CN200988773Y - Device for preparing high optic uniformity CVDZnS ball cover - Google Patents
Device for preparing high optic uniformity CVDZnS ball cover Download PDFInfo
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- CN200988773Y CN200988773Y CN 200620167585 CN200620167585U CN200988773Y CN 200988773 Y CN200988773 Y CN 200988773Y CN 200620167585 CN200620167585 CN 200620167585 CN 200620167585 U CN200620167585 U CN 200620167585U CN 200988773 Y CN200988773 Y CN 200988773Y
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Abstract
The utility model relates to a device for making CVD high optical uniform zinc sulphide ball, wherein a high temperature vacuum furnace is provided with a zinc tank, a zinc steam nozzle, a sulfureted hydrogen nozzle, a sediment chamber and a discharge box, a concave moulded ball cover mould is arranged on the side wall of the sediment chamber, and a baffle is arranged in the center of the ball cover mould. The ball cover mould and the baffle on the side plate of the sediment chamber of the utility model, which are cooperated with the process route of the device, solves the problems of thickness uniformity and optical quality uniformity in the process of CVD high optical uniform zinc sulphide ball effectively. The utility model can make the Phi270mm x 10mm to Phi50mm x 4mm zinc sulphide ball cover in the sediment chamber of 350mm wide, and the optical quality uniformity is excellent, and is free of obvious impurity. The device has a simple structure, as well as the process parameter and the technical process can be applied in the large-scale production of CVD ZnS ball cover.
Description
Technical field
The utility model relates to the equipment of a kind chemical vapor deposition method (CVD) preparation high optical homogeneity zinc sulphide (ZnS) ball cover, belongs to the field for preparing inorganic block materials equipment.
Background technology
The CVDZnS ball cover is a kind of infrared window of special requirement, and important purposes is arranged in weaponry.Adopt the chemical gas phase vapor deposition process can directly prepare the ball cover of all size, different shape, and the ball cover of preparation has the good advantages such as (near theoretical transmitance) of density height (reaching theoretical density), purity height and optical transmittance, thereby the zinc sulphide ball cover that generally adopts the chemical vapor deposition method growing optics to use in the world.
As shown in Figure 1, the common equipment for preparing zinc sulphide with chemical vapour deposition is to be respectively from bottom to top in vacuum high temperature furnace: zinc pond 21 is crucibles made from high purity graphite, holds highly purified zinc raw material in the crucible; Nozzle 22 is positioned at the top of crucible cover, connects crucible and sediment chamber; Sediment chamber 23 is square tubes of being made by high purity graphite, and inwall is the sedimentary place of zinc sulphide takes place; Dump box 24 is used to prevent that the powder that the space reaction produces from falling into the sediment chamber; Pump-line 25 links to each other with vacuum pump, provides reaction required pressure.
The Heating Zn pond makes the zinc fusing; High-purity argon gas 26 feeds zinc pond 21, carries zinc fume and enters the sediment chamber through nozzle; Hydrogen sulfide 27 enters the sediment chamber through after the argon-dilution through another nozzle 22.Sediment chamber's 23 inwalls are heated to 500-700 ℃, and the pressure in the sediment chamber maintains 30-70 τ.Following chemical reaction takes place in hydrogen sulfide and zinc on the inwall of sediment chamber 23:
H
2S+Zn→ZnS+H
2↑
The ZnS that reaction generates constantly is deposited on sediment chamber's 23 walls, and argon gas, hydrogen and unreacted hydrogen sulfide, zinc fume are extracted out by vacuum pump through dump box 24.General depositing time is 15 to 20 days, and utilization ratio of raw materials is about 70%.
Summary of the invention
The purpose of this utility model provides equipment and the technology thereof that a kind of chemical vapour deposition prepares high optical homogeneity zinc sulphide ball cover, makes prepared zinc sulphide ball cover have thickness evenness and optical quality homogeneity.
