CN102030330A - Polysilicon reduction furnace with outlet gas collector - Google Patents
Polysilicon reduction furnace with outlet gas collector Download PDFInfo
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- CN102030330A CN102030330A CN 201010542483 CN201010542483A CN102030330A CN 102030330 A CN102030330 A CN 102030330A CN 201010542483 CN201010542483 CN 201010542483 CN 201010542483 A CN201010542483 A CN 201010542483A CN 102030330 A CN102030330 A CN 102030330A
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- 229910021420 polycrystalline silicon Inorganic materials 0.000 title claims description 29
- 229920005591 polysilicon Polymers 0.000 title description 23
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 18
- 229910002804 graphite Inorganic materials 0.000 claims description 10
- 239000010439 graphite Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000007789 gas Substances 0.000 description 67
- 239000000498 cooling water Substances 0.000 description 18
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 9
- 239000005052 trichlorosilane Substances 0.000 description 9
- 239000001257 hydrogen Substances 0.000 description 7
- 229910052739 hydrogen Inorganic materials 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 6
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 4
- 239000005049 silicon tetrachloride Substances 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 3
- 238000005229 chemical vapour deposition Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000011863 silicon-based powder Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
Description
技术领域technical field
本发明涉及一种多晶硅的生产设备,特别涉及一种多晶硅还原炉。The invention relates to a polysilicon production equipment, in particular to a polysilicon reduction furnace.
背景技术Background technique
目前多晶硅生产企业主要采用改良西门子法。该方法的生产流程是利用氯气和氢气合成氯化氢(或外购氯化氢),氯化氢和冶金硅粉在一定温度下合成三氯氢硅,分离精馏提纯后的三氯氢硅进入还原炉被氢气还原,通过化学气相沉积反应生产高纯多晶硅。该流程包括五个主要环节:三氯氢硅的合成、三氯氢硅的精馏提纯、三氯氢硅的氢还原、尾气的回收和四氯化硅的氢化分离。At present, polysilicon production enterprises mainly adopt the improved Siemens method. The production process of this method is to use chlorine and hydrogen to synthesize hydrogen chloride (or purchased hydrogen chloride), hydrogen chloride and metallurgical silicon powder to synthesize trichlorosilane at a certain temperature, and the trichlorosilane after separation and rectification purification enters the reduction furnace and is reduced by hydrogen , to produce high-purity polysilicon by chemical vapor deposition reaction. The process includes five main links: synthesis of trichlorosilane, rectification and purification of trichlorosilane, hydrogen reduction of trichlorosilane, recovery of tail gas and hydrogenation separation of silicon tetrachloride.
其中,三氯氢硅的氢还原在大型钟罩式还原炉中进行。还原炉主要由炉体、硅芯、气路系统、电极加热系统和冷却系统组成,如图2所示。氢气和三氯氢硅混合气体经由进气管及其上设置的喷嘴进入还原炉内,混合气体高速向上喷射过程中在通电高温的硅芯表面发生化学气相沉积反应生成高纯多晶硅,得到棒状多晶硅产品,同时生成四氯化硅、二氯二氢硅、氯化氢等副产物尾气,尾气从底盘上设置的出气口和出气管排出。Among them, the hydrogen reduction of trichlorosilane is carried out in a large bell-type reduction furnace. The reduction furnace is mainly composed of furnace body, silicon core, gas system, electrode heating system and cooling system, as shown in Figure 2. The mixed gas of hydrogen and trichlorosilane enters the reduction furnace through the inlet pipe and the nozzles set on it. During the process of high-speed upward jetting of the mixed gas, a chemical vapor deposition reaction occurs on the surface of the energized and high-temperature silicon core to form high-purity polysilicon, and a rod-shaped polysilicon product is obtained. , and at the same time generate silicon tetrachloride, dichlorodihydrosilane, hydrogen chloride and other by-product tail gas, and the tail gas is discharged from the gas outlet and the gas outlet pipe set on the chassis.
