CN108165951A - The Preparation equipment of zinc sulphide or zinc selenide ball cover - Google Patents
The Preparation equipment of zinc sulphide or zinc selenide ball cover Download PDFInfo
- Publication number
- CN108165951A CN108165951A CN201711395684.XA CN201711395684A CN108165951A CN 108165951 A CN108165951 A CN 108165951A CN 201711395684 A CN201711395684 A CN 201711395684A CN 108165951 A CN108165951 A CN 108165951A
- Authority
- CN
- China
- Prior art keywords
- zinc
- ball cover
- source
- settling chamber
- carrier gas
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Classifications
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
- C23C16/305—Sulfides, selenides, or tellurides
- C23C16/306—AII BVI compounds, where A is Zn, Cd or Hg and B is S, Se or Te
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B28/00—Production of homogeneous polycrystalline material with defined structure
- C30B28/12—Production of homogeneous polycrystalline material with defined structure directly from the gas state
- C30B28/14—Production of homogeneous polycrystalline material with defined structure directly from the gas state by chemical reaction of reactive gases
-
- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/46—Sulfur-, selenium- or tellurium-containing compounds
- C30B29/48—AIIBVI compounds wherein A is Zn, Cd or Hg, and B is S, Se or Te
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mechanical Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Vapour Deposition (AREA)
- Physical Vapour Deposition (AREA)
Abstract
The present invention provides a kind of zinc sulphide or the Preparation equipment of zinc selenide ball cover, including chemical vapor deposition stove, vacuum extractor, the first carrier gas source and the second carrier gas source.Chemical vapor deposition stove includes：Settling chamber；Crucible for holding solid zinc source, connects below settling chamber and with settling chamber；Punch-pin substrate, appearance mirror polish are simultaneously fixed in settling chamber；Dust chamber above settling chamber and connects settling chamber；Primary heater, for being heated to settling chamber；And secondary heater, for being heated to crucible.The controlled connection dust chamber of vacuum extractor.First carrier gas source is controlled to be communicated in crucible.The controlled connection settling chamber of second carrier gas source.The material of punch-pin substrate is isostatic pressing formed graphite.In the Preparation equipment of zinc sulphide according to the present invention or zinc selenide ball cover, the use of isostatic pressing formed graphite can improve the quality and manufacturing process of the ball cover of the formation of chemical vapor deposition.
Description
Technical field
The present invention relates to chemical vapor deposition fields, and in particular to the Preparation equipment of a kind of zinc sulphide or zinc selenide ball cover.
Background technology
Zinc selenide (ZnSe) has direct transition type energy band, and as a kind of excellent luminescent material, luminous efficiency is high, and by
In its not only thoroughly infrared but also saturating visible ray, transparency range is wide, and has the characteristics that absorption coefficient is low, non-deliquescent, and with well
Mechanics and thermal property, be widely used as the window and lens of infrared acquisition, imaging device.Zinc sulphide (ZnS) is a kind of
The material of infrared window haveing excellent performance, its transmission wave band cover visible ray, in infrared and far infrared, and have good
Mechanics and thermal property are widely used in preparing infrared window and radome fairing of Infrared pod and precision guidance missile etc..Using
ZnSe/ZnS polycrystalline prepared by chemical vapour deposition technique (Chemical vapor deposition, CVD) has purity height, matter
Ground is uniform, low scattering, low absorption and the advantages that low hyperthermia radiation, performance is better than the product prepared using other techniques, thus state
Generally using original papers such as ball cover, window, the lens of chemical vapor deposition method growing optics on border.
Chemical vapor deposition is occurred between agent molecule to chemically react and generates specific solid product to react.Gas phase is given birth to
Long inherent characteristics are that growth rate is relatively low, therefore the thickness of CVD ZnSe/ZnS products is also restricted.So CVD
ZnSe/ZnS grows into very thick plank, and to be then cut into variously-shaped ball cover or prism not only difficult big, nor
It is economical.There is also larger difficulty for abnormity processing simultaneously.
In cvd furnace by place it is suitable, polished after punch-pin substrate, demould after deposition, replicate ball cover
The inner surface of inner surface and ball cover not only reduces difficulty of processing and workload, and reduce the waste of material without processing.
But the quality and preparation process of the ball cover of chemical vapor deposition formation are restricted by the material property of punch-pin substrate,
So still needing that punch-pin substrate and Preparation equipment is further improved, formed with further improving chemical vapor deposition
Ball cover quality and manufacturing process.
