CN102674359B - Device and method for cooing tail gas recovery liquid of polysilicon reduction furnace with inner tank - Google Patents

Device and method for cooing tail gas recovery liquid of polysilicon reduction furnace with inner tank Download PDF

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Publication number
CN102674359B
CN102674359B CN2012101418824A CN201210141882A CN102674359B CN 102674359 B CN102674359 B CN 102674359B CN 2012101418824 A CN2012101418824 A CN 2012101418824A CN 201210141882 A CN201210141882 A CN 201210141882A CN 102674359 B CN102674359 B CN 102674359B
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tail gas
inner bag
reduction furnace
chassis
storage tank
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CN102674359A (en
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刘春江
段长春
黄哲庆
周阳
段连
袁希钢
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Tianjin University
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Tianjin University
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/25Process efficiency
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
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Abstract

The invention discloses a device and a method for cooing tail gas recovery liquid of a polysilicon reduction furnace with an inner tank. A chassis exhaust manifold is connected with the lower side of the polysilicon reduction furnace with the inner tank and is connected with a condenser; the condenser is connected with a storage tank; the storage tank is provided with a storage tank exhaust pipe;the storage tank is connected to a tail gas recovery liquid inlet pipeline through a pump; and the tail gas recovery liquid inlet pipeline is provided with a venture injection device and a trichlorosilane liquid injection pipeline. Compared with the conventional polysilicon reduction furnace, the invention has the advantages that: an inner tank double-layer structure and a corresponding chassis structure can greatly reduce the energy radiation of a silicon rod to the inner wall of a bell jar, and silica powder cannot be deposited on the inner wall of the bell jar because of lower temperature,so that a polishing effect on the inner wall of the bell jar is kept, and the input amount of cooling water input into the bell jar of the polysilicon reduction furnace can be reduced. According to the tail gas recovery liquid cooling inner tank process of the energy-saving polysilicon reduction furnace, the using amount of trichlorosilane cooling liquid in the reduction furnace is reduced, the tail gas treatment amount is reduced, and the energy consumption is finally reduced.