现有技术存在的主要问题有:气路系统设置不合理,如图2所示,进气口9与出气口10′均设置在还原炉的底盘上,造成炉内底部由于气体扩散而发生短路,部分气体未与硅芯充分接触发生反应就直接经出气口排出,炉内气体分布不均匀,最终导致生成的多晶硅棒上下粗细不均匀,影响产品质量。尾气是否能够被均匀地收集和排出对于还原炉的操作性能和生成多晶硅棒产品的质量有非常大的影响,因此需要对还原炉的气体出口结构重新进行设计。中国专利CN201105995Y公开的改进型多晶硅还原炉,其特征是在底盘上增加一个尾气出气导管,使得气体出口与进口位置不在同一个平面上;中国专利CN101476153A公开的多晶硅的还原生产工艺及其生产用还原炉,将出气口设置在还原炉顶端,采用5~7管口式结构。这些结构的改变虽然较之传统还原炉内由于气体在底部扩散造成短路的现象有一定的改善作用,但并没有根本解决炉内气体分布不均匀的问题。The main problems existing in the prior art are: the setting of the gas circuit system is unreasonable, as shown in Figure 2, the
发明内容Contents of the invention
本发明的带有出口气体收集器的多晶硅还原炉,目的在于克服现有设备的上述缺点,提供一种能使炉内气体不易发生短路且分布均匀从而保证生产出的多晶硅棒上下粗细均匀的多晶硅还原炉。The purpose of the polysilicon reduction furnace with an outlet gas collector of the present invention is to overcome the above-mentioned shortcomings of the existing equipment, and to provide a polysilicon that can make the gas in the furnace less prone to short circuit and evenly distributed so as to ensure that the produced polysilicon rods are uniform in thickness up and down. reduction furnace.
本发明是通过以下技术方案实现的:The present invention is achieved through the following technical solutions:
本发明的一种多晶硅还原炉,包括炉体,夹套,底盘,支座,多对电极,带有石墨头的硅芯,混合气进气管及进气喷嘴,出气管和冷却系统等;其中炉内顶端设置有出口气体收集器,底盘中心设置有出气管,出气管与出口气体收集器连通。A polysilicon reduction furnace of the present invention comprises a furnace body, a jacket, a chassis, a support, a plurality of pairs of electrodes, a silicon core with a graphite head, a mixed gas inlet pipe and an inlet nozzle, an air outlet pipe and a cooling system, etc.; An outlet gas collector is arranged at the top of the furnace, and an outlet pipe is arranged at the center of the chassis, and the outlet pipe communicates with the outlet gas collector.
在出口气体收集器上设置有两根垂直连通的主接管;其中主接管I 19一端与设置在底盘中心的出气管连通,另一端与主接管II 20的中心位置垂直连通;主接管II上连接有若干根侧接管21,侧接管与主接管II垂直连通;侧接管和主接管II向下的一面即面向底盘的一面均匀设置有若干小孔22。The outlet gas collector is provided with two vertically connected main pipes; one end of the main pipe I 19 communicates with the outlet pipe arranged in the center of the chassis, and the other end communicates vertically with the center of the main pipe II 20; the main pipe II is connected There are several
所述主接管II 20和侧接管21均与炉体1内壁连接。The main connecting pipe II 20 and the
所述主接管II 20和侧接管21均通过搭接板24及螺栓25与炉体1内壁连接。The main connecting pipe II 20 and the
多对电极分圈正负交错均匀地布置在底盘上,与电极连接的带有石墨头的硅芯顶部两两搭接,电极可以设置为12对或15对或18对或24对或36对;混合气进气管上连接若干喷嘴,喷嘴均匀分布在底盘上。Multiple pairs of electrodes are evenly arranged on the chassis in positive and negative staggered circles, and the tops of the silicon cores with graphite heads connected to the electrodes are overlapped in pairs. The electrodes can be set to 12 pairs, 15 pairs, 18 pairs, 24 pairs, or 36 pairs. ; A number of nozzles are connected to the gas mixture intake pipe, and the nozzles are evenly distributed on the chassis.