For achieving the above object, the utility model is taked following technical scheme:
A kind of chemical vapour deposition prepares the equipment of high optical homogeneity zinc sulphide ball cover, be in vacuum high temperature furnace, to be respectively equipped with the zinc pond from bottom to top, sediment chamber and dump box, wherein, hold the zinc raw material in the zinc pond, the zinc pond is connected to the argon gas inlet pipe, the sediment chamber that cap in the zinc pond passes through zinc fume nozzle and its top connects, and have through the hydrogen sulfide inlet pipe of argon-dilution and connect this sediment chamber by the hydrogen sulfide nozzle, the sediment chamber is suitable for reading to communicate with the end opening of dump box, the zinc pond, sediment chamber and dump box constitute an airtight space, and, outside the suitable for reading straight-through vacuum high temperature furnace of dump box, with pump-line, vacuum pump links to each other, and is provided with well heater in vacuum high temperature furnace, the high efficiency filter that one cover high speed super-fine zinc dust is arranged between vacuum high temperature furnace and vacuum pump has a cover hydrogen sulfide absorption tower behind the vacuum pump.Key structure of the present utility model is: sediment chamber's sidewall is equipped with the ball cover mould of die form, and is provided with baffle plate on the central position of ball cover mould.The installation of baffle plate can hang from dump box.
Adopt the high optical homogeneity zinc sulphide ball cover of preparation, the problem of most critical is growth velocity, thickness evenness and the optical quality homogeneity that how to solve ball cover.At first, because the air-flow that reactant forms forms a dynamic distribution (being called gas flow pattern) in the sediment chamber, thereby the sedimentation rate difference at each position of inwall, sediment chamber, thereby cause inhomogeneous on the thickness.The ununiformity of thickness makes that the space availability ratio of sediment chamber descends, the ball cover growth velocity slows down, the thickness evenness variation, causes the reduction of production efficiency.Secondly, reactant is in the concentration difference at each position of the deposition interior space, and the position of excessive concentration forms the space nucleation easily, causes being mingled with in the product, causes the indicative of local optical downgrade; The time variation of reactant concn causes the timeliness of growth velocity inhomogeneous, the too fast situation of growth velocity appears in indivedual time periods, also can produce and be mingled with, bring disadvantageous effect for the optical quality of product, this is mainly because the zinc steam output is difficult to stable control causes; Three kinds of cloud, graniphyric and point-like are arranged being mingled with in the product usually, the optical quality homogeneity of product is descended, have a strong impact on yield rate.Equipment of the present utility model is the ball cover mould that the die form is housed at sediment chamber's sidewall, and is provided with baffle plate on the central position of ball cover mould, can solve growth velocity, thickness evenness and the optical quality homogeneity of ball cover.
Prepare in the equipment of high optical homogeneity zinc sulphide ball cover in chemical vapour deposition of the present utility model, described ball cover mould is installed in the middle part of sediment chamber's sidewall; Described baffle plate is square, and its length of side is basically less than ball cover mould bore.Wherein, the curvature of ball cover mould is slightly larger than the curvature of ball cover, and the installation site of ball cover mould is positioned at the positive middle part of sediment chamber's sidewall.
Prepare in the equipment of high optical homogeneity zinc sulphide ball cover in chemical vapour deposition of the present utility model, the sediment chamber is that the cross section is the orthogonal graphite tube, the high ratio of length and width is between 1: 2: 3 and 1: 3: 5, and the ratio of the zinc air outlet external diameter of sediment chamber's width and zinc fume nozzle is between 2: 1 to 5: 1.
Prepare in the equipment of high optical homogeneity zinc sulphide ball cover in chemical vapour deposition of the present utility model, the circular hole that the top, sediment chamber communicates with dump box also can exert an influence to the reactant gases flow pattern, and the ratio of the diameter of the circular hole that the top, sediment chamber communicates with dump box and sediment chamber's width is between 1: 1 to 1: 3.
Prepare in the equipment of high optical homogeneity zinc sulphide ball cover in chemical vapour deposition of the present utility model, in addition, dump box designs unreasonable meeting and causes powder wherein to fall into the sediment chamber, can form to be mingled with in product.In order to prevent that the powder that side reaction produces in the dump box from falling into the sediment chamber, in dump box, place the pallet of a circle, pallet is relative with top, sediment chamber circular hole, and the slightly larger in diameter of pallet is in the diameter of top, sediment chamber circular hole.
