CN219363794U - A chemical vapor deposition furnace for preparing ZnSe - Google Patents
A chemical vapor deposition furnace for preparing ZnSe Download PDFInfo
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- CN219363794U CN219363794U CN202320625756.XU CN202320625756U CN219363794U CN 219363794 U CN219363794 U CN 219363794U CN 202320625756 U CN202320625756 U CN 202320625756U CN 219363794 U CN219363794 U CN 219363794U
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- SBIBMFFZSBJNJF-UHFFFAOYSA-N selenium;zinc Chemical compound [Se]=[Zn] SBIBMFFZSBJNJF-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 238000005229 chemical vapour deposition Methods 0.000 title claims abstract description 14
- 238000000151 deposition Methods 0.000 claims abstract description 93
- 230000008021 deposition Effects 0.000 claims abstract description 90
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- 239000000428 dust Substances 0.000 claims description 11
- 238000004321 preservation Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 abstract description 17
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 14
- SPVXKVOXSXTJOY-UHFFFAOYSA-N selane Chemical compound [SeH2] SPVXKVOXSXTJOY-UHFFFAOYSA-N 0.000 abstract description 14
- 229910000058 selane Inorganic materials 0.000 abstract description 14
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 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 8
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052786 argon Inorganic materials 0.000 abstract description 7
- 239000011701 zinc Substances 0.000 abstract description 7
- 229910052725 zinc Inorganic materials 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000000463 material Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000010586 diagram Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000035515 penetration Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- -1 that is Chemical compound 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Physical Vapour Deposition (AREA)
Abstract
Description
技术领域technical field
本实用新型属于硒化锌制备技术领域,具体涉及一种制备ZnSe的化学气相沉积炉。The utility model belongs to the technical field of zinc selenide preparation, in particular to a chemical vapor deposition furnace for preparing ZnSe.
背景技术Background technique
ZnSe(硒化锌)呈黄色结晶性粉末,主要用于制造激光器中的光学器件,其具有散射损失极低等优点,并且对热冲击具有很高的承受能力。传统ZnSe生产设备在生产过程中原料利用率低,产品在沉积室停留时间短、产品转化率低、均匀性差。如中国实用新型专利公开了一种化学气相沉积炉(申请号:201821327035.6),其利用化学气相沉积法生产ZnSe,虽然一定程度上提高了产品转化率,但其生产方式以及反应过程优待进一步提升优化。为此,研发一种提高产品转化率的制备ZnSe的化学气相沉积炉是非常必要的。ZnSe (Zinc Selenide) is a yellow crystalline powder and is mainly used in the manufacture of optical devices in lasers. It has the advantages of extremely low scattering loss and high tolerance to thermal shock. Traditional ZnSe production equipment has low raw material utilization rate in the production process, short residence time of products in the deposition chamber, low product conversion rate and poor uniformity. For example, a Chinese utility model patent discloses a chemical vapor deposition furnace (application number: 201821327035.6), which uses chemical vapor deposition to produce ZnSe. Although the product conversion rate has been improved to a certain extent, its production method and reaction process should be further optimized. . For this reason, it is very necessary to develop a chemical vapor deposition furnace for preparing ZnSe that improves the product conversion rate.
实用新型内容Utility model content
本实用新型的目的在于提供一种制备ZnSe的化学气相沉积炉。The purpose of the utility model is to provide a chemical vapor deposition furnace for preparing ZnSe.