Description

Tail gas recycle liquid cooling radiator cooler and method with the polycrystalline silicon reducing furnace of inner bag
Technical field
The invention belongs to technical field of polysilicon production, relate to a kind of energy-saving polycrystalline silicon reduction furnace, particularly a kind of tail gas recycle liquid cooling radiator cooler and method of the polycrystalline silicon reducing furnace with inner bag.
Background introduction
At present, improved Siemens is mainly adopted in the production of polysilicon.In improved Siemens, the principal reaction that reduction workshop section occurs is that trichlorosilane is generated silicon and hydrogenchloride by hydrogen reducing, and this reaction is carried out in polycrystalline silicon reducing furnace.When reacting, polycrystalline silicon reducing furnace is in the energising condition of high temperature, temperature of reaction remains on about 1050~1150 ℃, body of heater chuck, chassis and the electrode etc. of reduction furnace locate all to be furnished with recirculating cooling water system simultaneously, come to carry out heat exchange to satisfy body of heater temperature requirement everywhere with the furnace high-temperature environment.
Traditional polycrystalline silicon reducing furnace energy consumption is very large, can reach 60~100KWh/kg polysilicon, and the reduction power consumption of production of polysilicon accounts for about 70% of total cost.The loss of reduction furnace self-energy is serious, and major cause is the hyperthermia radiation loss of polycrystalline silicon rod.Polycrystalline silicon rod transfers energy on the reduction furnace inwall by hyperthermia radiation, then by the chuck water coolant heat is taken away.The tradition polycrystalline silicon reducing furnace, such as patent CN200420060144.8, CN200720306394.9, CN200820105591.9, CN200920230836.5, CN201020215600.7 etc., its inlet mouth and air outlet all are distributed on the chassis, the shortcoming of this design is that the coupling in temperature field is unreasonable, easily is detained at the reduction furnace top owing to the flow field, produce flow dead, cause the gas temperature of regional area too high, produce silica flour, and these silica flours can cause the loss of raw material on the one hand, the silica flour that produces on the other hand easily is attached on the bell jar inwall, so that the smooth finish of bell jar inwall reduces, cause the energy of taking away because of radiation to rise violently, finally show as the reduction power consumption and raise; Flow owing to inlet fluid makes progress in addition, and the fluid of outlet flows downward, the fluid of these two bursts of countercurrent flows affects the transformation efficiency of reaction gas so that the fluid in the reduction furnace is the mixed flow state, has further increased the power consumption of reduction furnace.The present invention proposes a kind of tail gas recycle liquid cooling radiator cooler and method of correspondence on the basis with the polycrystalline silicon reducing furnace of inner bag.
Summary of the invention
The invention solves that traditional polycrystalline silicon reducing furnace interior temperature distribution is inhomogeneous, bell jar inwall deposition silica flour and the large problem of energy consumption, a kind of tail gas recycle liquid cooling radiator cooler and method of the polycrystalline silicon reducing furnace with inner bag are provided.
The inner-tube structure of Novel polysilicon reduction furnace is as follows:
The polycrystalline silicon reducing furnace inner bag comprises the inner and outer wall double-layer structure, and a fixed gap arranged between inwall and the outer wall, pass into high-purity trichlorosilane liquid between the inwall of polycrystalline silicon reducing furnace inner bag and the outer wall, space between the inner bag inner and outer wall and inner bag top base plate are connected with zone between the top board, it is that gas enters the inner bag top that liquid trichlorosilane absorbs heat of vaporization, and enters the conversion zone of reduction furnace by the muffler at inner bag top.
The chassis structure of Novel polysilicon reduction furnace is as follows:
Fix a gas box above polycrystalline silicon reduction furnace base plate, the top of the gas box that polycrystalline silicon reduction furnace base plate top is fixing has uniform hole, passes into liquid trichlorosilane in the fixing gas box in polycrystalline silicon reduction furnace base plate top; The silicon rod of polycrystalline silicon reducing furnace and chassis air inlet nozzle all pass the top of gas box, at chassis of reducing furnace liquid discharge pipe are housed simultaneously.
Under the prerequisite of above-mentioned polycrystalline silicon reducing furnace inner bag and chassis structure, tail gas recycle liquid cooling radiator cooler structure is as follows:
Be connected with chassis exhaust-gas receiver (19) below the polycrystalline silicon reducing furnace of inner bag, chassis exhaust-gas receiver (19) connects condenser (26), and condenser connects storage tank (27), is provided with storage tank vapor pipe (28) on the storage tank (27); Storage tank (27) is connected to tail gas recycle liquid inlet line (24) through pump (29); Be provided with Venturi induction apparatus (30) and trichlorosilane liquid ejecting pipeline (31) in tail gas recycle liquid inlet line (24).