A kind of processing method that adopts equipment of the present utility model, this method is with to adopt common equipment identical with the method that chemical vapour deposition prepares zinc sulphide, all comprise: forvacuum, intensification, feeding argon gas, feeding are through the hydrogen sulfide of argon-dilution, the growth step of control zinc sulphide ball cover, wherein
Feeding argon gas, feeding in the step of the hydrogen sulfide of argon-dilution, the dilution volume ratio of hydrogen sulfide and argon gas is controlled between 1: 5 to 1: 10; The volume ratio of the argon gas that carries zinc in feeding zinc pond and the argon gas of dilution hydrogen sulfide is controlled between 10: 1 to 5: 1.
In the growth step of control zinc sulphide ball cover, the mol ratio of zinc and hydrogen sulfide is controlled between 1: 1 to 1.5: 1; The pressure-controlling of reaction is at the 3000-10000 handkerchief; The temperature of sedimentary province is controlled between 550-700 ℃; The temperature in zinc pond is controlled between 500-800 ℃, does suitable adjustment according to steam output.
In above-mentioned processing method, described zinc raw material employing purity is 99.9999% zinc ingot metal; The purity of employed hydrogen sulfide is 99.995%; The purity of employed argon gas is 99.9995%.
Adopt the processing method detailed process of equipment of the present utility model as follows:
(1), forvacuum: by vacuum pump equipment is vacuumized, vacuum should be able to be evacuated to below 10 handkerchiefs, and the voltage rise rate less than 10 handkerchiefs per hour.
(2), at first sediment chamber's temperature is risen between 550-700 ℃ slowly, about 4 hours of heating-up time, subsequently zinc pond temperature is slowly risen between 500-550 ℃ about 2-4 of time hour.
(3), the zinc pond feed to set the argon gas of flow, regulates pressure controller, makes chamber pressure reach set(ting)value (3000-10000 handkerchief) gradually, the temperature of zinc pond and sediment chamber all keeps constant during this period.
(4), according to the zinc steam output that monitors, adjust the temperature in zinc pond, up to the zinc steam output that obtains to set, the temperature in zinc pond is controlled between 500-800 ℃.
(5), feed the hydrogen sulfide of setting flow and the gas mixture of argon gas, the dilution volume ratio of hydrogen sulfide and argon gas is controlled between 1: 5 to 1: 10, the volume ratio of the argon gas that carries zinc in feeding zinc pond and the argon gas of dilution hydrogen sulfide is controlled between 10: 1 to 5: 1, and the growth of zinc sulphide ball cover begins.
(6), detected a zinc steam output in the process of growth of zinc sulphide ball cover every one hour, the mol ratio of zinc and hydrogen sulfide is controlled between 1: 1 to 1.5: 1, if change then need zinc pond temperature is made corresponding adjustment (temperature in zinc pond is controlled between 500-800 ℃); At any time the pressure of monitoring reaction chamber, the pressure-controlling of reaction is at the 3000-10000 handkerchief, as changes and in time regulate diaphragm valve before the vacuum pump, and what keep-up pressure is stable; It is constant that whole growth process sediment chamber temperature keeps, and the temperature of sedimentary province is controlled between 550-700 ℃.
(7) contain a large amount of super-fine zinc dusts in the waste gas of from cvd furnace, extracting out and have neither part nor lot in the hydrogen sulfide of reaction, be through high efficiency filter device (filtration efficiency reaches more than 99%) and the processing of hydrogen sulfide absorption tower, prevent the mechanical pump fault and to the pollution of environment.
Its process was generally 10 to 20 days.Promptly finish the production process that a chemical vapour deposition prepares high optical homogeneity zinc sulphide ball cover.
6, in the process of growth if pressure or zinc steam output uncontrollable, indication growth failure, process stops; Otherwise, be generally 10 to 20 days by the time that lasts till setting described in 5.