本实用新型的目的是这样实现的,包括自下而上依次设置的坩埚、坩埚盖、沉积室、收料盒、导气管,坩埚外设有下加热室,下加热室用于加热坩埚,沉积室、收料盒外设有上加热室,上加热室用于加热沉积室、收料盒,收料盒顶部以及底部分别对应设置有气口,所述坩埚盖中心设有孔洞,所述坩埚盖下表面之孔洞四周布设有第一进气管,第一进气管通过坩埚盖内埋设的管路与坩埚盖侧面的供气口连通,第一进气管管口位于坩埚内,坩埚盖上表面之孔洞四周布设有第二进气管,第二进气管通过坩埚盖内埋设的管路与坩埚盖侧面的供气口连通,第二进气管管口穿过沉积室底部小孔伸入至沉积室内,所述孔洞之上盖设有半球形罩,半球形罩表面均布有透过孔,半球形罩穿过沉积室底部中心孔伸入至沉积室内;The purpose of the utility model is achieved in this way, including a crucible, a crucible cover, a deposition chamber, a material receiving box, and an air guide tube arranged sequentially from bottom to top, and a lower heating chamber is arranged outside the crucible, which is used for heating the crucible, depositing There is an upper heating chamber outside the chamber and the receiving box, the upper heating chamber is used to heat the deposition chamber and the receiving box, the top and the bottom of the receiving box are respectively provided with gas ports, the center of the crucible cover is provided with a hole, and the crucible cover The hole on the lower surface is surrounded by a first air intake pipe. The first air intake pipe communicates with the gas supply port on the side of the crucible cover through the pipeline embedded in the crucible cover. The mouth of the first air intake pipe is located in the crucible. A second air intake pipe is arranged around, and the second air intake pipe communicates with the gas supply port on the side of the crucible cover through the pipeline buried in the crucible cover, and the nozzle of the second air intake pipe extends into the deposition chamber through a small hole at the bottom of the deposition chamber, so that The upper cover of the hole is provided with a hemispherical cover, and the surface of the hemispherical cover is evenly distributed with through holes, and the hemispherical cover extends into the deposition chamber through the central hole at the bottom of the deposition chamber;
所述沉积室内的两侧分别自下而上水平设置有呈板状的沉积模具,左右相对应的每一组沉积模具之间上下错位,沉积模具上均布有透过孔。Both sides of the deposition chamber are respectively provided with plate-shaped deposition molds horizontally from bottom to top, each set of deposition molds corresponding to the left and right are misaligned up and down, and the deposition molds are evenly distributed with through holes.
所述沉积室两侧之外部分别纵向设置有回流管,且回流管位于上加热室内,回流管上端与沉积室内的上部连通,回流管下端与沉积室内的底部连通。The outer sides of the deposition chamber are respectively longitudinally provided with return pipes, and the return pipes are located in the upper heating chamber, the upper end of the return pipe communicates with the upper part of the deposition chamber, and the lower end of the return pipe communicates with the bottom of the deposition chamber.
优选地,所述沉积模具有四块,自下而上排列的第一沉积模具边缘、第二沉积模具边缘均与沉积室轴线之间有间距,第一沉积模具边缘、第二沉积模具边缘均与沉积室轴线重合。Preferably, the deposition mold has four pieces, the edges of the first deposition mold and the edges of the second deposition mold arranged from bottom to top have a distance from the axis of the deposition chamber, and the edges of the first deposition mold and the edge of the second deposition mold Coincident with the axis of the deposition chamber.
优选地,所述收料盒内设有集尘槽,集尘槽之上设有盖板,盖板上设有透过孔,所述下加热室以及上加热室外侧设有保温室,保温室起到保温的作用,具体可使用本领域技术人员熟知的保温材料;保温室外侧设有冷却室,冷却室用于给本化学气相沉积炉降温,具体可采用水冷结构。Preferably, a dust collection tank is provided in the receiving box, a cover plate is provided on the dust collection tank, and a through hole is provided on the cover board, and a heat preservation room is provided outside the lower heating chamber and the upper heating chamber to keep the heat The chamber plays the role of heat preservation, and specifically, insulation materials well known to those skilled in the art can be used; a cooling chamber is provided outside the heat preservation chamber, and the cooling chamber is used to cool down the chemical vapor deposition furnace, and specifically, a water-cooled structure can be used.