具体说明如下:The specific instructions are as follows:
带有出口气体收集器的多晶硅还原炉,包括炉体,夹套,底盘,支座,观察视镜,多对电极,带有石墨头的硅芯,混合气进气管及进气喷嘴,出口气体收集器,出气管,夹套冷却水进水口和出水口,底盘冷却水进水口和出水口,电极冷却水进水口和出水口及其他附属部件。多对电极分圈正负交错均匀地布置在底盘上,与电极连接的带有石墨头的硅芯顶部两两搭接,电极可设置为12对或15对或18对或24对或36对;混合气进气管上连接若干喷嘴,喷嘴均匀分布在底盘上;炉内顶端设置有出口气体收集器,底盘中心设置有出气管,出气管与出口气体收集器连通。Polysilicon reduction furnace with outlet gas collector, including furnace body, jacket, chassis, support, observation mirror, multiple pairs of electrodes, silicon core with graphite head, mixed gas inlet pipe and inlet nozzle, outlet gas Collector, air outlet pipe, jacket cooling water inlet and outlet, chassis cooling water inlet and outlet, electrode cooling water inlet and outlet and other accessories. Multiple pairs of electrodes are evenly arranged on the chassis in positive and negative staggered circles, and the tops of the silicon cores with graphite heads connected to the electrodes are overlapped in pairs. The electrodes can be set to 12 pairs, 15 pairs, 18 pairs, 24 pairs, or 36 pairs. A number of nozzles are connected to the mixed gas inlet pipe, and the nozzles are evenly distributed on the chassis; an outlet gas collector is arranged at the top of the furnace, and an outlet pipe is arranged at the center of the chassis, and the outlet pipe communicates with the outlet gas collector.
出口气体收集器上设置有两根垂直连通的主接管;其中主接管I 19一端与设置在底盘中心的出气管11连通,另一端与主接管II 20的中心位置垂直连通;主接管II 20上连接有若干根侧接管21,侧接管21与主接管II 20垂直连通;侧接管21和主接管II 20向下的一面即面向底盘的一面均匀设置有若干小孔22。主接管I 19与主接管II 20、主接管II 20与侧接管21均通过法兰23连接,主接管II 20和侧接管21均通过搭接板24及螺栓25与炉体1内壁连接。The outlet gas collector is provided with two vertically connected main pipes; one end of the main pipe I 19 communicates with the
本发明的特征在于多晶硅还原炉内顶端设置有出口气体收集器,设置在底盘中心的出气管与出口气体收集器连通。The present invention is characterized in that an outlet gas collector is arranged at the top of the polysilicon reduction furnace, and an outlet pipe arranged at the center of the chassis communicates with the outlet gas collector.
本发明的效果和优点是,氢气和三氯氢硅混合气体由进气管及进气喷嘴进入还原炉内,由于炉内顶端设置有出口气体收集器,且出口气体收集器与设置在底盘中心的出气管连通,使得气体在高速向上喷射的过程中,不会发生短路直接从出气口排出,并且能够均匀的分布于整个炉内空间,与通电高温的硅棒充分接触并在其表面发生化学气相沉积反应,生成高纯多晶硅均匀沉积于硅棒上,得到上下粗细均匀的棒状多晶硅产品。同时生成的四氯化硅、二氯二氢硅、氯化氢等副产物尾气向上运动至出口气体收集器,经由收集器下表面均匀设置的若干小孔进入收集器内,然后沿着收集器的主接管I向下运动至出气管排出。The effect and advantage of the present invention are that the mixed gas of hydrogen and trichlorosilane enters the reduction furnace through the inlet pipe and the inlet nozzle, because the top of the furnace is provided with an outlet gas collector, and the outlet gas collector is connected with the outlet gas collector arranged at the center of the chassis. The gas outlet pipe is connected so that the gas can be discharged directly from the gas outlet without short circuit during the process of high-speed upward injection, and can be evenly distributed in the entire furnace space, fully contacting the electrified high-temperature silicon rod and generating a chemical gas phase on its surface The deposition reaction produces high-purity polysilicon that is uniformly deposited on the silicon rod, and a rod-shaped polysilicon product with uniform thickness from top to bottom is obtained. Simultaneously generated by-product tail gas such as silicon tetrachloride, dichlorodihydrosilane, and hydrogen chloride moves upward to the outlet gas collector, enters the collector through a number of small holes uniformly arranged on the lower surface of the collector, and then flows along the main body of the collector. Connect pipe I and move downwards until the outlet pipe is discharged.
