GB2090237A - Optical element, especially of zinc sulphide or selenide, having improved optical quality - Google Patents
Optical element, especially of zinc sulphide or selenide, having improved optical quality Download PDFInfo
- Publication number
- GB2090237A GB2090237A GB8138005A GB8138005A GB2090237A GB 2090237 A GB2090237 A GB 2090237A GB 8138005 A GB8138005 A GB 8138005A GB 8138005 A GB8138005 A GB 8138005A GB 2090237 A GB2090237 A GB 2090237A
- Authority
- GB
- United Kingdom
- Prior art keywords
- pressure
- treatment
- zinc sulphide
- temperature
- mpa
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 28
- 230000003287 optical effect Effects 0.000 title claims abstract description 18
- 150000003346 selenoethers Chemical class 0.000 title description 3
- 230000005540 biological transmission Effects 0.000 claims abstract description 19
- 239000011888 foil Substances 0.000 claims abstract description 8
- 238000001228 spectrum Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 22
- 239000012535 impurity Substances 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 9
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 238000013508 migration Methods 0.000 claims 1
- 230000005012 migration Effects 0.000 claims 1
- -1 zinc selenide compound Chemical class 0.000 claims 1
- GTLQJUQHDTWYJC-UHFFFAOYSA-N zinc;selenium(2-) Chemical class [Zn+2].[Se-2] GTLQJUQHDTWYJC-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 18
- PFNQVRZLDWYSCW-UHFFFAOYSA-N (fluoren-9-ylideneamino) n-naphthalen-1-ylcarbamate Chemical compound C12=CC=CC=C2C2=CC=CC=C2C1=NOC(=O)NC1=CC=CC2=CC=CC=C12 PFNQVRZLDWYSCW-UHFFFAOYSA-N 0.000 abstract description 14
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 4
- 239000012530 fluid Substances 0.000 abstract description 3
- 229910052786 argon Inorganic materials 0.000 abstract description 2
- 238000001513 hot isostatic pressing Methods 0.000 description 18
- 238000005229 chemical vapour deposition Methods 0.000 description 15
- 238000010521 absorption reaction Methods 0.000 description 14
- 230000007547 defect Effects 0.000 description 11
- 238000009792 diffusion process Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000000411 transmission spectrum Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/08—Sulfides
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/02—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of crystals, e.g. rock-salt, semi-conductors
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
- G02B6/102—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type for infrared and ultraviolet radiation
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/50—Glass production, e.g. reusing waste heat during processing or shaping
- Y02P40/57—Improving the yield, e-g- reduction of reject rates
Landscapes
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Thermal Sciences (AREA)
- Toxicology (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Glass Compositions (AREA)
- Luminescent Compositions (AREA)
Abstract
Articles of polycrystalline zinc sulphide and zinc selenide achieve substantially improved optical quality by a treatment of heat and isostatic pressure by means of an inert working fluid, e.g. argon. The treated specimens are transparent and have substantial transmission in the infrared and visible range of the spectrum. Additional improvement in the transmission characteristics is achieved by wrapping the specimens in a foil of an inert material prior to treatment. Temperatures from 700 DEG C to 1050 DEG C and pressures from 34 MPa to 205 MPa may be used over periods from 3 hours upwards.
Description
SPECIFICATION
Optical element, especially of zinc sulphide or selenide, having improved optical quality
Zinc sulphide and zinc selenide are used in applications such as missile domes requiring long wavelength infrared transmission capability. Zinc sulphide is a major window material for air borne FLIR systems. These compounds are some of the most chemically and mechanically durable materials which are transparent in the infrared range of the electromagnetic spectrum to approximately 10 micrometers.
Elements made thereof are available in useful sizes, and have potential for transmission in the visible range of the spectrum. A problem with these compounds is that they do not have adequate transmission in the visible and near-infrared range of the electromagnetic spectrum. Additional applications for these compounds could be developed if their transparency at visible and near-infrared wavelengths could be improved. More specifically, they could then be used in applications requiring multi-spectral capability. While their far-infrared wavelength limitation is an intrinsic property of the material and is related to multi-phonon absorption, their short wavelength limitation is determined by several incompletely characterized extrinsic effects.
