CN103998648A - Deposition cartridge for production materials via the chemical vapor deposition process - Google Patents
Deposition cartridge for production materials via the chemical vapor deposition process Download PDFInfo
- Publication number
- CN103998648A CN103998648A CN201280042405.0A CN201280042405A CN103998648A CN 103998648 A CN103998648 A CN 103998648A CN 201280042405 A CN201280042405 A CN 201280042405A CN 103998648 A CN103998648 A CN 103998648A
- Authority
- CN
- China
- Prior art keywords
- deposition
- container
- deposition surface
- reactor
- melting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/02—Silicon
- C01B33/021—Preparation
- C01B33/027—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material
- C01B33/035—Preparation by decomposition or reduction of gaseous or vaporised silicon compounds other than silica or silica-containing material by decomposition or reduction of gaseous or vaporised silicon compounds in the presence of heated filaments of silicon, carbon or a refractory metal, e.g. tantalum or tungsten, or in the presence of heated silicon rods on which the formed silicon is deposited, a silicon rod being obtained, e.g. Siemens process
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/24—Deposition of silicon only
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/46—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for heating the substrate
Abstract
The present invention overcomes the limitations of Siemens reactors by providing for the deposition reaction to occur inside of a sealed crucible rather than inside of the overall cavity of a water-cooled reactor. The crucible itself is positioned inside of a cartridge reactor, which can have heat shields between crucible and the reactor walls to significantly reduce radiant energy losses. Additionally, the ratio of deposition surface area to cavity volume in the crucible is much higher than that in the ratio of rod deposition surface area to overall cavity volume in Siemens reactors, which results in a much higher contact percentage of gas molecules with the deposition surfaces. This in turn results in a much higher actual conversion ratio of material in the gas to material on the deposition surfaces.
Description
Technical field
Present patent application mode by reference merges the U.S. Patent application No.12/597 that the name of submitting on October 22nd, 2009 is called " deposition of the high purity silicon of or liquid-vapo(u)r interface gas-solid by high surface area and via the recovery (Deposition of high-purity silicon via high-surface-area gas-solid or gas-liquid interfaces and recovery via liquid phase) of liquid phase ", 151(" ' 151 patent application ") full content.The application also mode by reference merges the full content that the name of simultaneously submitting to above-mentioned patent application is called the common pending application of " for the deposition cylinder (DEPOSITION CARTRIDGE FOR PRODUCTION OF MATERIALS VIA THE CHEMCIAL VAPOR DEPOSITION PROCESS) of the material produce via chemical vapor deposition process " (its application number increases after knowing).The name that present patent application also requires to submit on July 1st, 2011 is called the U.S. Provisional Patent Application No.61504148(" ' 148 temporary patent application " of " for the deposition cylinder (Deposition cartridge for production of high-purity amorphous and crystalline silicon and other materials) of highly purified amorphous silicon and crystalline silicon and other material produce ") right of priority, and the name submitted to is called the U.S. Provisional Patent Application No.61504145(" ' 145 temporary patent application " of " for the barrel reactor (Cartridge reactor for production of high-purity amorphous and crystalline silicon and other materials) of highly purified amorphous silicon and crystalline silicon and other material produce " on July 1st, 2011) right of priority, its full content is incorporated to herein by reference at this.In ' 151 patent applications, term " deposition plate " is defined as the surface that silicon deposits thereon, but in this patent application, when describing actual physical feature, for clearer object, " deposition surface " is defined as to the surface that material deposits thereon, and " deposition plate " is defined as material thereon, the actual physics dull and stereotyped (with respect to its edge, its side has the object of much bigger surface-area) preferably depositing on two sides and one or more edge.Therefore, the side of deposition plate and edge are deposition surfaces.Term " deposition cylinder " is defined as to the combination of distribution pillar and deposition of solids plate or is defined as simply the deposition plate of tortuous pattern, any one be associated with insulation layer wherein or distance piece.Term " siemens (Siemens) reactor " is defined as to deposition reactor, and its initial design is for utilizing seed rod.
Background technology
The restriction of Siemens reactor has been described in ' 151 patent applications, and it comprises:
1. the harmonic(-)mean surface-area of polysilicon bar, its cause low volume deposition and therefore cause Siemens reactor compared with poor efficiency (turnout by polysilicon in preset time section is measured, annual several tonnes conventionally).
2. the low ratio of the surface-area of polysilicon bar and volume, it causes high energy consumption, and this energy consumption is to extend the deposition in the period and keep required surface temperature in order to realize, and this prolongations period is to deposit the required prolongation period of volume for realize target.
3. the characteristic that in bar felling process, labour intensive and being easy to is polluted.