Invention content
In view of the problem of background technology, the purpose of the present invention is to provide a kind of zinc sulphide or zinc selenide ball covers
Preparation equipment can improve the quality and manufacturing process of the ball cover of the formation of chemical vapor deposition.
To achieve these goals, the present invention provides the Preparation equipments of a kind of zinc sulphide or zinc selenide ball cover to include chemistry
Gaseous phase deposition stove, vacuum extractor, the first carrier gas source and the second carrier gas source.Chemical vapor deposition stove includes：Settling chamber；Earthenware
Crucible for holding solid zinc source, connects below settling chamber and with settling chamber；Punch-pin substrate, appearance mirror polish are simultaneously fixed on
In settling chamber；Dust chamber above settling chamber and connects settling chamber；Primary heater, for being heated to settling chamber；With
And secondary heater, for being heated to crucible and solid zinc source being made to become fused zinc source and zinc fume source.Vacuum extractor
Controlled connection dust chamber.First carrier gas source is controlled to be communicated in crucible, is steamed for being passed through the first carrier gas and the first carrier gas being made to carry zinc
In vapour source to settling chamber.The controlled connection settling chamber of second carrier gas source, the second carrier gas for that will carry sulphur source or selenium source are supplied to
So that sulphur source or selenium source that the second carrier gas carries are reacted simultaneously with the zinc fume source that the first carrier gas carries in settling chamber in settling chamber
It deposits to punch-pin substrate and grows to form zinc sulphide or zinc selenide ball cover.Wherein, the material of punch-pin substrate is isostatic pressing formed graphite.
Beneficial effects of the present invention are as follows：In the Preparation equipment of zinc sulphide according to the present invention or zinc selenide ball cover, etc.
The use of static pressure graphite can improve the quality and manufacturing process of the ball cover of the formation of chemical vapor deposition.
Description of the drawings
Fig. 1 is the schematic diagram of the Preparation equipment of zinc sulphide or zinc selenide ball cover according to the present invention.
Wherein, the reference numerals are as follows：
1 chemical vapor deposition stove, 3 first carrier gas source
11 settling chamber, 4 second carrier gas source
12 crucible, 5 exhaust gas processing device
13 punch-pin substrate, 6 cover body
14 dust chamber, 7 surge tank
8 collecting tank of 15A primary heaters
15B secondary heater V valves
2 vacuum extractors
Specific embodiment
Illustrate the Preparation equipment of zinc sulphide or zinc selenide ball cover according to the present invention with reference to the accompanying drawings.
As shown in Figure 1, the Preparation equipment of zinc sulphide according to the present invention or zinc selenide ball cover includes chemical vapor deposition stove
1st, vacuum extractor 2, the first carrier gas source 3 and the second carrier gas source 4.
Chemical vapor deposition stove 1 includes；Settling chamber 11；Crucible 12, for holding solid zinc source, positioned at 11 lower section of settling chamber
And it is connected with settling chamber 11；Punch-pin substrate 13, appearance mirror polish are simultaneously fixed in settling chamber 11；Dust chamber 14, positioned at settling chamber
11 tops simultaneously connect settling chamber 11；Primary heater 15A, for being heated to settling chamber 11；And secondary heater 15B,
For being heated to crucible 12 and solid zinc source being made to become fused zinc source and zinc fume source.The controlled connection of vacuum extractor 2 is received
Dirt room 14.First carrier gas source 3 is controlled to be communicated in crucible 12, is arrived for being passed through the first carrier gas and the first carrier gas being made to carry zinc fume source
In settling chamber 11.Second carrier gas source, 4 controlled connection settling chamber 11, it is heavy that the second carrier gas for that will carry sulphur source or selenium source is supplied to
So that sulphur source or selenium source that the second carrier gas carries are reacted simultaneously with the zinc fume source that the first carrier gas carries in settling chamber in product room 11
It deposits to punch-pin substrate 13 and grows and form zinc sulphide or zinc selenide ball cover.Wherein, the material of punch-pin substrate 13 is isostatic pressed stone
Ink.