According to the present invention there is provided a method of treating an optical element to improve its optical characteristics which comprises hot isostatically pressing the element.
Hot isostatic pressing (HIP) is the simultaneous application of heat and pressure by means of an inert working fluid. It has been discovered that HIP treatment of zinc sulphide and zinc selenide specimens produces improvement beyond the elimination of pores. It substantially improves the transparency at wavelengths shorter than two microns. Specimens of zinc sulphide have also been found to have improved transmission characteristics throughout their effective spectral band. The limitation in the transparency of zinc sulphide and zinc selenide is due to scattering and absorption mechanism. At wavelengths below two micrometers, it is believed that scatter, not absorption, is the principal mechanism that limits transmission.It is found that HIP treatment reduces scatter, not only by reducing or eliminating porosity, but also by reducing or eliminating second phase inclusions, by allowing out-diffusion of impurities, and, in the case of zinc sulphide, by promoting inversion of zinc sulphide non-cubic polymorphs to their cubic form. Overall, absorption is reduced by HIP treatment by allowing diffusion of absorbing species that might be present. HIP treatment is also found to produce the stoichiometric ratio of the component atoms for both ZnS and ZnSe.
A further improvement can be achieved by controlling the chemical potential on the surface of the article while heating the article and applying isostatic pressure. Preferabiy the chemical potential control is achieved by wrapping the article in a foil of an inert material while still allowing some vapour exchange.
The invention wil! be further described by way of example, with reference to the accompanying drawing, which shows the transmission spectra for a specimen of ZnS before and after treatment.
Hot Isostatic Pressing (HIP), the simultaneous application of heat and pressure by means of an inert working fluid, is used in metallurgical fabrication of powder metal compacts and castings to improve fracture strength and fatigue resistance. This invention uses similar HIP equipment to treat specimens of zinc sulphide and zinc selenide. The specimens to be treated are placed in a HIP furnace of conventional design. The furnace is evacuated, and then pressurized with an inert gas, such as argon.
Heat is applied and the temperature and pressure allowed to stabilize. The pressure and heat are maintained for a period of time sufficient to substantially eliminate a variety of impurities and defects from the specimens. The specimens treated have included chemical vapour deposition (CVD) zinc sulphide as well as hotpressed zinc sulphide. Specimens of CVD zinc selenide were also treated.
Currently available specimens of zinc sulphide and zinc selenide are coloured and translucent. For zinc sulphide, the coiouration results from deviations from a strict stoichiometric ratio of the atoms in the material. The specimens are translucent rather than transparent because light is scattered by defects in the bulk of the material. The exact nature of all the different types of defects is not known. The colour, types and relative amounts of light scattering defects are determined by the technique used to prepare the material and by the processing conditions of the preparation. The scattering defects severely limit the transparency at wavelengths shorter than approximately two micrometers. Additionally, there are some absorption bands at different wavelengths which depend on the method of fabrication of the specimen.The long wavelength limit of the transmission band is an intrinsic property of the material and is due to a multi-phonon absorption phenomenon. For wavelengths between approximately 2 ym and the long wavelength limit, the transmission is limited principally by impurity-related absorption phenomena. The limitation in transparency in these materials at visible and near infrared wavelengths is due to a combination of incompletely characterized absorption and scattering phenomena, but scattering predominates. The short wavelength limit of the transmission band is ultimately an intrinsic material characteristic, but non-stoichiometry, impurities and other point defects can diminish transparency at wavelengths close to the short wavelength limit.Hot isostatic processing (HIP) treatment reduces these limitations not only by reducing or eliminating the porosity of the material but also by reducing or eliminating many of the defects that contribute to scatter and absorption. This is due to a combination of factors produced by HIP treatment through a simultaneous application of heat and pressure. The applied heat allows substantial out-diffusion of impurities normally present in the
material. These impurities may consist of actual impurities formed by contaminating atoms of elements other than those forming the ideal compound, or may consist of defects in the crystal lattice, such as
vacancies and interstitial atoms. In any event, these impurities will diffuse out to the surface of the
specimen at a rate which is a function of temperature.Impurity atoms may be present within the
sulphide or selenide crystals as separate distinct phases. The heat supplied also helps to reduce or
eliminate these inclusions of second phase precipitates of the compound being treated. The applied
pressure helps to eliminate such residual porosity as may be present in the specimen prior to the
treatment, and restrains the formation of new porosity which could otherwise develop during the
process. Additionally, the pressure is used to limit the volatilization of the compounds, since the
compounds used have appreciable vapour pressure at useful treatment temperatures. In the case of zinc
sulphide compounds, the optically isotropic cubic crystalline form has a higher density than the
birefringent hexagonal form. The pressure of the HIP treatment is found to favour inversion of non-cubic
polymorphs into cubic crystals.Furthermore, the pressure decreases the equilibrium concentration of
interstitial atoms and vacancies of the crystal lattice, and generally decreases the solubility of impurities.