The invention that ' 151 patent applications are described is by providing high surface area electric heating deposition plate to overcome these restrictions.Silicon is processed and is deposited on these plates by chemical vapor deposition (CVD) with high volume fraction, then by extra plate, heats to reclaim.Extra heating produces the deposit spathic silicon of thin layer very with liquefaction at board interface place, and the solid sclerderm of the polysilicon of deposition can be mechanically or by being pulled away from gravity slave plate.In Siemens reactor, use larger size panel with respect to using conventional seed rod, increased the productivity of reactor, yet, with respect to using seed rod, use small size plate to reduce the energy consumption of reactor, keep identical productivity simultaneously.Yet also there is further restriction in Siemens reactor, includes but not limited to:
1. the high radiating capacity loss from bar to reactor wall, must carry out reactor wall coolingly, deposits on wall preventing polysilicon is on depositing to bar.
2. the deposition gases molecule causing with the low ratio of the total cavity volume of reactor due to deposition table area and the low percentage that contacts of deposition table area.With respect to the theoretical yield being determined by molecular balance, low contact percentage causes silicon in gas to the low actual conversion of the silicon on bar.
Summary of the invention
The present invention is by making deposition reaction occur in the restriction that the crucible inside of sealing rather than the whole cavity inside of water-cooled reactor have overcome above-mentioned Siemens reactor.Owing to causing the loss of material to be produced, the deposition on reactor wall is undesirable, and deposition on crucible inwall is actual required, and it is because extra deposition table area has increased volume sedimentation rate.Crucible itself is positioned at barrel reactor inside, and it can have heat shield piece between crucible and reactor wall, significantly to reduce radiating capacity loss.Conventionally the energy up to 60%-70% using in Siemens reactor is lost to it not in the water wall of conductively-closed.
In addition, in crucible, deposition table area is more much higher than the ratio of Siemens reactor center pillar deposition table area and whole cavity volume with the ratio of cavity volume, this cause gas molecule higher with deposition surface contact per-cent.This causes again material in gas to the higher actual conversion of material on deposition surface.
Accompanying drawing explanation
Fig. 1 illustrates the elevation cross-sectional view of a preferred embodiment of the primary member of barrel reactor;
Fig. 2 illustrates the top plan view of a preferred embodiment of the primary member of barrel reactor;
Fig. 3 illustrates the skeleton view of a preferred embodiment of the deposition cylinder of barrel reactor;
Fig. 4 illustrates the elevation cross-sectional view of a preferred embodiment of the barrel reactor that has the base assemblies of decline and be mounted with crucible;
Fig. 5 illustrates the elevation cross-sectional view of a preferred embodiment of the barrel reactor of the reactor that has the base assemblies of rising and pressurizeed by rare gas element;
Fig. 6 illustrates the elevation cross-sectional view of a preferred embodiment of the barrel reactor with the crucible of rising and the deposition cylinder of preheating;
Fig. 7 illustrates the elevation cross-sectional view of a preferred embodiment of the barrel reactor in the serial process of deposition;
Fig. 8 is illustrated in reactor the elevation cross-sectional view of carrying out a preferred embodiment of barrel reactor in the process of directional solidification with rare gas element;
Fig. 9 illustrates the elevation cross-sectional view of a preferred embodiment of barrel reactor in cooling and air washing process;
Figure 10 illustrates the elevation cross-sectional view of a preferred embodiment of the barrel reactor that has the base assemblies of decline and be mounted with crucible;
Figure 11 illustrates the side cutaway view of a preferred embodiment of reactor top parts;
Figure 12 illustrates the place ahead elevation cross-sectional view of a preferred embodiment of reactor top parts;
Figure 13 illustrates the top plan view (upwards observing) of a preferred embodiment of reactor top parts;
Figure 14 is illustrated in the side elevation sectional view of a preferred embodiment of crucible between the depositional stage that gas flow pattern is shown;
Figure 15 is illustrated in the top plan view that a preferred embodiment of crucible after the deposition of material sclerderm is shown.
Embodiment
Fig. 1 illustrates the primary member for a preferred embodiment of the barrel reactor 50 of the material produce via CVD processing.In this embodiment, the effect of reactor top parts 1 is to support deposition cylinder 2(in ' 148 patent applications, ' 145 patent applications and the name of simultaneously submitting to are called the patent application of " for the deposition cylinder (DEPOSITION CARTRIDGE FOR PRODUCTION OF MATERIALS VIA THE CHEMCIAL VAPOR DEPOSITION PROCESS) of the material produce via chemical vapor deposition process " and have described this deposition cylinder), deposition gas mixture is distributed on the deposition surface of deposition cylinder 2, remove Exhaust Gas, and affect the heat exchange between Exhaust Gas and deposition gas mixture.If required the finished product are polycrystalline materials, the array of deposition cylinder 2 preferably has square top plan view, if or required the finished product are monocrystal materials, the array of deposition cylinder 2 preferably has circular top plan view.By thering is the reactor flange 9 of air seals, reactor top parts 1 is mounted to reactor intermediate module 3.Reactor intermediate module 3 accommodates crystallization well heater 4.Reactor bottom assembly 6 can rise to reactor intermediate module 3 or decline from it, and reactor bottom assembly 6 accommodates crucible holder 5, and crucible holder 5 is equipped with bottom coohng device 10, and for cooling crucible during directional solidification, and crucible holder 5 can vertically move.The all component of reactor is associated with heat shield piece, to minimize radiating capacity loss.