附图说明Description of drawings
图1为本发明的带有出口气体收集器的多晶硅还原炉结构示意图;Fig. 1 is the structural representation of the polysilicon reduction furnace with outlet gas collector of the present invention;
图2为现有多晶硅还原炉结构示意图;Fig. 2 is the structural representation of existing polysilicon reduction furnace;
图3为本发明的出口气体收集器的结构示意图;Fig. 3 is the structural representation of outlet gas collector of the present invention;
图4为本发明的出口气体收集器的A-A结构示意图;Fig. 4 is the A-A structural representation of outlet gas collector of the present invention;
其中:1-炉体,2-夹套,3-底盘,4-支座,5-硅芯,6-电极,7-石墨头,8-进气管,9-进气喷嘴,10-出口气体收集器,10′-出气口,11-出气管,12-观察视镜,13-夹套冷却水进口,14-夹套冷却水出口,15-底盘冷却水进口,16-底盘冷却水出口,17-电极冷却水进口,18-电极冷却水出口,19-出口气体收集器主接管I,20-出口气体收集器主接管II,21-出口气体收集器侧接管,22-出口气体收集器小孔,23-法兰,24-搭接板,25-螺栓。Among them: 1-furnace body, 2-jacket, 3-chassis, 4-support, 5-silicon core, 6-electrode, 7-graphite head, 8-intake pipe, 9-intake nozzle, 10-outlet gas Collector, 10'-air outlet, 11-air outlet pipe, 12-observation mirror, 13-jacket cooling water inlet, 14-jacket cooling water outlet, 15-chassis cooling water inlet, 16-chassis cooling water outlet, 17-electrode cooling water inlet, 18-electrode cooling water outlet, 19-exit gas collector main connection I, 20-exit gas collector main connection II, 21-exit gas collector side connection, 22-exit gas collector small Hole, 23-flange, 24-lap plate, 25-bolt.
具体实施方式Detailed ways
下面根据附图对本发明作进一步的详细说明:The present invention will be described in further detail below according to accompanying drawing:
如图1所示,带有出口气体收集器的多晶硅还原炉包括炉体1,夹套2,底盘3,支座4,观察视镜12,多对电极6,带有石墨头7的硅芯5,混合气进气管8及进气喷嘴9,出口气体收集器10,出气管11,夹套冷却水进水口13,夹套冷去水出水口14,底盘冷却水进水口15,底盘冷却水出水口16,电极冷却水进水口17,电极冷却水出水口18等。多对电极6分圈正负交错均匀地布置在底盘上,与电极6连接的带有石墨头7的硅芯5顶部两两搭接,电极6可以设置为12对或15对或18对或24对或36对;混合气进气管8上连接若干喷嘴9,喷嘴9均匀分布在底盘上;炉内顶端设置有出口气体收集器10,底盘中心设置有出气管11,出气管11与出口气体收集器10连通。As shown in Figure 1, a polysilicon reduction furnace with an outlet gas collector includes a
如图3、图4所示,出口气体收集器10上设置有两根垂直连通的主接管,其中主接管I19一端与出气管11连通,另一端与主接管II 20的中心位置垂直连通;主接管II 20上设置有若干根侧接管21,侧接管21与主接管II 20垂直连通;侧接管21和主接管II 20向下的一面即面向底盘的一面均匀设置有若干小孔22。主接管I 19与主接管II 20、主接管II 20与侧接管21均通过法兰23连接,主接管II 20和侧接管21均通过搭接板24及螺栓25与炉体1内壁连接。As shown in Fig. 3 and Fig. 4, the