Specimens of zinc sulphide have included both the chemical vapour deposition (CVD) and hot
pressed types. Zinc selenide specimens have been of the CVD type. It is found that hot-pressed zinc
selenide specimens have substantially inferior transmission characteristics as compared to CVD zinc
selenide specimens and thus are not generally available. However, this treatment should improve the
characteristics of hot-pressed zinc selenide as well. The duration of the treatment depends on the initial
quality of the specimen. The better the quality, i.e. transmission capability, of the specimen, the shorter
the treatment time can be to achieve a predetermined level of transmission improvement. It has been found that hot pressed zinc sulphide material has larger concentrations of impurities or defects that
affect scattering as compared to zinc sulphide prepared by the CVD process.The duration of the
treatment is also determined by thickness of the starting sample. The greater the thickness the longer
the treatment has to last to achieve a predetermined level of transmission improvement.
As discussed above, it has been discovered that subjecting specimens to HIP treatment improves
the optical characteristic of optical elements. This is due to a combination of factors. The heat provided
seems to favour an out-diffusion of impurities from the core of the specimen to the outside surface. The
pressure limits the volatilization of the compound and also helps to eliminate and prevent the formation
of porosity. In the case of zinc sulphide, the pressure is also believed to force any noncubic polymorphs
present into their cubic form. This provides a guideline in the selection of operating temperature and
pressure. The temperature should be high enough to allow the out-diffusion of impurities from the body of the specimen. The pressure should be high enough to both prevent volatilization, and to substantially eliminate porosity in the specimen.The duration of the treatment is determined by both the thickness of the specimen as well as its initial optical quality. The less transmitting samples normally require a longer ti eatment time to achieve a predetermined level of optical transparency. However, an upper limit to the duration of the treatment might be determined by an excessive amount of grain growth that might take place during an unreasonably long treatment. It is also found that the CVD type zinc sulphide achieves a substantially better amount of optical improvement than the hot-pressed zinc sulphide specimens. This is probably due to the fact that the hot-pressing process tends to produce larger size defects which do not out-diffuse as well with this process.
A six millimeter specimen of CVD zinc sulphide was processed in three hours by the application of 9900C and 5,000 psi (34 MPa) and resulted in visible improvement of the optical characteristics of the specimen. A pressure of 30,000 psi (205 MPa) and a temperature of 1 0000C was used for a hotpressed specimen of zinc sulphide and a CVD zinc selenide specimen, again resulting in substantial optical improvement. A 1 5 millimeter specimen of CVD zinc sulphide, using a temperature of approximately 1 0000C and pressure of 30,000 psi (205 MPa) as above, was successfully treated in approximately twenty-four hours. Temperatures in the range of 7000C to 1 0500C and pressures in the range of 5,000 to 30,000 psi (34 to 205 MPa) have been used to date on different types of specimens.