As shown in Figure 2, the reactor wall 35 of the reactor wall 35 of reactor top parts 1, the reactor wall 35 of reactor intermediate module 3 and reactor bottom assembly 6 is preferably circle in top plan view, and it also preferably uses water-cooled energy.If polycrystalline material is required, the top plan view of heat shield piece 13, the deposition cylinder top plan view of 2 arrays are, the top plan view of the top plan view of crystallization well heater 4 and bottom coohng device 10 is preferably square, if monocrystal material is required, above-mentioned top plan view is preferably circle.
Fig. 3 illustrates the skeleton view of a preferred embodiment of deposition cylinder 2 arrays that are mounted to reactor top parts.Deposition cylinder 2 is connected to power distribution rod 32 by its electrode contact blade 53 through electrode bracket 57.Have 16 deposition cylinders 2, these deposition cylinder 2 distances with about 5cm are spaced apart and have the height of about 42cm and the about length of 75cm.The thickness of supposing the deposition sclerderm on deposition cylinder 2 and on crucible inwall is about 2cm, in the preferred embodiment, by the Array Design of deposition cylinder 2, for fitting in the crucible inside of 85cm * 85cm, this crucible is generally used for the crystallization of deposition material (including but not limited to polysilicon).
The preferred embodiment of barrel reactor 50 operates with following preferred seven steps:
1. Fig. 4 illustrates crucible and loads step.Preferably, reactor bottom assembly 6 declines, and crucible 11(is preferably quartz) be accurately positioned on crucible holder 5.
2. Fig. 5 shows rare gas element washing step.Preferably, reactor bottom assembly 6 rises, and by 6 sealings of the airtight reactor flange of reactor bottom assembly and reactor intermediate module 3.Use gas feed and the outlet of gas reactor import 18 and reactor top parts 1, by rare gas element, reactor cavity is washed, rare gas element is preferably nitrogen.Preferably, also barrel reactor 50 is applied to working pressure (preferably in the scope of 6 bar).
3. Fig. 6 shows pre-heating step.Preferably, crucible holder 5 rises, and makes the top of crucible 11 compress seals 19 and form gas-tight seal.Preferably, then will deposit cylinder 2 electrical pre-heatings to optimal deposition temperature, when deposition material is polysilicon, optimal deposition temperature is preferably in the scope of 850 ℃ to 1150 ℃.Heat shield piece 13 in barrel reactor 50 minimizes radiating capacity loss, and the cooling power of the reactor wall 35 of water-cooled is minimized.
4. Fig. 7 shows deposition series of steps.Preferably, the gas feed of deposition gas mixture from reactor top parts 1 is pumped to crucible 11, while rare gas element remains in the rest part of the reactor cavity outside crucible, when deposition material is polysilicon, deposition gas mixture is preferably trichlorosilane and hydrogen or silicomethane, and rare gas element is preferably nitrogen.For safety, preferably, rare gas element, makes in the unlikely incident of leakage in seals 19 in slightly high pressure than deposition gases, and rare gas element will leak in crucible 11 rather than inflammable deposition gas mixture leaks into crucible 11 outsides.Alternatively, in the preferred embodiment, if exist and leak in reactor flange 9, rare gas element will leak to the outside of barrel reactor 50, rather than inflammable deposition gas mixture leaks to barrel reactor 50 outsides, this is to improve with respect to the additional safety of Siemens reactor.Seals 19 is preferably chosen as can bear relatively high temperature, has several preferred sealing member materials for this reason, and such as carbon-based material, but seals is preferably born relatively little pressure reduction.Preferably, the deposition gas mixture that is pumped to crucible 11 contacts with the deposition surface that is heated of deposition cylinder 2, and experience deposition reaction, is converted into Exhaust Gas, and shifts out through the pneumatic outlet of reactor top parts 1.In the preferred embodiment, this process lasts till that material sclerderm 14 is accumulated on deposition surface, and the most of void volume in crucible 11 is filled.Now, with suitable rare gas element, the inside and outside of crucible 11 washed, suitable rare gas element is preferably argon gas, and preferably to crucible 11 is inside and outside, all vacuumizes.Then, deposition surface is further heated to material melting point or on material melting point, make the layer material liquefaction at the deposition surface place of deposition cylinder 2, and material sclerderm comes off from deposition cylinder 2.