优选地,沉积模具与沉积室内壁对应的一侧为楔形结构,沉积模具的楔形结构卡入沉积室内壁的楔形凹槽中,这种可拆装的结构,使得模具尺寸、厚度可以灵活选择,更具灵活性。Preferably, the side of the deposition mold corresponding to the inner wall of the deposition chamber has a wedge-shaped structure, and the wedge-shaped structure of the deposition mold snaps into the wedge-shaped groove on the inner wall of the deposition chamber. This detachable structure allows the mold size and thickness to be flexibly selected. More flexibility.
本实用新型的有益效果:The beneficial effects of the utility model:
1、本实用新型第一进气管、第二进气管均通入硒化氢和氩气,即在坩埚内硒化氢与锌蒸汽发生反应,生成的ZnSe以及部分未反应的硒化氢、锌蒸汽进入沉积室,再与第二进气管通入沉积室的硒化氢和氩气接触反应,使得硒化锌的生成率提高;1. Both the first intake pipe and the second intake pipe of the utility model are fed with hydrogen selenide and argon, that is, hydrogen selenide reacts with zinc vapor in the crucible, and the generated ZnSe and part of unreacted hydrogen selenide and zinc The steam enters the deposition chamber, and then contacts and reacts with hydrogen selenide and argon gas that are passed into the deposition chamber through the second inlet pipe, so that the formation rate of zinc selenide is increased;
2、均布有透过孔的半球形罩可使得由坩埚进入沉积室的气体均匀分布,这种出口呈放射状的流动方式可使气流覆盖沉积模具的边缘,有利于提高产品转化率、均匀性、原料利用率;2. The hemispherical cover evenly distributed with penetration holes can make the gas entering the deposition chamber from the crucible evenly distributed. This radial flow mode of the outlet can make the gas flow cover the edge of the deposition mold, which is conducive to improving the product conversion rate and uniformity , Raw material utilization rate;
3、沉积模具采用四块,第三、第四沉积模具可以进一步沉积第一、第二沉积模具未沉积的物料,进一步提高产品转化率、原料利用率;并且沉积模具双面均可沉积;3. Four deposition molds are used. The third and fourth deposition molds can further deposit the undeposited materials of the first and second deposition molds, further improving product conversion rate and raw material utilization rate; and both sides of the deposition mold can be deposited;
4、沉积室的回流管充分利用沉积室的气流,从而提升转化率;回流管在上加热室内部,温度控制稳定;本实用新型还可设置保温室和冷却室,整体结构设计合理,对称,容易安装;除此之外,本实用新型还可以用于制备其他粉体或者ZnS晶体等。4. The return pipe of the deposition chamber makes full use of the airflow in the deposition chamber, thereby improving the conversion rate; the return pipe is inside the upper heating chamber, and the temperature control is stable; the utility model can also be equipped with a heat preservation chamber and a cooling chamber, and the overall structure design is reasonable and symmetrical, Easy to install; in addition, the utility model can also be used to prepare other powders or ZnS crystals.
附图说明Description of drawings
图1为本实用新型的剖面结构示意图;Fig. 1 is the sectional structure schematic diagram of the present utility model;
图2为坩埚盖的表面结构示意图;Fig. 2 is the surface structure schematic diagram of crucible lid;
图3为坩埚盖的底面结构示意图;Fig. 3 is the bottom surface structure schematic diagram of crucible lid;
图4为半球形罩的俯视结构示意图;Fig. 4 is a top view structural schematic diagram of a hemispherical cover;
图5为沉积模具的俯视结构示意图;Fig. 5 is a top view structural schematic diagram of a deposition mold;
图6为沉积模具与沉积室内壁之间的楔形连接结构示意图;Fig. 6 is a schematic diagram of the wedge-shaped connection structure between the deposition mold and the inner wall of the deposition chamber;
图中:1-坩埚,2-坩埚盖,3-沉积室,4-收料盒,5-导气管,6-下加热室,7-上加热室,8-孔洞,9-第一进气管,10-第二进气管,11-半球形罩,12-沉积模具,13-回流管,14-集尘槽,15-盖板,16-保温室,17-冷却室。In the figure: 1-crucible, 2-crucible cover, 3-deposition chamber, 4-receiving box, 5-air duct, 6-lower heating chamber, 7-upper heating chamber, 8-hole, 9-first air intake pipe , 10-second air intake pipe, 11-hemispherical cover, 12-deposition mold, 13-return pipe, 14-dust collection tank, 15-cover plate, 16-insulation chamber, 17-cooling chamber.