The times range from three hours for the smaller thickness mentioned to thirty-six hours for larger sample thicknesses. However, the invention is not limited to these operating parameters. Substantially different combinatjons of temperature, pressure and duration of the treatment will produce improvements of the optical quality of the treated specimens to some degree. The actual operating parameters are normally dictated by the requirements of specific applications. Substantially lower temperatures and pressures might be used to produce a predetermined amount of improvement.
Some specimens were first wrapped in a foil prior to the application of heat and pressure in the
HIP apparatus. The wrappings are not vacuum tight but they serve to limit the vapour exchange between the specimens and the reaction chamber and also serve to control the chemical potential of the volatile species in the specimens in order to enhance the treatment. This control of the chemical potential of the volatile species on the surface of the specimens could be achieved by other means, such as use of dopants in the working gas or solids that will give off vapour species. Different types of material have been used. Graphite, mild steel, tantalum, copper and platinum foils have been used. The platinum wrapping foil results in the best improvement of transmission characteristics for the samples.
This is probably due to its inert nature.
Referring now to the drawing, there is shown the transmission spectrum of a six millimeter thick
CVD zinc sulphide specimen. Line 10 is for the original specimen prior to treatment and line 20 is for the same specimen after a HIP treatment for three hours at 1 0000C and 30,000 psi (205 MPa). The HIP treatment has substantially improved short wavelength transmittance of the material and has also eliminated the infrared absorption band at six micrometers. Absorption bands in zinc sulphide depend on the manufacturing method and operating conditions but these are expected to be substantially improved by the HIP treatment. Visually, the untreated specimen is yellow-orange and haxy to the extent that it cannot be used for imaging at visible wavelengths.The treated material is colourless because treatment has adjusted the stoichiometry to the correct one-to-one zinc to sulphur ratio and is water clear because the treatment has very substantially reduced the concentration of light scattering defects. HIP treatment substantially improves the transmissivity at wavelengths greater than 2 micrometers. Other specimens of ZnS were similarly treated at 30,000 psi (205 MPa) at 9900C for twenty-four hours. Specimens rangad in thickness from 0.4 to 1.5 centimeters.
The following table summarizes absorption coefficient measures for a 6 millimeter thick ZnS specimen. These apparent absorptance values were calculated by dividing the fraction of absorbed light by the thickness of the specimen and thus includes surface contribution to the absorption.
Apparent Absorption Coefficient of CVD ZnS (cm-')
Wavelength After
(Micrometer) Untreated Treatment
2.8 4.09 x ?0-3 8.6 x 10-4
3.8 2.19 x10-2 2.16 x10-3 9.27 8.41 x 10-2 1.29 x 10-2
10.6 2.54 x 10-' 1.92 x 10-1 A six millimeter thick spectrum of CVD zinc selenide was also treated for three hours at 1 0000C and 30,000 psi (205 MPa). Visually, the untreated specimen is yellow in colour and hazy. After treatment, the colour is yellow-green and transparent. This colour is due to the correct stoichiometry for zinc selenide. The transparency in the visible range is substantially improved.Using a spectrometer, the transmission of the specimen at 0.5 micrometer was measured before treatment and was found to be 5%, while after treatment transmission was found to be 50%. This substantial improvement is due mainly to the adjustment to the stoichiometric ratio that the treatment provides. A measure was also obtained of the scattering of light of the specimen before and after treatment. A He-Ne laser was used to provide a source of light at .6238 micrometers. The fraction of light scattered at 900 to the incident laser beam was measured in (Steradian)-I as follows:
Prior to treatment 2 x 10-3
After treatment 4.5 x 10-4
This indicates that the types of impurities in this material give rise substantially to scatter, the phenomenon that is responsible for reduced transmission at low wavelength and the one that HIP treatment is believed to reduce effectively.
Claims (15)
1. A method of treating an optical element to improve its optical characteristics which comprises hot isostatically pressing the element.
2. A method according to claim 1, wherein the optical element is an element of zinc sulphide or zinc selenide compounds.
3. A method according to claim 2, wherein the element is heated and subjected to a superatmospheric isostatic pressure.
4. A method according to claim 3, wherein the temperature and pressure are maintained substantially constant throughout the treatment.