5. Fig. 8 shows crystallisation step.Preferably, the crucible holder 5 that is loaded with crucible 11 and material sclerderm 14 drops in reactor intermediate module 3, and further heats by 4 pairs of material sclerderm 14 of crystallization well heater, until it becomes fluent material 15.Preferably, heat shield piece 13 can be associated with reflecting layer, to minimize radiating capacity loss, and the insulation layer in outside, reflecting layer, to minimize, transmit and conduction energy waste.In the preferred embodiment, by one or more modes, realize directional solidification, which comprises the startup of bottom coohng device 10, the control of crystallization well heater 4 and/or crucible holder 5 leave the motion of crystallization well heater 4.In this crystallisation step process, close the heat shield piece 12 of rotation, to provide isolation in crucible 11 over top, thus minimum energy losses.Cured article 16 above moves up through fluent material 15, forms the block of crystalline material 17 at its rear.In another preferred embodiment of above-mentioned crystallisation step, by depositing cylinder 2 melting material sclerderm 14 completely, while crucible 11 is the position in rising completely still.Then, crucible 11 declines with controllable manner, and deposition cylinder 2 continues heating liquid silicon simultaneously, and starts bottom coohng device 10 to start directional solidification.The preferred embodiment can be accelerated crystallization treatment, and by cured article above 16 being kept to such an extent that more smoothly produce higher-quality silicon metal.Above-mentioned preferred embodiment is all realized the production of polycrystalline material, and array, crucible 11 and the bottom coohng device 10 of deposition cylinder 2 are preferably the square profile geometric shape of overlooking.Yet, in another preferred embodiment, if this overlooks profile geometric shape is circular, and rotating rod is introduced into fluent material 15 from reactor top parts 1, can also passes through vertical pulling crystallization (Czochralski crystallization) and process generation single crystal ingot.Finally, in another preferred embodiment, can omit this whole crystallisation step, and barrel reactor 50 is used in crucible and produces amorphous material, for further processing elsewhere.
6. Fig. 9 shows cooling and air washing step, in this step, with circulated inert gas, replaces vacuum, and cooling for convection current, rare gas element is preferably argon gas.After crucible abundant cooling, be convenient to subsequent disposal, rare gas element is by preparing for opening and reduce the air washing of reactor bottom assembly 6.In omitting the preferred embodiment of crystallisation step, the cooling of crucible 11 and material sclerderm 14 also can omit, to be suitable for the energy consumption minimizing in subsequent processing steps.
7. Figure 10 shows crucible unloading step.Preferably, open and reduce reactor bottom assembly, and unloading has the crucible 11 of block of crystalline material 17.
The feature of the preferred embodiment of barrel reactor 50 is effectively to distribute the deposition gas mixture obtaining in reactor top parts 1 with preheating.Figure 11 is the side elevation sectional view of reactor top parts 1, and in Figure 11, deposition gas mixture enters deposition gas mixture inlet manifold 29 via deposition gas mixture import 20.In the preferred embodiment, deposition gas mixture enters in a plurality of deposition gas mixture entry nozzles 24 according to path, this nozzle to downward-extension and directly above deposition cylinder 2 in the lower surface place of reactor top parts 1 opening.Deposition gas mixture penetrates through each deposition gas mixture nozzle 24, moves down, and impact crucible 11 bottoms between deposition cylinder 2.Leaving deposition gas mixture nozzle 24(preferably in downward air-flow) deposition gas mixture and deposition cylinder 2 between (also referring to Figure 12, Figure 13, and Figure 14 particularly), the blocking effect of the adjacent air-flow of the deposition gas mixture of impact crucible 11 bottoms minimizes the side diffusion of deposition gas mixture, and forces it preferably moving to refluxing significantly with eddy current or turbulent model.This turbulent flow preferably causes a contact more completely of deposition gas mixture and deposition cylinder 2, and therefore makes material in deposition gas mixture to the conversion more completely of the material on deposition surface.
In the preferred embodiment, Exhaust Gas continues upwards to advance, and locates it by Exhaust Gas, export loop turn 25 and shift out at this, and this loop turn is around deposition gas mixture entry nozzle 24 and be only vent path.This Exhaust Gas being heated of upwards advancing through Exhaust Gas outlet loop turn 25 heats the deposition gas mixture of advancing downwards through deposition gas mixture nozzle 24.This Exhaust Gas being heated also heats the water coolant that in Exhaust Gas aftercooler 26, advance in Exhaust Gas outlet loop turn outside.Other preferred embodiments of deposition gas mixture allocation model comprise the independent import replacing and outlet nozzle or the import replacing and outlet nozzle in a row.
