samples, could influence the behavior of abrasives interacting with the sample and result in a different flaw size in the CVD versus HIPped materials
4 DISCUSSION
In assessing x-ray diffraction data, optical transmittance, and strength, CVD ZnS samples can be grouped into three categories The first is the standard CVD materials, including Raytran, IIVI, RH, Rafael, and Vitron Measured hexagonality is 5 – 10 % and extinction at 1064 nm is 1.5 – 6.6 cm-1 The second group includes the more transparent as-deposited samples, including redZnS, Chinese ZnS, and elemental ZnS Measured hexagonality is 2 – 5% and extinction at 1064 nm is 0.3 – 0.7 cm-1 The third group includes the HIPped samples, including msZnS, Rafael msZnS, Vitron msZnS, PS msZnS, and PS HH Measured hexagonality is <1% and extinction at 1064 nm is 0.03 to 0.26cm-1 Biaxial strength is essentially the same for all the as-deposited CVD ZnS (groups 1 and 2) with the possible exception
of IIVI which appears to be slightly stronger Some notable differences remain to be explained Particularly, the 6 μm absorption is considerably different within the above categories above (e.g RafZnS has small α6.0 while other CVD ZnS have large α6.0, and Chinese ZnS has small α6.0 while elemental and red ZnS have large α6.0) Hot pressed ZnS and Bridgeman crystals are, as expected, considerably different from CVD ZnS It is clear that there are still some property-processing relationships that remain to be elicited in the understanding of CVD and HIPped CVD ZnS
Table 4: ZnS biaxial flexure results Mean and standard deviation is shown for actual samples
Weibull scale factor is normalized to 1cm 2 stressed areas as described in Reference 17
Table 3: T-test matrix on biaxial flexure strength data of ZnS samples; matrix is symmetric so actual
values are shown on the bottom half and statistically “different” (X) or “not different” (O) on the top
Trang 8Acknowledgements
Thanks to those who supplied samples of their ZnS material for testing including Stephen Jacobs of the University of Rochester for the Chinese ZnS, Klaus Wöhner of Vitron in Germany, and Shay Joseph of Rafael in Israel Todd Stefanik and C Scott Nordahl at Raytheon performed some of the polycrystalline x-ray measurements Thanks to Brian Zelinski, W Howard Poisl, and Gavin Buttigieg for valuable discussions Also thanks to Patrick Hogan who participated in the early parts of this work
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[20] Klein, C.A., R.P Miller, and R.L Gentilman, "Characteristic strength and Weibull modulus of selected infrared-transmitting materials," Optical Engineering, 41(2), 3151-3160 (2002)