A kind of reactor drum that is used to produce the tubulose polysilicon
Technical field
The utility model relates to a kind of reactor drum of producing polysilicon, more specifically to a kind of shell and tube reactor of producing the tubulose polysilicon.
Background technology
At present, most method for preparing polysilicon is the improvement siemens process, mainly use belljar with 8mm that electrode links to each other about the silicon core as deposition substrate, employing high temperature reduction technology is with high-purity SiHCl
3At H
2Reduce deposition in the atmosphere and generate polysilicon.
Above-mentioned chemical vapor deposition processes is in the reduction furnace of bell jar type, to carry out, and this reaction vessel seals, and discharge port and opening for feed and some counter electrode are installed on the chassis; The silicon core that is connecting diameter 5-10mm, length 1500-3000mm on the electrode; Two silicon rods on every counter electrode interconnect through short silicon rod at the other end again, and when applying the high pressure about 6 ~ 12kV on the counter electrode, the breakdown conduction of silicon rod also is heated to 1000-1150 ℃ and reacts; Through hydrogen reduction; Silicon increases the diameter of silicon rod at the surface deposition of silicon rod gradually, finally reaches about 120-200mm.Generally, producing diameter is the high purity silicon rods of 120-200mm, and the required reaction times is approximately 150-300 hour.
Use this mode of production, reactant gases reacts at the reduction furnace inner space, and in the silicon rod outside deposition; Comfort zone is merely the silicon rod surface, and the most spaces in the reduction furnace are idle space, and a large amount of side reactions take place in idle space; Cause feed stock conversion extremely low, and the silicon rod speed of growth is slow, productive rate is lower; Simultaneously, in order to prevent a large amount of siliceous depositss, must cool off to keep the reduction furnace internal surface temperature the reduction furnace wall and be not higher than 350 ° of C in the reduction furnace inner wall surface; Therefore, the form that a large amount of heat energy conducts with convection current conduction and radiation is reduced furnace wall chuck heat-eliminating medium and takes away, and the heat energy that the silicon rod energising is transformed in the reduction furnace is over half through reduction furnace wall coolant medium consumption; Therefore thermo-efficiency is lower, and capacity usage ratio is not enough, and production energy consumption is higher.
Change traditional deposition carrier into the hollow shell pipe by solid slim rods, and, can improve the reaction compartment utilization ratio greatly depositing in the unstripped gas access tube; Improve transformation efficiency of raw material and sedimentation velocity, and raw material reacts in the space in pipe; Space reactor can adopt insulated design; Reduce energy to greatest extent and scatter and disappear, cut down the consumption of energy greatly, the reduction production cost.On this basis, the present invention proposes and adopt the shell and tube design, make silicon-containing material gas, produce the tubulose polysilicon at open tube internal reaction and deposit spathic silicon.
Summary of the invention
The utility model technical problem to be solved provides a kind of reactor drum that is used to produce the tubulose polysilicon, and this reactor drum has changed the structure of traditional reactor, adopts the shell and tube design, changes traditional outside deposition mode into the internal surface depositional mode.
For solving the problems of the technologies described above, the technical scheme that the utility model adopts is following:
A kind of reactor drum of producing the tubulose polysilicon that is applicable to, it comprises shell, liner, end socket, tube sheet, virgin gas import and export, deposited tube, graphite external member, electrode and center heating member; Liner is arranged on outer casing inner wall, and tube sheet is connected to shell and liner two ends, and the tube sheet opposite side connects end socket respectively; The end socket top is provided with virgin gas and imports and exports, and end socket, tube sheet and shell adopt outer bolt to fix, and tube sheet is provided with the gas duct; Tube sheet inside is provided with electrode, and set inside is an annular to electrode in the gas duct, and combines with gas duct inner tight; The tubular graphene external member is passed ring electrode inside and is closely linked to each other with electrode inner wall; Each deposited tube two ends is fixed on respectively in the graphite external member of two ends tube sheet correspondence position, and the tube sheet central position is provided with the heating member electrode, and the center heating member is connected on the heating member electrode.
Wherein, Said shell and said end socket are metal material, and have cooling jacket design, optional water of heat-eliminating medium or thermal oil; Be preferably thermal oil; Metal material is preferably carbon steel or stainless steel, and the mode that said shell preferably adopts side to open is carried out folding, is provided preferably with view port on the said shell.