A plurality of Exhaust Gas outlet loop turns 25 by Exhaust Gas from Exhaust Gas outlet manifold 27 are gathered into single stream, and leave reactor top parts through Exhaust Gas outlet 22.Meanwhile, the cooling-water flowing being heated in Exhaust Gas aftercooler 26, to deposition gas mixture preheater 28, provides initial heating at this to the deposition gas mixture that just enters deposition gas mixture entry nozzle 24.Then this water coolant leaves reactor top parts 1 through cooling water outlet 21.
Figure 11 and Figure 13 show a preferred embodiment of reactor top parts 1, and deposition gas mixture entry nozzle 24 is directly positioned on the interval between the deposition cylinder 2 being connected with power distribution rod 32.Figure 11 and Figure 13 also illustrate deposition cylinder 2 and are electrically connected to parallel way via power distribution rod 32, and power distribution rod 32 self is connected to power supply by power distribution rod electrode 31, and power distribution rod electrode 31 forms electrical isolation gas-tight seal with the sidewall of Exhaust Gas aftercooler 26.In another preferred structure, electrode contact blade 53 or electrode bracket 57 can extend past the top of reactor top parts 1 upwardly and outwardly via insulation steel pipe, and can be connected to power supply in the position at the top of reactor top parts 1.
Figure 15 shows from the preferred embodiment of the crucible 11 of deposition cylinder 2 depositions and after separating.The material depositing on the deposition surface of crucible 11 inwalls and deposition cylinder 2 is filled most of volume of crucible, and remains with narrow deposition cylinder space 36 in the appropriate location of deposition cylinder 2.
Barrel reactor is compared tool with Siemens reactor and is had the following advantages:
1. because the more high surface area having for depositing is realized volume sedimentation rate faster;
2. due to deposition table area and the higher ratio of deposition gas mixture volume, and contacted more completely with deposition gas mixture by the possible deposition surface constituting of deposition cylinder geometrical shape and gas inlet nozzle geometrical shape, realize in deposition gas mixture material to the higher actual conversion rate of material of material on deposition surface;
3. the conserve energy owing to minimizing the radiant heat loss that caused by deposition cylinder geometrical shape.The photothermal major portion of sending from the deposition surface that is heated is absorbed by adjacent deposition surface;
4. because the radiant heat loss, heat by conduction loss and the convective heat loss that minimize to water-cooled reactor wall realize conserve energy.The crucible that occurs in sealing due to deposition is inner, and the reactor wall of crucible outside can be stopped by heat shield piece;
5. due to depositing temperature rather than because surrounding temperature causes realizing conserve energy for the material melting of crystallization.No matter crystallization occurs in barrel reactor or in independent crystallization apparatus, and material is in crucible and do not need directly to process and therefore do not need to be cooled to surrounding temperature;
6. there is not the material contamination being caused by processing, and omit for reducing the operation of the pollution being caused by processing, such as acid etching;
7. omit by material be pressed into can process size piece to pack the operation of crucible into;
8. because deposition cylinder controllably exits from molten silicon, realize faster and higher-quality crystallization;
Therefore 9. because deposition gas mixture changes into Exhaust Gas more completely and make Exhaust Gas still less to the processing in barrel reactor downstream, thereby save shop equipment;
With in Siemens reactor for the single electrode of each coupled columns to comparing, with in parallel or be connected in series the power system that the list of deposition cylinder forms electrode and be simplified;
11. remain on the pressure slightly higher than the deposition gas mixture in crucible owing to inflammable deposition gas mixture being sealed in to the extra pars intramuralis of crucible and the rare gas element in reactor cavity, have increased like this security;
12. designs that are easy to peel off.Increase simply barrel reactor overlook cross section with the height that comprises the longer deposition cylinder of the deposition gas mixture entry nozzle of greater amt and greater amt and increase deposition cylinder can increase significantly barrel reactor throughput and without other parts that redesign barrel reactor.For the indirect heating with melting material, realizing the directional solidification that is easy to peel off is a challenge, but is heated and can be realized from its controlled exiting the directional solidification that is easy to peel off by molten silicon by deposition cylinder.