The working method of tail gas recycle liquid cooling radiator cooler of the present invention is as follows:
The inner tail gas that produces of polycrystalline silicon reducing furnace inner bag (2) is discharged through chassis vapor pipe (6), the tail gas that produces between inner bag (2) and the bell jar (1) is discharged through the vapor pipe (25) between inner bag and the bell jar, after entering chassis exhaust-gas receiver (19) discharge reduction furnace after two strands of tail gas converge, through entering storage tank (27) after condenser (26) condensation, uncooled gas is discharged from storage tank vapor pipe (28) and is entered subsequent disposal workshop section, and the liquid after the condensation cooling is squeezed into reduction furnace tail gas recycle liquid inlet line (24) as the cooling fluid of reduction furnace inner bag through pump (29); Venturi induction apparatus (30) before entering reduction furnace, is installed tail gas recycle liquid simultaneously, with the part trichlorosilane liquid in the stove through trichlorosilane liquid ejecting pipeline (31) injection to tail gas recycle liquid inlet line (24), after mixing, the two enters the space between reduction furnace inner bag (2) and the bell jar (1), inner bag (2) is cooled off, cooling fluid becomes gas under hot environment, enter chassis exhaust-gas receiver (19) through the vapor pipe (25) between inner bag and the bell jar, inner bag internal high temperature hyperbaric environment issues biochemical reaction and generates polysilicon, tail gas also enters chassis exhaust-gas receiver (19) through chassis vapor pipe (6) simultaneously, and whole process stove inner exhaust gas circulates.
The advantage that the present invention has is:
Compare with traditional polycrystalline silicon reducing furnace, inner bag bilayer structure and corresponding chassis structure can reduce silicon rod greatly to the energy emission of bell jar inwall, the bell jar inwall can not deposit silica flour because temperature is low, the polishing effect that has kept the bell jar inwall can also reduce the intake of polycrystalline silicon reducing furnace bell jar water coolant.
The tail gas recycle liquid cooling of energy-saving polycrystalline silicon reduction furnace but inner bag technique has reduced trichlorosilane coolant in the reduction furnace, has reduced the vent gas treatment amount, has finally reduced energy consumption.
Description of drawings
Fig. 1 is the internal structure schematic diagram of a kind of energy-saving polycrystalline silicon reduction furnace of the present invention;
Fig. 2 is the but inner container process flow figure of tail gas recycle liquid cooling of a kind of energy-saving polycrystalline silicon reduction furnace of the present invention.
Wherein, 1-reduction furnace bell jar, 2-inner bag, 3-silicon core, 4-chassis, 5-chassis air inlet pipe, 6-chassis escape pipe, 7-electrode, 8-graphite chuck, 9-body of heater entrance of cooling water, 10-body of heater cooling water outlet, 11-chassis total inlet pipe, 12-chassis liquid discharge pipe, the liquid trichlorosilane inlet pipe in 13-chassis, the liquid trichlorosilane inlet pipe in 14-inner bag top, the liquid trichlorosilane inlet pipe of 15-side wall of inner, 16-chassis cold gas box, 17-inner bag top escape pipe, 18-inner bag top muffler, 19-chassis exhaust-gas receiver, the inwall of 20-inner bag, the outer wall of 21-inner bag, 22-inner bag top base plate, 23-inner bag top top board, 24-tail gas recycle liquid inlet line, vapor pipe between 25-inner bag and the bell jar, 26-condenser, 27-storage tank, 28-storage tank vapor pipe, the 29-pump, 30-Venturi induction apparatus, 31-trichlorosilane liquid ejecting pipeline.
Embodiment
Be described in further detail below in conjunction with the tail gas recycle cooling liner technique of the drawings and specific embodiments to a kind of energy-saving polycrystalline silicon reduction furnace provided by the invention.
As shown in Figure 1, reduction furnace bell jar (1) is fixed to chassis of reducing furnace (4) upward and sealing, silicon core (3) is connected with chassis electrode (7) by graphite chuck (8) and seals, and chassis electrode (7) is fixed to chassis of reducing furnace (4) and sealing, and is connected with power supply system; Chassis air inlet control device (11) is connected with chassis air inlet pipe (5), and chassis exhaust control device (19) is connected with chassis vapor pipe (6).Liquid trichlorosilane enters polycrystalline silicon reduction furnace base plate cold gas box (16) by the liquid trichlorosilane inlet pipe in chassis (13), liquid trichlorosilane enters the polycrystalline silicon reducing furnace top by the liquid trichlorosilane inlet pipe in inner bag top (14), liquid trichlorosilane enters the polycrystalline silicon reducing furnace side wall of inner by the liquid trichlorosilane inlet pipe of side wall of inner (15), chassis of reducing furnace (4), reduction furnace bell jar (1) passes into water coolant by chassis entrance of cooling water and body of heater cooling water inlet respectively, and the chassis cooling water outlet is connected with the hot system of need respectively with the body of heater cooling water outlet.