Wherein, Said liner is prepared by heat insulation material, and preferably by the preparation of the one or more combination in aerosil, zirconium white, the pure aluminium silicate lagging material, said liner is arranged on said enclosure and is fixed on the said outer casing inner wall; The inner wall surface of said liner is provided preferably with the electrically heated coil; The electrically heated coil links to each other with the electrode that passes liner and shell, and one or more in said liner internal space filling helium, neon, argon gas, krypton gas, the xenon are preferably argon gas; Pressure is 0.5bar ~ 6bar, is preferably 1 ~ 2bar.
Wherein, said tube sheet is a multi-layer compound structure, and material is made up of in silicon nitride, silit, quartz, graphite and the SP 1 one or more; Said tube sheet inside is provided with said electrode; Be furnished with the gas duct that gas is passed on the said tube sheet, said electrode stretches out said tube sheet in inside, gas duct, is respectively loop design; Internal surface preferably is processed with screw thread, and said tube sheet central position is provided with the heating member electrode.
Wherein, said virgin gas is imported and exported and is separately positioned on said end socket two ends.
Wherein, said graphite external member can be divided into three parts, comprises bolt, nut and fastener; The bolt outside surface preferably is processed with screw thread, is passed by the ring electrode inside in the gas duct on the said tube sheet, closely links to each other with ring electrode; Fastener has annular recesses; Fastener bottom links to each other with bolt one end, and by fixed by nut on bolt, bolt nut and fastener are the hollow ring structure; Said graphite external member inwall preferably has no diffusion coating, and the coating material is preferably silicon nitride or silit.
Wherein, heating member two ends, said center are connected on the heating member electrode at said tube sheet center, and the material of center heating member is preferably one or more in graphite, tantalum, molybdenum, the tungsten.
Wherein, said deposited tube is the hollow shell shape, and two ends are nested in respectively in the said graphite external member, and length of tube is 0.5 ~ 3m, is preferably 1 ~ 2m, and thickness of pipe is 0.1 ~ 10mm, is preferably 0.5 ~ 3mm, and bore is 50 ~ 250mm, is preferably 100 ~ 180mm.Material can be selected silicon for use, also can select other metallic conductor for use, and the metallic conductor material is preferably tantalum, molybdenum or tungsten.
Beneficial effect: adopt the described device of the utility model to make polysilicon, compared with prior art, have the following advantages: the heat energy utilization rate is high; Unit consumption of energy is low, and sedimentation rate is high, and is with short production cycle; Production capacity is big, and quality product is high, the substandard products that produced in the no traditional technology; Transformation efficiency height of raw material, by-product is few.
Description of drawings
Fig. 1 is the production of polysilicon device synoptic diagram that the utility model relates to.Wherein, 1, shell; 2, liner; 3, end socket; 4, tube sheet; 5, virgin gas is imported and exported; 6, deposited tube; 7, graphite external member; 8, electrode; 9, center heating member.
Fig. 2 is a reactor tube plate structure synoptic diagram.Wherein, 401, center heating member; 402, gas duct; 403, fixing threaded hole.
Fig. 3 is a graphite external member structural representation.Wherein, 701, bolt; 702, nut; 703, fastener.
Fig. 4 is that the reactor shell side direction is opened synoptic diagram.
Embodiment
Below through concrete embodiment and combine accompanying drawing that the apparatus system in the utility model is elaborated, but these embodiment only are illustrative purposes, are not intended to the scope of the utility model is carried out any qualification.
Embodiment 1:
The production of polysilicon device synoptic diagram that Fig. 1 relates to for the utility model.Wherein, mainly comprise 1 shell, 2 liners, 3 end sockets, 4 tube sheets, the import and export of 5 virgin gass, 6 deposited tubes, 7 graphite external members, 8 electrodes, 9 center heating members.As shown in Figure 1, virgin gas is imported and exported 5 and is separately positioned on end socket 3 two ends, and two ends end socket 3 is connected with shell 1 two ends with tube sheet 4 and utilizes the bolt (not shown) to be tightly connected; Liner 2 is fixed on shell 1 inside; Two ends closely contact with tube sheet 4, and liner 2 inwalls can be provided with electrically heated coil (not shown), and the electrically heated coil is connected with the outer electrode (not shown); Can carry out boosting to inside; Electrode 8 is arranged on tube sheet 4 inside, and links to each other with externally fed system (not shown), and graphite external member 7 is nested on the tube sheet 4 and closely is connected with electrode 8 respectively; Deposited tube 6 two ends are separately fixed in the graphite external member 7, and the two ends of center heating member 9 are separately fixed at tube sheet 4 central positions.