Claims (2)
1. for produce a method for material via chemical vapor deposition process, comprising:
A. provide can with the container of the sealing of freeboard around;
B., the deposition surface that can be heated and can be arranged on described internal tank is provided;
C. provide deposition gas mixture to enter flowing of described container, avoid deposition gas mixture flowing in described container freeboard around simultaneously;
D. provide Exhaust Gas to flow out flowing of described container, avoid Exhaust Gas flowing in described container freeboard around simultaneously;
E. described deposition surface is arranged in described container, seals described container, heat described deposition surface, make deposition gas mixture flow into described container and make Exhaust Gas flow out described container with described freeboard around, make material sclerderm deposit on described deposition surface and fully fill the void volume of described container;
F. stop and washing the deposition gas mixture stream that enters described container, and with the following any-mode continuous production cycle:
I. in the situation that described deposition surface consists of the material identical with described deposition material, open simply described container, and reclaim by the described container of fully filling for the described material sclerderm of further processing;
Ii. in the situation that described deposition surface compare with material to be produced by thering is the material of high melting temperature more or combination of materials forms and solid phase prod is required:
1. described deposition surface is further heated to the described melt temperature of described material or on described melt temperature, make the layer material liquefaction of described deposition surface interface, and material sclerderm comes off;
2. open described container and make described in the deposition surface that is heated separated with the material sclerderm coming off in described container;
3. reclaim by the described container of fully filling for the material sclerderm of further processing;
Iii. in the situation that described deposition surface compare with material to be produced by thering is the material of high melting temperature more or combination of materials forms and fused product is required:
1. described deposition surface is further heated to the described melt temperature of described material or on described melt temperature, and keeps described deposition surface to contact with described material until described material melting;
2. open described container and make described in the deposition surface that is heated separated with the melting material in described container;
3. reclaim by the described container of fully filling for the melting material of further processing;
Iv. in the situation that described deposition surface compare with material to be produced by thering is the material of high melting temperature more or combination of materials forms and crystalline product is required:
1. described deposition surface is further heated to the described melt temperature of described material or on described melt temperature, and keeps described deposition surface to contact with described material until described material melting;
2. open described container and make described in the deposition surface that is heated separated with melting material with controlled speed, thereby the specific cooling and crystallization of generating material;
3. reclaim by the described container of fully filling for the crystalline material of further processing.
2. for produce method and the reactor of material via chemical vapor deposition process, comprising:
A. provide can with the reactor of the sealing of freeboard around;
B., the container that can be arranged on described inside reactor and can seal with all the other freeboards of described inside reactor is provided;
C., the deposition surface that can be heated and can be arranged on described internal tank is provided;
D. provide deposition gas mixture from described reactor outside, to enter flowing of described internal tank in described reactor, avoid deposition gas mixture flowing in all the other freeboards of described inside reactor simultaneously;
E., Exhaust Gas flowing from the described internal tank in described reactor to described reactor outside is provided, avoids Exhaust Gas flowing in all the other freeboards of described inside reactor simultaneously;
F. described container is arranged on to described inside reactor and by described reactor and the sealing of freeboard around;
G. described deposition surface is arranged on to described internal tank, and all the other freeboard sealings from described inside reactor by described container;
H. heat described deposition surface, make deposition gas mixture flow into described container, and make Exhaust Gas flow out described container, make material sclerderm be deposited on described deposition surface and abundant void volume of filling described container;
I. stop and washing the deposition gas mixture stream that enters described container, and with the following any-mode continuous production cycle:
I. in the situation that described deposition surface consists of the material identical with described deposition material, open simply described container, open described reactor, and reclaim by the described container of fully filling for the material sclerderm of further processing;
Ii. in the situation that described deposition surface compare with material to be produced by thering is the material of high melting temperature more or combination of materials forms and solid phase prod is required:
1. described deposition surface is further heated to the described melt temperature of described material or on described melt temperature, make the layer material liquefaction of described deposition surface interface, and material sclerderm comes off;
2. open described container and make described in the deposition surface that is heated separated with the material sclerderm coming off in described container;
3. open described reactor and reclaim by the described container of fully filling for the material sclerderm of further processing;
Iii. in the situation that described deposition surface compare with material to be produced by thering is the material of high melting temperature more or combination of materials forms and fused product is required:
1. described deposition surface is further heated to the described melt temperature of described material or on described melt temperature, and keeps described deposition surface to contact with described material until described material melting;
2. open described container and make described in the deposition surface that is heated separated with the melting material in described container;
3. open described reactor and reclaim by the described container of fully filling for the melting material of further processing;
Iv. in the situation that described deposition surface compare with material to be produced by thering is the material of high melting temperature more or combination of materials forms and crystalline product is required:
1. described deposition surface is further heated to the described melt temperature of described material or on described melt temperature, layer material liquefaction and the material sclerderm of described deposition surface interface is come off;
2. with material described in following any-mode melting:
A. the deposition plate being heated by maintenance contacts with described material until material melting, thereby uses described deposition surface to carry out melting;
B. use at described external container but carry out melting at the well heater of described inside reactor, it comprises:
I. open described container, and the deposition surface being heated is separated with the material sclerderm coming off in described container;
Ii. use described well heater to carry out melting to the material in described container, described well heater is positioned at described external container but is positioned at described inside reactor;
3. with following any-mode, make described melting material crystallization:
A. the deposition surface of opening described container and making with controlled rate to be heated is separated with described melting material, thus the specific cooling and crystallization of generating material;
B. with controlled rate, provide the heating from described well heater, this well heater is positioned at described external container but is positioned at described inside reactor, thus the specific cooling and crystallization of generating material;
C., water cooler is provided, and this water cooler is positioned at described external container but is positioned at described inside reactor, and provides cooling from described water cooler with controlled rate, thus the specific cooling and crystallization of generating material;
D., rotating rod is provided, and this rotating rod immerses melting material and pulls out from melting material with controlled rate, thus the crystallization of generating material;
4. open described reactor and reclaim by the described container of fully filling for the crystalline material of further processing.