5. A method according to claim 3 or 4, wherein the temperature to which the element is heated is sufficient to cause outward migration of impurities in the element.
6. A method according to claim 3, 4 or 5, wherein the isostatic pressure is sufficient to eliminate existing porosity of the element and to limit the formation of new porosity during the treatment.
7. A method according to any of claims 3 to 6, wherein the isostatic pressure is applied for a period of at least three hours.
8. A method according to any of claims 3 to 7, wherein the temperature to which the element is heated lies in the range of 7000C to 1 0500C.
9. A method according to any of claims 3 to 8, wherein the applied pressure used lies in the range of 5,000 to 30,000 psi (34 MPa to 205 MPa).
10. A method according to any of claims 3 to 7, wherein the temperature and pressure of the temperature are approximately 10000C and 5,000 psi (34 MPa).
11. A method according to any of claims 3 to 10, wherein the pressure is applied by an inert gas.
12. A method according to claim 1 1, wherein the vapour exchange between the article and the inert gas is controlled.
13. A method according to any of claims 3 to 12, wherein the chemical potential of the volatile species on the surface of the element is controlled to enhance the treatment.
14. A method according to any of claims 3 to 13, wherein the element is wrapped in an inert foil prior to the application of heat and pressure.
15. A method according to claim 14, wherein the wrapping foil is not vacuum tight.
1 6. A method according to claim 14 or 15, wherein the wrapping foil is made of platinum.
1 7. An article of zinc sulphide or zinc selenide compound having substantial transmission in the visible and infrared range of the electromagnetic spectrum.
1 8. An article according to claim 17, further having a substantially stoichiometric ratio of the component atoms of the compound.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US22094480A | 1980-12-29 | 1980-12-29 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| GB2090237A true GB2090237A (en) | 1982-07-07 |
| GB2090237B GB2090237B (en) | 1985-12-11 |
Family
ID=22825678
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB8138005A Expired GB2090237B (en) | 1980-12-29 | 1981-12-16 | Optical element especially of zinc sulphide or selenide having improved optical quality |
| GB08323505A Expired GB2125023B (en) | 1980-12-29 | 1983-09-01 | Optical element especially of zinc sulphide or selenide having improved optical quality |
Family Applications After (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| GB08323505A Expired GB2125023B (en) | 1980-12-29 | 1983-09-01 | Optical element especially of zinc sulphide or selenide having improved optical quality |
Country Status (7)
| Country | Link |
|---|---|
| JP (3) | JPS57135723A (en) |
| CA (1) | CA1181557A (en) |
| DE (1) | DE3150525A1 (en) |
| FR (2) | FR2497361B1 (en) |
| GB (2) | GB2090237B (en) |
| IT (1) | IT1172159B (en) |
| SE (1) | SE8107840L (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0157040A2 (en) * | 1983-04-05 | 1985-10-09 | Sumitomo Electric Industries Limited | Method of producing transparent polycrystalline ZnS body |
| EP0322881A2 (en) * | 1987-12-28 | 1989-07-05 | Tosoh Corporation | Method of producing uniform silica glass block |
| US4866007A (en) * | 1987-03-18 | 1989-09-12 | Sumitomo Electric Industries Co. | Method for preparing single-crystal ZnSe |