具体实施方式Detailed ways
下面结合实施例及附图对本实用新型作进一步的说明,但不以任何方式对本实用新型加以限制,基于本实用新型教导所作的任何变换或替换,均属于本实用新型的保护范围。The utility model will be further described below in conjunction with the embodiments and accompanying drawings, but the utility model is not limited in any way. Any transformation or replacement based on the teaching of the utility model belongs to the protection scope of the utility model.
实施例1Example 1
如附图1~图3所示,本实施例制备ZnSe的化学气相沉积炉包括自下而上依次设置的坩埚1、坩埚盖2、沉积室3、收料盒4、导气管5,坩埚1外设有下加热室6,沉积室3、收料盒4外设有上加热室7,收料盒4顶部以及底部分别对应设置有气口,所述坩埚盖2中心设有孔洞8,所述坩埚盖2下表面之孔洞8四周布设有第一进气管9,第一进气管9通过坩埚盖2内埋设的管路与坩埚盖2侧面的供气口连通,第一进气管9管口位于坩埚1内,坩埚盖2上表面之孔洞8四周布设有第二进气管10,第二进气管10通过坩埚盖2内埋设的管路与坩埚盖2侧面的供气口连通,第二进气管10管口穿过沉积室3底部小孔伸入至沉积室3内,所述孔洞8之上盖设有半球形罩11,半球形罩11表面均布有透过孔,半球形罩11穿过沉积室3底部中心孔伸入至沉积室3内;As shown in accompanying drawings 1 to 3, the chemical vapor deposition furnace for preparing ZnSe in this embodiment includes a crucible 1, a crucible cover 2, a deposition chamber 3, a receiving box 4, an air guide tube 5, and a crucible 1 arranged in sequence from bottom to top. A lower heating chamber 6 is arranged outside, an upper heating chamber 7 is arranged outside the deposition chamber 3 and the receiving box 4, the top and bottom of the receiving box 4 are respectively provided with gas ports, and the center of the crucible cover 2 is provided with a hole 8, the The hole 8 on the lower surface of the crucible cover 2 is surrounded by a first air intake pipe 9. The first air intake pipe 9 communicates with the gas supply port on the side of the crucible cover 2 through the pipeline embedded in the crucible cover 2. The mouth of the first air intake pipe 9 is located at In the crucible 1, a second air intake pipe 10 is arranged around the hole 8 on the upper surface of the crucible cover 2, and the second air intake pipe 10 communicates with the gas supply port on the side of the crucible cover 2 through the pipeline buried in the crucible cover 2. 10 The nozzle passes through the small hole at the bottom of the deposition chamber 3 and extends into the deposition chamber 3. The upper cover of the hole 8 is provided with a hemispherical cover 11, and the surface of the hemispherical cover 11 is evenly distributed with through holes, and the hemispherical cover 11 passes through. extend into the deposition chamber 3 through the center hole at the bottom of the deposition chamber 3;
所述沉积室3内的两侧分别自下而上水平设置有呈板状的沉积模具12,左右相对应的每一组沉积模具12之间上下错位,沉积模具12上均布有透过孔。Plate-shaped deposition molds 12 are arranged horizontally on both sides of the deposition chamber 3 from bottom to top, and each set of deposition molds 12 corresponding to the left and right is misaligned up and down, and the deposition molds 12 are evenly distributed with penetration holes. .
所述沉积室3两侧之外部分别纵向设置有回流管13,且回流管13位于上加热室7内,回流管13上端与沉积室3内的上部连通,回流管13下端与沉积室3内的底部连通。The outside of the two sides of the deposition chamber 3 is respectively longitudinally provided with a return pipe 13, and the return pipe 13 is located in the upper heating chamber 7, the upper end of the return pipe 13 communicates with the upper part of the deposition chamber 3, and the lower end of the return pipe 13 communicates with the upper part of the deposition chamber 3. connected at the bottom.