The utility model has the advantages that:
The utility model adopts sediment chamber's side plate ball cover mould, the baffle arrangement that is different from prior art, operational path in conjunction with this equipment of being suitable for has solved present chemical vapour deposition effectively and has prepared thickness evenness and optical quality homogeneity question in the zinc sulphide ball cover technology.In equipment of the present utility model, can prepare at present the zinc sulphide ball cover of Φ 270mm * 10mm～φ 50mm * 4mm in the wide sediment chamber of 350mm, and optical quality has good uniformity, there is not tangible inclusion.Device structure of the present utility model, and processing parameter and technological process can be applied in the production of extensive CVDZnS ball cover fully.
Description of drawings
Fig. 1 is the known equipment synoptic diagram for preparing zinc sulphide with chemical vapour deposition
Fig. 2 prepares the equipment synoptic diagram of high optical homogeneity zinc sulphide ball cover for chemical vapour deposition of the present utility model
Embodiment
As shown in Figure 2, a kind of chemical vapour deposition of the present utility model prepares the equipment of high optical homogeneity zinc sulphide ball cover, be in vacuum high temperature furnace, to be respectively equipped with zinc pond 1 from bottom to top, nozzle 2, sediment chamber 3, ball cover mould 4, baffle plate 5 and dump box 8, wherein, hold the zinc raw material in the zinc pond 1, zinc pond 1 is connected to argon gas inlet pipe 7, cap in zinc pond 1 is connected by the sediment chamber 3 of zinc fume nozzle 2 with its top, and have through the hydrogen sulfide inlet pipe 6 of argon-dilution and connect this sediment chamber 3 by hydrogen sulfide nozzle 2 ', the end opening of the suitable for reading and dump box 8 of sediment chamber 3 communicates, zinc pond 1, sediment chamber 3 and dump box 8 constitute an airtight space, and, outside the suitable for reading straight-through vacuum high temperature furnace of dump box 8, with pump-line 9, high efficiency filter 12, vacuum pump 13, hydrogen sulfide absorption tower 14 links to each other, and is provided with well heater 10 in vacuum high temperature furnace, and zinc fume nozzle 2 is a concentric structure with the structure of hydrogen sulfide nozzle 2 ', and hydrogen sulfide nozzle 2 ' is a central nozzle, and zinc fume nozzle 2 is the outer shroud nozzle.Key structure of the present utility model is: ball cover mould 4 adopts die, and mounting height is positioned at 3 sidewall centers, sediment chamber, and baffle plate 5 is square, and the length of side is slightly less than ball cover mould bore, and mounting height is positioned near the ball cover mold center.
Prepare in the equipment of high optical homogeneity zinc sulphide ball cover in chemical vapour deposition of the present utility model, adopt the graphite resistance heating, rotary-vane vaccum pump is bled.Hydrogen sulfide through argon-dilution directly enters sediment chamber 3 through hydrogen sulfide nozzle 2 ', and other one road argon gas at first feeds the zinc pond, carries zinc fume and enters sediment chamber 3 through zinc fume nozzle 2.Hydrogen sulfide and the zinc inwall in the sediment chamber reacts and deposits,
The equation of reaction is: H
2S+Zn → ZnS+H
2↑
Reacted residual gas enters dump box 8, and here the reactant air thorough mixing can have living space to react and take place.Tail gas enters a high efficiency filter 12 through pump-line 9 and filters zinc powder, is extracted out by vacuum pump 13, disposes hydrogen sulfide by hydrogen sulfide absorption tower 14 then, enters atmosphere at last.
The production whole process (comprising preparatory stage, growth phase, ending phase) that chemical vapour deposition of the present utility model prepares the equipment of high optical homogeneity zinc sulphide ball cover is as follows:
The first step: preparatory stage
1, corrosion treatment sediment chamber and zinc crucible: soak sediment chamber and crucible 8-12 hour with chloroazotic acid, boil cleaning with deionized water subsequently, until neutral, 100-110 ℃ of baking is 12-24 hour in baking oven.
2, corrosion treatment zinc ingot metal:, remove oxide on surface with 1: 1 salt acid soak zinc ingot metal 10-30 minute.
3, the surface treatment of sediment chamber and ball cover: use a kind of colloid in the sediment chamber and the ball cover inner wall surface form the slick high-purity coating of a kind of densification, the effect of this coating is to repair the microlesion of sediment chamber and ball cover inwall and can make the disengaging smoothly behind growth ending of zinc sulphide and sediment chamber's inwall and ball cover.