Under the range being applicable in chemical vapor deposition, as the mechanical strength of the raising isostatic pressing formed graphite of temperature does not drop not only
It is low, it increases instead, this is very beneficial for keeping the shape of punch-pin substrate 13 steady at a high temperature of chemical vapor deposition in settling chamber
It is qualitative, so that depositing and growing the zinc sulphide of formation or the size dimensionally stable at high temperature of zinc selenide ball cover；Working as
After learning vapor deposition, as the mechanical strength relatively-high temperature of the reduction isostatic pressing formed graphite of temperature reduces, so as to growing shape
Into zinc sulphide or zinc selenide ball cover cooling shrink generate resistance (or drag) reduce, and then reduce cooling shrink zinc sulphide
Or the internal stress of zinc selenide ball cover, avoid the rupture of zinc sulphide or zinc selenide ball cover；Further, since the punch-pin lining of isostatic pressing formed graphite
Bottom 13 is shunk the resistance (or drag) generated to the zinc sulphide of growth formation or the cooling of zinc selenide ball cover and is reduced, but also finally
Zinc sulphide or zinc selenide ball cover are easily separated from punch-pin substrate 13；Further more, isostatic pressing formed graphite has isotropic characteristic, this causes
Chemical vapor deposition is conducive to zinc sulphide polycrystalline at high temperature or zinc selenide polycrystalline is each from internal layer to outer layer on the surface of punch-pin
The phase same sex is grown, and then the optical quality of the ball cover improved.In other words, the use of isostatic pressing formed graphite can improve chemical vapor deposition
The quality and manufacturing process of the ball cover of long-pending formation.
The quality and preparation process for the ball cover that chemical vapor deposition is formed are restricted by the material property of isostatic pressing formed graphite, tool
Illustrate to body the influence of the grain size of isostatic pressing formed graphite, density, coefficient of thermal expansion and ash content.
If the grain size of isostatic pressing formed graphite is small, smooth, bright surface is readily available when polishing punch-pin substrate 13；Deng
The grain size of static pressure graphite is big, increases polishing difficulty, while the obtained surface of punch-pin substrate 13 has bumps on microcosmic, influences
Zinc sulphide or the growth of zinc selenide polycrystalline and demoulding.It is preferred that the grain size of isostatic pressing formed graphite is not more than 15 μm, is polished with synthesis, is more
Crystals growth and demoulding.
If the density of isostatic pressing formed graphite is small, particle is loose, and when polishing easily polishes off more isostatic pressing formed graphites, reduces convex
The service life at die bush bottom 13；In addition, easily generating fine hole, the out-of-flatness on surface is easy to cause initially in deposition process
The zinc sulphide or zinc selenide polycrystalline of generation are coarse granule, influence optical property.Preferably, the density of isostatic pressing formed graphite is more than
1.80g/cm3。
The ash content of isostatic pressing formed graphite is few, and the impurity volatilized at high temperature is few.Impurity can influence the polycrystalline finished product of generation
Rate and its optical property.It is thus preferable that the ash content of isostatic pressing formed graphite is not more than 200ppm.
The isostatic pressing formed graphite of above-mentioned specific material property can be by purchased in market or customize, such as external Japan from manufacturer
Carbon Co., Ltd. of Japan, French rowland carbon group, SGL Carbon Group etc..
First carrier gas is identical with the second carrier gas.Based on cost consideration, the first carrier gas and the second carrier gas are selected from argon gas.
The polishing on 13 surface of punch-pin substrate may be used various modes and carry out.For example, punch-pin substrate 13 is by from thick to thin
Sand paper polishing polished with surface.Specifically, sand paper from thick to thin is the SiC sand of 320 mesh, 800 mesh, 1200 mesh, 1500 mesh
Paper.In addition, punch-pin substrate 13 can also be polished by newspaper or the sand paper back side again after sand paper polishing.
Solid zinc source is pure zinc, and sulphur source can be hydrogen sulfide, and selenium source can be hydrogen selenide.
In order to which the extra material for having neither part nor lot in reaction in settling chamber 11 is handled, with reference to Fig. 1, the zinc sulphide or selenizing
The Preparation equipment of zinc ball cover further includes：Exhaust gas processing device 5, it is controlled to be communicated in vacuum extractor 2.Further, the vulcanization
The Preparation equipment of zinc or zinc selenide ball cover further includes：Cover body 6 above dust chamber 14 and is communicated in dust chamber 14；Surge tank
7, between cover body 6 and vacuum extractor 2 and it is communicated in dust chamber 14 and vacuum extractor 2；Collecting tank 8, positioned at surge tank 7
Lower section, and be communicated in surge tank 7.Collecting tank 8 is used to collect solid material.
In the Preparation equipment of zinc sulphide according to the present invention or zinc selenide ball cover, with reference to Fig. 1, " controlled connection " can lead to
Valve V is crossed to carry out.