氢气和三氯氢硅混合气经由进气管8及其上设置的若干喷嘴9高速喷射进入还原炉1内,带有石墨头7的硅芯电极6通电产生高温,同时在夹套冷却水进水口13和出水口14之间、底盘冷却水进水口15和出水口16之间、电极冷却水进水口17和出水口18之间通以冷却水。气体高速向上喷射运动,炉内顶端出口气体收集器10保证了混合气体不易发生短路且均匀地分布于整个炉内空间,与通电高温硅芯5充分接触,在硅芯5表面发生化学气相沉积反应,生成高纯多晶硅并沉积于硅芯上,得到上下粗细均匀的棒状多晶硅产品。反应中生成的四氯化硅、二氯二氢硅、氯化氢等副产物尾气向上运动至炉内顶端的出口气体收集器10,从收集器下表面均匀设置的若干小孔22进入收集器内,然后沿着收集器的主接管I 19向下运动至底盘中心的出气管11排出。炉体侧壁上从上至下设置3个观察视镜12,以方便观察多晶硅棒各个部位的生长情况。The mixed gas of hydrogen and trichlorosilane is sprayed into the
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102320607A (en) * | 2011-09-15 | 2012-01-18 | 中国恩菲工程技术有限公司 | Polycrystalline silicon reducing furnace |
CN103158200A (en) * | 2011-12-09 | 2013-06-19 | 洛阳金诺机械工程有限公司 | C-shaped silicon core lap joint method |
CN103158202A (en) * | 2011-12-09 | 2013-06-19 | 洛阳金诺机械工程有限公司 | Lap joint method of hollow silicon core |
CN103708464A (en) * | 2013-12-18 | 2014-04-09 | 天津大学 | Arrangement mode and connection method of decomposition furnace with 3 pairs of rods for producing polysilicon through silane method |
CN103880009A (en) * | 2014-03-18 | 2014-06-25 | 天津大学 | Polycrystalline silicon reduction furnace with exhaust outlet connected with inner stretching tube and connecting method |
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Cited By (8)
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CN102320607A (en) * | 2011-09-15 | 2012-01-18 | 中国恩菲工程技术有限公司 | Polycrystalline silicon reducing furnace |
CN103158200A (en) * | 2011-12-09 | 2013-06-19 | 洛阳金诺机械工程有限公司 | C-shaped silicon core lap joint method |
CN103158202A (en) * | 2011-12-09 | 2013-06-19 | 洛阳金诺机械工程有限公司 | Lap joint method of hollow silicon core |
CN103158200B (en) * | 2011-12-09 | 2016-07-06 | 洛阳金诺机械工程有限公司 | A kind of bridging method of C-shaped silicon core |
CN103158202B (en) * | 2011-12-09 | 2016-07-06 | 洛阳金诺机械工程有限公司 | A kind of bridging method of hollow silicon core |
CN103708464A (en) * | 2013-12-18 | 2014-04-09 | 天津大学 | Arrangement mode and connection method of decomposition furnace with 3 pairs of rods for producing polysilicon through silane method |
CN103880009A (en) * | 2014-03-18 | 2014-06-25 | 天津大学 | Polycrystalline silicon reduction furnace with exhaust outlet connected with inner stretching tube and connecting method |
CN103880009B (en) * | 2014-03-18 | 2016-01-13 | 天津大学 | A polysilicon reduction furnace in which the tail gas outlet is connected to an inner extension pipe and its connection method |
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