4, zinc crucible, nozzle, sediment chamber and ball cover, baffle plate and dump box carefully are installed, are made it become a closed system, later reactant gas and argon gas only flow in this system, do not leak into beyond this system.
5, forvacuum: equipment installs final vacuum and should be able to be evacuated to below 10 handkerchiefs, and the voltage rise rate less than 10 handkerchiefs per hour.
Second step: growth phase
1, at first sediment chamber's temperature is risen between 550-700 ℃ slowly, about 4 hours of heating-up time, subsequently zinc pond temperature is slowly risen between 500-550 ℃ about 2-4 of time hour.
2, the zinc pond feeds the argon gas of setting flow, regulates pressure controller, makes chamber pressure reach set(ting)value gradually, and the temperature of zinc pond and sediment chamber all keeps constant during this period.
3, according to the zinc steam output that monitors, adjust the temperature in zinc pond, up to the zinc steam output that obtains to set, the temperature in zinc pond is controlled between 500-800 ℃.
4, feed the hydrogen sulfide of setting flow and the gas mixture of argon gas, the dilution volume ratio of hydrogen sulfide and argon gas is controlled between 1: 5 to 1: 10, the volume ratio of the argon gas that carries zinc in feeding zinc pond and the argon gas of dilution hydrogen sulfide is controlled between 10: 1 to 5: 1, and the growth of zinc sulphide ball cover begins.
5, detected a zinc steam output in the process of growth of zinc sulphide ball cover every one hour, the mol ratio of zinc and hydrogen sulfide is controlled between 1: 1 to 1.5: 1, if change then need zinc pond temperature is made corresponding adjustment (temperature in zinc pond is controlled between 500-800 ℃); At any time the pressure of monitoring reaction chamber, the pressure-controlling of reaction is at the 3000-10000 handkerchief, as changes and in time regulate diaphragm valve before the vacuum pump, and what keep-up pressure is stable; It is constant that whole growth process sediment chamber temperature keeps, and the temperature of sedimentary province is controlled between 550-700 ℃.
6, in the process of growth if pressure or zinc steam output uncontrollable, indication growth failure, process stops; Otherwise, be generally 10 to 20 days by the time that lasts till setting described in 5.
The 3rd step: ending phase
1, the well heater in zinc pond outage, H is closed in cooling naturally
2S gas.
2, total system was vacuumized 1-2 hour the hydrogen sulfide of remnants in the discharge system.
3, with argon gas system is charged to a normal atmosphere.
4, the cooling process that the sediment chamber carry out is set, rate of temperature fall are controlled between 6 ℃/h to 20 ℃/h, until reducing to room temperature.
In sum, chemical vapor deposition method prepare the key issue of zinc sulphide ball cover be how to solve in the sediment chamber ball cover growth velocity with and thickness evenness and optical quality homogeneity.The utility model adopts cooperating of cooperating of ball cover former and baffle plate and structure of nozzle and deposition chamber dimension, reactant gases flow pattern in the sediment chamber has been played conclusive effect, and adopted the processing method that adapts with equipment of the present utility model, effectively solve these two problems, thereby prepare the thinization zinc ball cover of high optical homogeneity.
Claims (5)
1, a kind of chemical vapour deposition prepares the equipment of high optical homogeneity zinc sulphide ball cover, be in vacuum high temperature furnace, to be respectively equipped with the zinc pond from bottom to top, the sediment chamber, and dump box, wherein, hold the zinc raw material in the zinc pond, the zinc pond is connected to the argon gas inlet pipe, the sediment chamber that cap in the zinc pond passes through zinc fume nozzle and its top connects, and have through the hydrogen sulfide inlet pipe of argon-dilution and connect this sediment chamber by the hydrogen sulfide nozzle, the end opening of the suitable for reading and dump box of sediment chamber communicates, the zinc pond, sediment chamber and dump box constitute an airtight space, and, outside the suitable for reading straight-through vacuum high temperature furnace of dump box, with pump-line, high efficiency filter, vacuum pump, the hydrogen sulfide absorption tower links to each other, in vacuum high temperature furnace, be provided with well heater, it is characterized in that: sediment chamber's sidewall is equipped with the ball cover mould of die form, and is provided with baffle plate on the central position of ball cover mould.