| EP0530589A1 (en) * | 1991-09-04 | 1993-03-10 | WILD LEITZ SYSTEMTECHNIK GmbH | Omnivision periscope for day and night vision |
| US5324353A (en) * | 1990-11-14 | 1994-06-28 | Raytheon Company | Zinc sulfide bodies having improved optical transmittance characteristics and mechanical characteristics |
| WO1995029277A1 (en) * | 1994-04-26 | 1995-11-02 | Kuepper Lukas | Process for producing micro-optical elements or a fibre end in the form of a micro-optical element, and the use of such elements |
| EP0770584A1 (en) * | 1994-04-28 | 1997-05-02 | Heraeus Quarzglas GmbH | Method for producing heat-resistant synthetic quartz glass |
| US6716659B2 (en) | 1999-01-04 | 2004-04-06 | Infineon Technologies Ag | Method and apparatus for shaping semiconductor surfaces |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5957951A (en) * | 1982-09-27 | 1984-04-03 | 住友電気工業株式会社 | Manufacture of zns polycrystal body |
| JPS607413A (en) * | 1983-06-28 | 1985-01-16 | Matsushita Electric Ind Co Ltd | Lens for converging beam |
| FR2898962B1 (en) | 2006-03-23 | 2008-05-09 | Brandt Ind Sas | DOMESTIC GAS COOKING OVEN AND METHOD OF IGNITING AT LEAST ONE GAS BURNER IN SUCH GAS DOMESTIC COOKING OVEN |
| US7790072B2 (en) * | 2007-12-18 | 2010-09-07 | Raytheon Company | Treatment method for optically transmissive bodies |
| EP2511236B1 (en) * | 2011-04-14 | 2015-07-01 | Rohm and Haas Company | Improved quality multi-spectral zinc sulfide |
| JP5444397B2 (en) * | 2012-03-09 | 2014-03-19 | 住友電気工業株式会社 | Manufacturing method of optical components |
| US20130271610A1 (en) | 2012-04-16 | 2013-10-17 | Keith Gregory ROZENBURG | Polycrystalline chalcogenide ceramic material |
| JP5876798B2 (en) * | 2012-09-14 | 2016-03-02 | 住友電気工業株式会社 | ZnSe polycrystal and method for producing the same |
| JP5621828B2 (en) * | 2012-10-11 | 2014-11-12 | 住友電気工業株式会社 | Manufacturing method of optical components |
| JP6989102B2 (en) * | 2017-04-05 | 2022-01-05 | 日本電気株式会社 | Manufacturing method of zinc sulfide sintered body and zinc sulfide sintered body |
Family Cites Families (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3131025A (en) * | 1959-10-29 | 1964-04-28 | Eastman Kodak Co | Zinc sulfide optical element |
| FR1272294A (en) * | 1960-10-26 | 1961-09-22 | Kodak Pathe | New optical element and method and apparatus for its manufacture |
| US3454685A (en) * | 1961-08-21 | 1969-07-08 | Eastman Kodak Co | Method of forming zinc selenide infrared transmitting optical elements |
| CH389176A (en) * | 1961-08-21 | 1965-03-15 | Kodak Sa | Optical element and method for its manufacture |
| DE1244433B (en) * | 1961-08-21 | 1967-07-13 | Eastman Kodak Co | Optical material and process for its manufacture |
| US3177759A (en) * | 1961-10-04 | 1965-04-13 | Barnes Eng Co | Apparatus for the spectrum examination of materials |
| FR2286394A1 (en) * | 1974-09-30 | 1976-04-23 | Comp Generale Electricite | OPTICAL DEVICE |
| GB1547172A (en) * | 1976-06-24 | 1979-06-06 | Nat Res Dev | Methods and apparatus for cutting welding drilling and surface treating |
| JPS55113802A (en) * | 1979-02-24 | 1980-09-02 | Sumitomo Electric Ind Ltd | Production of high-purity sintered body by hot hydrostatic press |
| JPS6016391B2 (en) * | 1979-03-31 | 1985-04-25 | 住友電気工業株式会社 | Manufacturing method of high purity, high strength ZnSe sintered body by hot forging method |
| DE2949512C2 (en) * | 1979-12-08 | 1982-10-21 | W.C. Heraeus Gmbh, 6450 Hanau | Process for the aftertreatment of zinc sulphide bodies for optical purposes |