As shown in Figure 2, be connected with chassis exhaust-gas receiver (19) below the polycrystalline silicon reducing furnace of inner bag, chassis exhaust-gas receiver (19) connects condenser (26), and condenser connects storage tank (27), is provided with storage tank vapor pipe (28) on the storage tank (27); Storage tank (27) is connected to tail gas recycle liquid inlet line (24) through pump (29); Be provided with Venturi induction apparatus (30) and trichlorosilane liquid ejecting pipeline (31) in tail gas recycle liquid inlet line (24).
Specific embodiment:
As shown in Figure 1, with the operating process of the polycrystalline silicon reducing furnace of inner bag:
(1) at first opens chassis air inlet house steward (11) and chassis exhaust-gas receiver (19);
(2) next body of heater, chassis of reducing furnace at reduction furnace pass into water coolant simultaneously, liquid trichlorosilane is passed into polycrystalline silicon reduction furnace base plate cold gas box (16) by the liquid trichlorosilane inlet pipe in chassis (13), the external diameter of chassis cold gas box (16) is than the little 10mm of polysilicon reduction furnace inner bag diameter, the height of drum is 5cm, and the wall thickness of drum is 0.5cm;
(3) again with the SiHCl that purifies 3With H 2Mix by a certain percentage, then gas mixture is passed into polycrystalline silicon reducing furnace from chassis air inlet pipe (5);
(4) power supply system that starts reduction furnace is to the heating of silicon core, and the temperature that keeps the silicon core is at 1150 ℃, and the reduction furnace internal pressure is 0.8Mpa.When the temperature of silicon wicking surface reaches SiHCl 3With H 2During the condition of reaction, gas mixture begins to occur reduction reaction, and reacted silicon will deposit on the silicon core, finds that by the temp probe thermometric temperature on chassis is lower than 300 ℃ all the time;
(5) reacted tail gas is discharged through chassis escape pipe (6), and the temperature of tail gas is controlled at 450 ℃ ± 20, until the growth in thickness of silicon core when above to 200mm, stops power supply, and after the by the time silicon core cooling, taking-up silicon core;
As shown in Figure 2, reclaim the working method of liquid cooling radiator cooler with the polysilicon reducing furnace tail gas of inner bag as follows:
The inner tail gas that produces of polycrystalline silicon reducing furnace inner bag (2) is discharged through chassis vapor pipe (6), the tail gas that produces between inner bag (2) and the bell jar (1) is discharged through the vapor pipe (25) between inner bag and the bell jar, after entering chassis exhaust-gas receiver (19) discharge reduction furnace after two strands of tail gas converge, through entering storage tank (27) after condenser (26) condensation, uncooled gas is discharged from storage tank vapor pipe (28) and is entered subsequent disposal workshop section, and the liquid after the condensation cooling is squeezed into reduction furnace cooling liquid inlet pipeline (24) as the cooling fluid of reduction furnace inner bag through pump (29); Venturi induction apparatus (30) before entering reduction furnace, is installed tail gas recycle liquid simultaneously, with the part trichlorosilane liquid in the stove through trichlorosilane liquid ejecting pipeline (31) injection to tail gas recycle liquid inlet line (24), after mixing, the two enters the space between reduction furnace inner bag (2) and the bell jar (1), inner bag (2) is cooled off, cooling fluid becomes gas under hot environment, enter chassis exhaust-gas receiver (19) through the escape pipe (25) between inner bag and the bell jar, inner bag internal high temperature hyperbaric environment issues biochemical reaction and generates polysilicon, tail gas enters chassis exhaust-gas receiver (19) through chassis vapor pipe (6), and whole process stove inner exhaust gas circulates.
The tradition polycrystalline silicon reducing furnace with water or deep fat as refrigerant, cooling bell jar, chassis and electrode etc., silicon rod to Wall Radiation a large amount of energy, water or cooling oil are taken away and these energy finally are cooled, this is the major cause that causes the polycrystalline silicon reducing furnace energy consumption huge; Polycrystalline silicon reducing furnace with inner bag, because the heat insulating effect of inner bag has greatly reduced the thermal radiation of silicon rod to wall, comes cooling liner with liquid trichlorosilane simultaneously, can greatly reduce like this energy consumption of reduction furnace, the Energy Intensity Reduction 20% of the more traditional polycrystalline silicon reducing furnace of energy consumption; Tail gas recycle liquid cooling radiator cooler and the method for the polycrystalline silicon reducing furnace with inner bag of the present invention, that the trichlorosilane that cooling liner is used is recycled, reduced the usage quantity of trichlorosilane, this device and technique are so that the energy consumption of reduction furnace continues reduction, than the band inner bag polycrystalline silicon reducing furnace Energy Intensity Reduction 5% that does not use the circulation trichlorosilane.
The above example only is to prove absolutely the present invention and the preferred embodiment of lifting, and protection scope of the present invention is not limited to this.Being equal to that those skilled in the art do on basis of the present invention substitutes or conversion, all within protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.