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US201161504145P | 2011-07-01 | 2011-07-01 | |
| US201161504148P | 2011-07-01 | 2011-07-01 | |
| US61/504,148 | 2011-07-01 | ||
| US61/504,145 | 2011-07-01 | ||
| PCT/US2012/045177 WO2013006523A1 (en) | 2011-07-01 | 2012-07-01 | Cartridge reactor for production of materials via the chemical vapor deposition process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103998648A true CN103998648A (en) | 2014-08-20 |
Family
ID=47437386
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201280042301.XA Pending CN103958732A (en) | 2011-07-01 | 2012-07-01 | Deposition cartridge for production materials via the chemical vapor deposition process |
| CN201280042405.0A Pending CN103998648A (en) | 2011-07-01 | 2012-07-01 | Deposition cartridge for production materials via the chemical vapor deposition process |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201280042301.XA Pending CN103958732A (en) | 2011-07-01 | 2012-07-01 | Deposition cartridge for production materials via the chemical vapor deposition process |
Country Status (8)
| Country | Link |
|---|---|
| EP (2) | EP2726646A1 (en) |
| JP (2) | JP2014522799A (en) |
| KR (2) | KR20140082638A (en) |
| CN (2) | CN103958732A (en) |
| IN (1) | IN2014MN00197A (en) |
| RU (2) | RU2014103707A (en) |
| TW (2) | TW201305376A (en) |
| WO (2) | WO2013006522A1 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB2534192B (en) * | 2015-01-16 | 2019-10-23 | Oxford Instruments Nanotechnology Tools Ltd | Surface Processing Apparatus and Method |
| JP2018123033A (en) * | 2017-02-02 | 2018-08-09 | 信越化学工業株式会社 | Method for producing polycrystalline silicon rod and polycrystalline silicon rod |
| JP6969917B2 (en) * | 2017-07-12 | 2021-11-24 | 信越化学工業株式会社 | Manufacturing method of polycrystalline silicon rod and polycrystalline silicon rod |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4710260A (en) * | 1982-12-22 | 1987-12-01 | Texas Instruments Incorporated | Deposition of silicon at temperatures above its melting point |
| CN101218175A (en) * | 2005-04-10 | 2008-07-09 | 瑞科硅公司 | Production of polycrystalline silicon |
| CN101707871A (en) * | 2007-04-25 | 2010-05-12 | 卡甘·塞兰 | Deposition of high-purity silicon via high-surface area gas-solid or gas-liquid interfaces and recovery via liqued phase |
| US20100272922A1 (en) * | 2009-04-24 | 2010-10-28 | Vithal Revankar | Process for Improved Chemical Vapor Deposition of Polysilicon |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5320680A (en) * | 1991-04-25 | 1994-06-14 | Silicon Valley Group, Inc. | Primary flow CVD apparatus comprising gas preheater and means for substantially eddy-free gas flow |
| JP5428303B2 (en) * | 2007-11-28 | 2014-02-26 | 三菱マテリアル株式会社 | Polycrystalline silicon manufacturing method |
| KR101115697B1 (en) * | 2009-12-02 | 2012-03-06 | 웅진폴리실리콘주식회사 | Cvd reactor with energy efficient thermal-radiation shield |
-
2012
- 2012-07-01 KR KR1020147002798A patent/KR20140082638A/en not_active Application Discontinuation
- 2012-07-01 EP EP12808029.8A patent/EP2726646A1/en not_active Withdrawn
- 2012-07-01 CN CN201280042301.XA patent/CN103958732A/en active Pending
- 2012-07-01 WO PCT/US2012/045176 patent/WO2013006522A1/en active Application Filing
- 2012-07-01 RU RU2014103707/02A patent/RU2014103707A/en not_active Application Discontinuation
- 2012-07-01 KR KR1020147002797A patent/KR20140082637A/en not_active Application Discontinuation
- 2012-07-01 EP EP12807788.0A patent/EP2726645A1/en not_active Withdrawn
- 2012-07-01 WO PCT/US2012/045177 patent/WO2013006523A1/en active Application Filing
- 2012-07-01 RU RU2014103710/02A patent/RU2014103710A/en not_active Application Discontinuation
- 2012-07-01 JP JP2014519212A patent/JP2014522799A/en active Pending
- 2012-07-01 JP JP2014519213A patent/JP2014523488A/en active Pending
- 2012-07-01 CN CN201280042405.0A patent/CN103998648A/en active Pending
- 2012-07-02 TW TW101123832A patent/TW201305376A/en unknown
- 2012-07-02 TW TW101123695A patent/TWI472654B/en not_active IP Right Cessation
-
2014
- 2014-01-30 IN IN197MUN2014 patent/IN2014MN00197A/en unknown