Claims (9)
1. the Preparation equipment of a kind of zinc sulphide or zinc selenide ball cover, including：
Chemical vapor deposition stove, including：
Settling chamber；
Crucible for holding solid zinc source, connects below settling chamber and with settling chamber；
Punch-pin substrate, appearance mirror polish are simultaneously fixed in settling chamber；
Dust chamber above settling chamber and connects settling chamber；
Primary heater, for being heated to settling chamber；And
Secondary heater, for being heated to crucible and solid zinc source being made to become fused zinc source and zinc fume source；
Vacuum extractor, controlled connection dust chamber；
First carrier gas source, it is controlled to be communicated in crucible, for being passed through the first carrier gas and the first carrier gas being made to carry zinc fume source to deposition
In room；And
Second carrier gas source, controlled connection settling chamber, the second carrier gas for sulphur source or selenium source will to be carried be supplied in settling chamber with
The sulphur source or selenium source for making the second carrier gas carrying react in settling chamber with the zinc fume source that the first carrier gas carries and deposit to punch-pin
Substrate and grow to form zinc sulphide or zinc selenide ball cover；
It is characterized in that, the material of punch-pin substrate is isostatic pressing formed graphite.
2. the Preparation equipment of zinc sulphide according to claim 1 or zinc selenide ball cover, which is characterized in that isostatic pressing formed graphite
Grain size is not more than 15 μm.
3. the Preparation equipment of zinc sulphide according to claim 1 or zinc selenide ball cover, which is characterized in that isostatic pressing formed graphite
Density is more than 1.80g/cm3。
4. the Preparation equipment of zinc sulphide according to claim 1 or zinc selenide ball cover, which is characterized in that isostatic pressing formed graphite
Ash content is not more than 200ppm.
5. the Preparation equipment of zinc sulphide according to claim 1 or zinc selenide ball cover, which is characterized in that the first carrier gas and
Two carrier gas are identical.
6. the Preparation equipment of zinc sulphide according to claim 5 or zinc selenide ball cover, which is characterized in that the first carrier gas and
Two carrier gas are argon gas.
7. the Preparation equipment of zinc sulphide according to claim 1 or zinc selenide ball cover, which is characterized in that solid zinc source is pure
Zinc, sulphur source are hydrogen sulfide, and selenium source is hydrogen selenide.
8. the Preparation equipment of zinc sulphide according to claim 1 or zinc selenide ball cover, which is characterized in that the zinc sulphide or
The Preparation equipment of zinc selenide ball cover further includes：
Exhaust gas processing device, it is controlled to be communicated in vacuum extractor.
9. the Preparation equipment of zinc sulphide according to claim 8 or zinc selenide ball cover, which is characterized in that the zinc sulphide or
The Preparation equipment of zinc selenide ball cover further includes：
Cover body above dust chamber and is communicated in dust chamber；
Surge tank between cover body and vacuum extractor and is communicated in dust chamber and vacuum extractor；
Collecting tank positioned at the lower section of surge tank, and is communicated in surge tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711395684.XA CN108165951A (en) | 2017-12-21 | 2017-12-21 | The Preparation equipment of zinc sulphide or zinc selenide ball cover |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711395684.XA CN108165951A (en) | 2017-12-21 | 2017-12-21 | The Preparation equipment of zinc sulphide or zinc selenide ball cover |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108165951A true CN108165951A (en) | 2018-06-15 |
Family
ID=62523175
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711395684.XA Pending CN108165951A (en) | 2017-12-21 | 2017-12-21 | The Preparation equipment of zinc sulphide or zinc selenide ball cover |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108165951A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110529736A (en) * | 2019-09-05 | 2019-12-03 | 广东先导先进材料股份有限公司 | A kind of chemical gas-phase deposition system and feeder and air supply method |
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| US5183689A (en) * | 1991-07-15 | 1993-02-02 | Cvd, Inc. | Process for an improved laminated of znse and zns |
| CN200988773Y (en) * | 2006-12-20 | 2007-12-12 | 北京有色金属研究总院 | Device for preparing high optic uniformity CVDZnS ball cover |
| CN101649449A (en) * | 2009-09-17 | 2010-02-17 | 北京中材人工晶体研究院有限公司 | Preparation method and preparation mould of ZnS/ZnSe composite infrared transmission material |
| CN101760725A (en) * | 2008-12-25 | 2010-06-30 | 北京有色金属研究总院 | Preparation method of zinc sulphide head cap with high optical quality |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110529736A (en) * | 2019-09-05 | 2019-12-03 | 广东先导先进材料股份有限公司 | A kind of chemical gas-phase deposition system and feeder and air supply method |
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