Claims (2)

1. tail gas recycle liquid cooling radiator cooler with the polycrystalline silicon reducing furnace of inner bag, its feature is being connected with chassis exhaust-gas receiver (19) below the polycrystalline silicon reducing furnace of inner bag, chassis exhaust-gas receiver (19) connects condenser (26), condenser connects storage tank (27), is provided with storage tank vapor pipe (28) on the storage tank (27); Storage tank (27) is connected to tail gas recycle liquid inlet line (24) through pump (29); Be provided with Venturi induction apparatus (30) and trichlorosilane liquid ejecting pipeline (31) in tail gas recycle liquid inlet line (24).
2. the method with the tail gas recycle liquid cooling radiator cooler of the polycrystalline silicon reducing furnace of inner bag of claim 1, it is characterized in that: the inner tail gas that produces of polycrystalline silicon reducing furnace inner bag (2) is discharged through chassis vapor pipe (6), the tail gas that produces between inner bag (2) and the bell jar (1) is discharged through the vapor pipe (25) between inner bag and the bell jar, after entering chassis exhaust-gas receiver (19) discharge reduction furnace after two strands of tail gas converge, through entering storage tank (27) after condenser (26) condensation, uncooled gas is discharged from storage tank vapor pipe (28) and is entered subsequent disposal workshop section, and the liquid after the condensation cooling is squeezed into reduction furnace tail gas recycle liquid inlet line (24) as the cooling fluid of reduction furnace inner bag through pump (29); Venturi induction apparatus (30) before entering reduction furnace, is installed tail gas recycle liquid simultaneously, with the part trichlorosilane liquid in the stove through trichlorosilane liquid ejecting pipeline (31) injection to tail gas recycle liquid inlet line (24), after mixing, the two enters the space between reduction furnace inner bag (2) and the bell jar (1), inner bag (2) is cooled off, cooling fluid becomes gas under hot environment, enter chassis exhaust-gas receiver (19) through the vapor pipe (25) between inner bag and the bell jar, inner bag internal high temperature hyperbaric environment issues biochemical reaction and generates polysilicon, tail gas also enters chassis exhaust-gas receiver (19) through chassis vapor pipe (6) simultaneously, and whole process stove inner exhaust gas circulates.
CN2012101418824A 2012-05-09 2012-05-09 Device and method for cooing tail gas recovery liquid of polysilicon reduction furnace with inner tank Expired - Fee Related CN102674359B (en)

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CN104947087B (en) * 2014-03-31 2018-03-06 甘志银 Extraordinary pressure chemical vapor deposition device
CN109724402B (en) * 2019-01-25 2024-02-13 东莞市瑾耀精密设备有限公司 High-temperature sintering furnace
CN110436467B (en) * 2019-08-16 2024-03-19 洛阳中硅高科技有限公司 Feeding system of polysilicon reduction furnace
CN113072074A (en) * 2021-04-25 2021-07-06 森松(江苏)重工有限公司 Furnace barrel cooling method and device of reduction furnace and polycrystalline silicon reduction production method

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CN102001660A (en) * 2010-11-24 2011-04-06 天津大学 Polysilicon reducing furnace with multiple gas outlets on chassis
CN102205967A (en) * 2011-04-29 2011-10-05 宁夏阳光硅业有限公司 Energy-saving polysilicon reduction furnace and manufacturing method for polysilicon
JP5360147B2 (en) * 2011-07-11 2013-12-04 三菱マテリアル株式会社 Polycrystalline silicon reduction furnace

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