| JPS5711824A (en) * | 1980-06-23 | 1982-01-21 | Matsushita Electric Ind Co Ltd | Preparation of semiconductive zinc sulfide |
| JPS5717411A (en) * | 1980-07-02 | 1982-01-29 | Agency Of Ind Science & Technol | Manufacture of polycrystalline zinc selenide body |
| DE3039749C2 (en) * | 1980-10-22 | 1982-08-19 | Heraeus Quarzschmelze Gmbh, 6450 Hanau | Process for the production of bubble-free, glassy material |
| JPS606307B2 (en) * | 1980-12-22 | 1985-02-16 | 工業技術院長 | Method for producing polycrystalline zinc selenide |
-
1981
- 1981-11-06 CA CA000389659A patent/CA1181557A/en not_active Expired
- 1981-12-16 GB GB8138005A patent/GB2090237B/en not_active Expired
- 1981-12-16 IT IT49921/81A patent/IT1172159B/en active
- 1981-12-21 DE DE19813150525 patent/DE3150525A1/en not_active Ceased
- 1981-12-25 JP JP56216050A patent/JPS57135723A/en active Granted
- 1981-12-28 FR FR818123571A patent/FR2497361B1/en not_active Expired
- 1981-12-29 SE SE8107840A patent/SE8107840L/en not_active Application Discontinuation
-
1983
- 1983-09-01 GB GB08323505A patent/GB2125023B/en not_active Expired
-
1987
- 1987-09-29 FR FR878713457A patent/FR2610730B1/en not_active Expired - Lifetime
-
1990
- 1990-12-26 JP JP2406626A patent/JPH03271122A/en active Granted
- 1990-12-26 JP JP2406625A patent/JPH03271107A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0157040A2 (en) * | 1983-04-05 | 1985-10-09 | Sumitomo Electric Industries Limited | Method of producing transparent polycrystalline ZnS body |
| EP0157040A3 (en) * | 1983-04-05 | 1987-11-25 | Sumitomo Electric Industries Limited | Method of producing transparent polycrystalline zns body |
| US4866007A (en) * | 1987-03-18 | 1989-09-12 | Sumitomo Electric Industries Co. | Method for preparing single-crystal ZnSe |
| EP0322881A2 (en) * | 1987-12-28 | 1989-07-05 | Tosoh Corporation | Method of producing uniform silica glass block |
| EP0322881A3 (en) * | 1987-12-28 | 1990-09-12 | Tosoh Corporation | Method of producing uniform silica glass block |
| US5324353A (en) * | 1990-11-14 | 1994-06-28 | Raytheon Company | Zinc sulfide bodies having improved optical transmittance characteristics and mechanical characteristics |
| EP0530589A1 (en) * | 1991-09-04 | 1993-03-10 | WILD LEITZ SYSTEMTECHNIK GmbH | Omnivision periscope for day and night vision |
| WO1995029277A1 (en) * | 1994-04-26 | 1995-11-02 | Kuepper Lukas | Process for producing micro-optical elements or a fibre end in the form of a micro-optical element, and the use of such elements |
| EP0770584A1 (en) * | 1994-04-28 | 1997-05-02 | Heraeus Quarzglas GmbH | Method for producing heat-resistant synthetic quartz glass |
| US6716659B2 (en) | 1999-01-04 | 2004-04-06 | Infineon Technologies Ag | Method and apparatus for shaping semiconductor surfaces |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2610730B1 (en) | 1990-10-12 |
| GB2090237B (en) | 1985-12-11 |
| FR2497361B1 (en) | 1989-03-31 |
| SE8107840L (en) | 1982-06-30 |
| GB2125023A (en) | 1984-02-29 |
| GB8323505D0 (en) | 1983-10-05 |
| IT1172159B (en) | 1987-06-18 |
| CA1181557A (en) | 1985-01-29 |
| JPH0469090B2 (en) | 1992-11-05 |
| DE3150525A1 (en) | 1982-08-26 |
| FR2497361A1 (en) | 1982-07-02 |
| JPH0451489B2 (en) | 1992-08-19 |
| JPH03271122A (en) | 1991-12-03 |
| FR2610730A1 (en) | 1988-08-12 |
| IT8149921A0 (en) | 1981-12-16 |
| JPH03271107A (en) | 1991-12-03 |
| GB2125023B (en) | 1985-11-13 |
| JPS57135723A (en) | 1982-08-21 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PE20 | Patent expired after termination of 20 years |
Effective date: 20011215 |