Shell of reactor shown in Fig. 1 can be preferably cylindrical for common square, regular polygon etc.Said shell has the cooling jacket structure, and refrigerant can be enumerated common water or thermal oil.
A kind of design form of the reactor drum tube sheet that Fig. 2 relates to for the utility model.Wherein, mainly comprise 401 heating member electrodes, 402 gas ducts, 403 fixing threaded holes.Heating member electrode 401 is arranged on tube sheet 4 geometric centre positions, and gas duct 402 takes uniform array to arrange at tube sheet 4 center surfaces, and electrode 8 stretches out tube sheet 4 and is annular design in 402 inside, gas duct.
A kind of design form of the graphite external member that adopts in the reactor drum that Fig. 3 relates to for the utility model.Wherein, mainly comprise 701 bolts, 702 nuts, 703 fasteners.Bolt 701 passes tube sheet 4 and closely is connected with electrode 8, and nut 702 is fixed on bolt 701 tops with fastener 703, and reaction can the tubulose polysilicon be struck down together with fastener 703, and bolt 701 and nut 702 can reuse after finishing.
Fig. 4 opens synoptic diagram for the shell of reactor sidepiece that the utility model relates to, and when reaction finished, shell side was to opening and dismounting.
In the depositing operation of the utility model, can adopt silicomethane as raw material; Also can adopt the halo silicomethane as raw material and additional hydrogen, the volume ratio of halo silicomethane and hydrogen is 3:1 ~ 9:1.
Further specify the technique effect of the utility model below through several more concrete embodiment, but the utility model is not had any restriction.
Embodiment 2
1) adopt pure silicomethane as unstripped gas.
2) the deposited tube material adopts molybdenum, and the pipe number is 36, pipe range 2m, and thickness of pipe 0.3mm, internal diameter are 130mm.
3) feedstock gas pressures is 2bar, alternately changes airintake direction one time in per 2 hours, and flow is 22.2m
3/ h.
Directly deposited tube on load voltage heating power is warming up to about 800 ° of C when 4) producing beginning, continuous production stopped in 60 hours, took out deposited tube, obtained the about 2000kg of polysilicon behind the employing nitration mixture dissolution of metals molybdenum, and total power consumption is about 4 * 10
4KWh, unit power consumption is about 20kWh/kg, and the element silicon once through yield is about 80%.
Embodiment 3:
1) adopt pure Trichloromonosilane and hydrogen as unstripped gas.
2) the deposited tube material adopts pure silicon, and the pipe number is 36, pipe range 2m, and thickness of pipe 1mm, internal diameter are 150mm.
3) feedstock gas pressures is 3bar, alternately changes airintake direction one time in per 5 hours, and the Trichloromonosilane flow is 80m
3/ h, hydrogen flowing quantity is about 250m
3/ h.
4) produce when beginning to the energising of center heating member or simultaneously to liner inwall heater coil heating boosting silicone tube; On load voltage made the silicone tube heating power be warming up to about 1100 ° of C at the electrode two ends when silicone tube was warming up to about 600 ° of C; Can cut off center heating member and heater coil power supply this moment; Continuous production stopped in 100 hours, approximately produced polysilicon 2000kg, and total power consumption is about 10
5KWh, unit power consumption is about 50kWh/kg, and the element silicon once through yield is about 20%.
The shell and tube reactor that the utility model relates to not only can improve polysilicon deposition speed and unstripped gas once through yield and reduce unit power consumption and can not produce in the traditional technology because the not good low-quality product that causes of silicon rod surface topography.
Although preceding text have given to describe in detail and explanation to the embodiment of the utility model; But should indicatedly be; We can carry out various equivalences to above-mentioned embodiment according to the conception of the utility model and change and modification; When the function that it produced does not exceed spiritual that specification sheets and accompanying drawing contain yet, all should be within the protection domain of the utility model.