实施例2Example 2
本实施例制备ZnSe的化学气相沉积炉是在实施例1的基础上,所述沉积模具12有四块,自下而上排列的第一沉积模具边缘、第二沉积模具边缘均与沉积室3轴线之间有间距,第一沉积模具边缘、第二沉积模具边缘均与沉积室3轴线重合;所述收料盒4内设有集尘槽14,集尘槽14之上设有盖板15,盖板15上设有透过孔,所述下加热室6以及上加热室7外侧设有保温室16,保温室16外侧设有冷却室17。The present embodiment prepares the chemical vapor deposition furnace of ZnSe on the basis of embodiment 1, and described deposition mold 12 has four pieces, and the first deposition mold edge that arranges from bottom to top, the second deposition mold edge are all connected with deposition chamber 3 There is a distance between the axes, and the edge of the first deposition mold and the edge of the second deposition mold coincide with the axis of the deposition chamber 3; a dust collection tank 14 is provided in the collection box 4, and a cover plate 15 is provided on the dust collection tank 14 , The cover plate 15 is provided with through holes, the outer side of the lower heating chamber 6 and the upper heating chamber 7 is provided with a heat preservation chamber 16 , and the outer side of the heat preservation chamber 16 is provided with a cooling chamber 17 .
本实用新型工作原理和工作过程:将固体原料锌装到坩埚1里,并安装坩埚盖2及相应供气管道,以及沉积室3、收料盒4、导气管5等部件,启动与化学气相沉积炉配套的电气控制系统,各设备开始运行;硒化氢和氩气通过第一进气管9进入坩埚1内,在氩气保护下,硒化氢与锌蒸汽发生反应,生成的ZnSe以及部分未反应的硒化氢、锌蒸汽经半球形罩11的透过孔进入沉积室3,与通过第二进气管10送入沉积室3的保护气体氩气和硒化氢气体进一步接触并反应,使得硒化锌的生成率提高;硒化氢在沉积室3的沉积模具12上沉积,使得大部分硒化锌沉积到沉积室3内;部分气体通过回流管13再次送回沉积室3底部进一步反应;部分未沉积的硒化锌和未反应的硒化氢随着气流进入到收料盒4内,收料盒4和集尘槽14对部分硒化锌粉尘进行收集,其余未收集的硒化锌粉尘由导气管5进入到后端收尘系统进一步收集,尾气通过真空系统进入到尾气处理系统进行处理,达标外排。The working principle and working process of the utility model: put the solid raw material zinc into the crucible 1, and install the crucible cover 2 and the corresponding gas supply pipeline, as well as the deposition chamber 3, the receiving box 4, the air guide tube 5 and other components, start and chemical gas phase The electrical control system supporting the deposition furnace, and each equipment starts to operate; hydrogen selenide and argon enter the crucible 1 through the first inlet pipe 9, and under the protection of argon, hydrogen selenide reacts with zinc vapor, and the generated ZnSe and some Unreacted hydrogen selenide and zinc vapor enter the deposition chamber 3 through the penetration hole of the hemispherical cover 11, and further contact and react with the protective gas argon and hydrogen selenide gas sent into the deposition chamber 3 through the second inlet pipe 10, The generation rate of zinc selenide is improved; hydrogen selenide is deposited on the deposition mold 12 of deposition chamber 3, and most of zinc selenide is deposited in deposition chamber 3; Reaction: part undeposited zinc selenide and unreacted hydrogen selenide enter in the receiving box 4 along with the air flow, receiving box 4 and dust collection tank 14 collect part zinc selenide dust, all the other uncollected selenium Zinc dust enters the back-end dust collection system from the air duct 5 for further collection, and the exhaust gas enters the exhaust gas treatment system through the vacuum system for treatment, and is discharged out when it reaches the standard.
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