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4710260A (en) * | 1982-12-22 | 1987-12-01 | Texas Instruments Incorporated | Deposition of silicon at temperatures above its melting point |
| CN101218175A (en) * | 2005-04-10 | 2008-07-09 | 瑞科硅公司 | Production of polycrystalline silicon |
| CN101707871A (en) * | 2007-04-25 | 2010-05-12 | 卡甘·塞兰 | Deposition of high-purity silicon via high-surface area gas-solid or gas-liquid interfaces and recovery via liqued phase |
| US20100272922A1 (en) * | 2009-04-24 | 2010-10-28 | Vithal Revankar | Process for Improved Chemical Vapor Deposition of Polysilicon |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2014522799A (en) | 2014-09-08 |
| WO2013006523A1 (en) | 2013-01-10 |
| CN103958732A (en) | 2014-07-30 |
| RU2014103707A (en) | 2015-08-10 |
| TW201305376A (en) | 2013-02-01 |
| RU2014103710A (en) | 2015-08-10 |
| KR20140082638A (en) | 2014-07-02 |
| WO2013006522A9 (en) | 2013-02-14 |
| IN2014MN00197A (en) | 2015-08-21 |
| JP2014523488A (en) | 2014-09-11 |
| WO2013006522A1 (en) | 2013-01-10 |
| EP2726645A1 (en) | 2014-05-07 |
| TW201305400A (en) | 2013-02-01 |
| TWI472654B (en) | 2015-02-11 |
| EP2726646A1 (en) | 2014-05-07 |
| KR20140082637A (en) | 2014-07-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102084038B (en) | Direct silicon or reactive metal casting | |
| CN102120579B (en) | Method and device for efficiently and continuously smelting and purifying polysilicon with electron beams | |
| JP5530351B2 (en) | Precipitation of high-purity silicon using a high surface area gas-solid or gas-liquid interface and recovery from the liquid phase | |
| CN1364203A (en) | Method and apparatus for chemical vapor deposition of polysilicon | |
| CN102145894B (en) | Method and device for smelting and purifying polysilicon by using electron beams and adopting slag filtering | |
| US4265859A (en) | Apparatus for producing semiconductor grade silicon and replenishing the melt of a crystal growth system | |
| KR20110120617A (en) | A high-throughput apparatus for manufacturing silicon ingots for the polycrystalline silicon solar cell | |
| CN103998648A (en) | Deposition cartridge for production materials via the chemical vapor deposition process | |
| CN200971318Y (en) | Microwave heating and purifying device for silicon material | |
| CN103420380A (en) | Method and device for manufacturing polycrystalline silicon by coupling electron beam smelting technology and directional solidification technology | |
| CN102120578B (en) | Method and device for coupling and purifying polysilicon and removing phosphorus and metal with electron beams | |
| CN102408112A (en) | Method and equipment for purification of polysilicon by using electron beam melting under action of high purity silicon substrate | |
| CN201309981Y (en) | Vacuum electron-beam melting furnace for purifying polysilicon | |
| CN216863655U (en) | Silane thermal decomposition furnace capable of promoting uniform and compact deposition of zone-melting-level polycrystalline silicon | |
| CN102492980A (en) | Method and device for preparing silicon cores for polycrystalline silicon deposition | |
| US20140131911A1 (en) | Cartridge Reactor for Production of Materials via the Chemical Vapor Deposition Process | |
| CN101708849B (en) | Method and device of removing boron in polysilicon by local evaporation | |
| CN102060298A (en) | Polycrystalline silicon production device and method | |
| KR20100085299A (en) | Refine furnace for poly silicon | |
| CN201665537U (en) | Device for continuous production of liquid silicon | |
| CN202046892U (en) | Equipment for purifying polysilicon by efficient and continuous smelting of electron beams | |
| CN102787305A (en) | Device and method for reducing impurity deposit in chemical vapor deposition process | |
| KR101626645B1 (en) | Apparatus for producing polysilicon and preparation of polysilicon using same | |
| KR101821006B1 (en) | Apparatus and method for producing polycrystalline silicon using horizontal reactor | |
| CN202046890U (en) | Device for purifying polysilicon through vacuum melting of shallow molten pool |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20140820 |