2, chemical vapour deposition according to claim 1 prepares the equipment of high optical homogeneity zinc sulphide ball cover, and it is characterized in that: described ball cover mould is installed in the middle part of sediment chamber's sidewall; Described baffle plate is square, and its length of side is basically less than ball cover mould bore.
3, chemical vapour deposition according to claim 1 and 2 prepares the equipment of high optical homogeneity zinc sulphide ball cover, it is characterized in that: described sediment chamber is that the cross section is the orthogonal graphite tube, the high ratio of length and width is between 1: 2: 3 and 1: 2: 5, and the ratio of the zinc air outlet external diameter of sediment chamber's width and zinc fume nozzle is between 2: 1 to 5: 1.
4, chemical vapour deposition according to claim 3 prepares the equipment of high optical homogeneity zinc sulphide ball cover, it is characterized in that: the diameter of the circular hole that top, described sediment chamber communicates with dump box and the ratio of sediment chamber's width are between 1: 1 to 1: 3.
5, chemical vapour deposition according to claim 4 prepares the equipment of high optical homogeneity zinc sulphide ball cover, it is characterized in that: the pallet of in described dump box, placing a circle, pallet is relative with top, sediment chamber circular hole, and the slightly larger in diameter of pallet is in the diameter of top, sediment chamber circular hole.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200620167585 CN200988773Y (en) | 2006-12-20 | 2006-12-20 | Device for preparing high optic uniformity CVDZnS ball cover |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200620167585 CN200988773Y (en) | 2006-12-20 | 2006-12-20 | Device for preparing high optic uniformity CVDZnS ball cover |
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| CN200988773Y true CN200988773Y (en) | 2007-12-12 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760725B (en) * | 2008-12-25 | 2011-09-07 | 北京有色金属研究总院 | Preparation method of zinc sulphide head cap with high optical quality |
| CN101759225B (en) * | 2008-12-25 | 2012-02-29 | 北京有色金属研究总院 | Device for growing ZnS at low temperature by chemical vapor deposition and technique thereof |
| CN106735665A (en) * | 2016-12-29 | 2017-05-31 | 武汉工程大学 | A kind of device for welding cvd diamond and hard alloy, method and its application |
| CN108165951A (en) * | 2017-12-21 | 2018-06-15 | 清远先导材料有限公司 | The Preparation equipment of zinc sulphide or zinc selenide ball cover |
| CN109250749A (en) * | 2017-07-14 | 2019-01-22 | 清远先导材料有限公司 | The production method of zinc sulphide |
| CN113321236A (en) * | 2020-07-31 | 2021-08-31 | 上海交通大学 | Method for preparing zinc sulfide ultrafine powder by using zinc skins of waste zinc-manganese battery |
-
2006
- 2006-12-20 CN CN 200620167585 patent/CN200988773Y/en not_active Expired - Lifetime
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760725B (en) * | 2008-12-25 | 2011-09-07 | 北京有色金属研究总院 | Preparation method of zinc sulphide head cap with high optical quality |
| CN101759225B (en) * | 2008-12-25 | 2012-02-29 | 北京有色金属研究总院 | Device for growing ZnS at low temperature by chemical vapor deposition and technique thereof |
| CN106735665A (en) * | 2016-12-29 | 2017-05-31 | 武汉工程大学 | A kind of device for welding cvd diamond and hard alloy, method and its application |
| CN106735665B (en) * | 2016-12-29 | 2019-03-08 | 武汉工程大学 | A kind of device for welding cvd diamond and hard alloy, method and its application |
| CN109250749A (en) * | 2017-07-14 | 2019-01-22 | 清远先导材料有限公司 | The production method of zinc sulphide |
| CN108165951A (en) * | 2017-12-21 | 2018-06-15 | 清远先导材料有限公司 | The Preparation equipment of zinc sulphide or zinc selenide ball cover |
| CN113321236A (en) * | 2020-07-31 | 2021-08-31 | 上海交通大学 | Method for preparing zinc sulfide ultrafine powder by using zinc skins of waste zinc-manganese battery |
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