KR20140082638A - Cartridge reactor for production of materials via the chemical vapor deposition process - Google Patents

Cartridge reactor for production of materials via the chemical vapor deposition process Download PDF

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KR20140082638A
KR20140082638A KR1020147002798A KR20147002798A KR20140082638A KR 20140082638 A KR20140082638 A KR 20140082638A KR 1020147002798 A KR1020147002798 A KR 1020147002798A KR 20147002798 A KR20147002798 A KR 20147002798A KR 20140082638 A KR20140082638 A KR 20140082638A
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container
reactor
deposition
deposition surface
heated
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KR1020147002798A
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Korean (ko)
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케이갠 세란
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그린리 그룹 포 솔라 테크놀로지스 엘티디
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Publication of KR20140082638A publication Critical patent/KR20140082638A/en

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    • 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

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Chemical Vapour Deposition (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

The present invention overcomes the limitations of the Siemens reactor by allowing the deposition reaction to occur in a sealed crucible rather than in the entire cavity of a water-cooled reactor. The crucible itself is disposed within the reactor of the cartridge, which may have a heat shield (13) between the crucible and the reactor wall to significantly reduce radiant energy losses. Additionally, the ratio of the deposition surface area to the cavity volume in the crucible is much higher than the ratio of the rod deposition surface area to the total cavity volume in the Siemens reactor, resulting in a much higher contact ratio of gas molecules to the deposition surface. This results in a much higher actual conversion rate to the material on the deposition surface of the material in the gas.

Description

TECHNICAL FIELD The present invention relates to a cartridge reactor for producing a material through a chemical vapor deposition process. BACKGROUND OF THE INVENTION 1. Field of the Invention [0001]

This patent application is a continuation-in-part of US patent application Ser. No. 12 / 597,151, entitled "Deposition of High-purity Silicon through High Area Gas-Solid or Gas-Liquid Interfaces and Recovering Through Liquids," filed October 22, 151 patent application ") is incorporated by reference in its entirety.

This application is also incorporated by reference in its entirety as co-pending application entitled " Deposition Cartridge for the Production of Materials via Chemical Vapor Deposition Process " filed concurrently with this application (to be added when the application number is known) . The present application is also related to US patent application Ser. No. 61504148 ("'148 Patented"), and U.S. Provisional Patent Application Ser. Filed on July 1, 2006, entitled " A cartridge reactor for the production of high purity amorphous and crystalline silicon and other materials ", filed on Jul. 1, Are incorporated by reference in their entirety. In the '151 patent application, the term "deposition plate" is defined as the surface on which silicon is deposited, but when describing actual physical components in the present patent application for the purpose of improved clarity, "Deposition plate" is defined as an actual physical flat plate (an object with a significantly larger surface area on its side with respect to its edges) on which material is deposited, preferably on one or more edges as well as on one or more edges . The sides and edges of the deposition plate are therefore the deposition surface. The term "deposition cartridge" is defined as a combination of a distribution rod and a solid deposition plate, or simply as a meander pattern deposition plate, any of which may include an insulating layer or a spacer. The term "Siemens reactor" is defined as the deposition reactor originally designed to utilize a seed rod.

The '151 patent application describes the limitations of the Siemens reactor, including:

1. Low average surface area of the polysilicon rod resulting in low volumetric deposition rates and hence low Siemens reactor productivity (as measured by a predetermined time period per year, typically the mass of polysilicon produced over metric tons) .

2. A low percentage of the surface area to volume of the polysilicon rod, resulting in high energy consumption to maintain the surface temperature required to achieve deposition during the extended time period required to achieve a meaningful deposition volume.

3. Labor-intensive and pollution-prone characteristics of the harvesting process.

The present invention described in the '151 patent application overcomes the first and second limitations by providing a high area electrically heated deposition plate. Silicon is deposited on this plate in high volume ratios through CVD processing, and then resealed by further heating of the plate. The additional heating allows a very thin layer of polysilicon to be liquefied at the plate interface and the solid crust of deposited polysilicon can be pulled from the plate mechanically or by gravity. The use of large size plates in Siemens reactors increases reactor productivity with respect to using conventional seed rods, while the use of small size plates results in the same productivity with respect to using seed rods While reducing the energy consumption of the reactor. However, additional limitations of the Siemens reactor remain, including, but not limited to, the following:

1. From the rod, in addition to the rod, a high radiant energy loss to the reactor wall to be cooled to prevent the deposition of polysilicon on the wall

2. Low contact percentage of the deposition gas molecules to the deposition surface area due to the low ratio of the deposition surface area to the overall cavity volume of the reactor. The low actual conversion rate of silicon in the gas to the silicon on the rod, which is related to the theoretical conversion rate, controlled by the reaction equilibrium, is the result of a low contact percentage.

The present invention overcomes the limitations of the Siemens reactor described above by allowing the deposition reaction to occur in a sealed crucible rather than in the entire cavity of a water-cooled reactor.

Deposition at the inner wall of the reactor is undesirable because it results in loss of material to be produced, while deposition at the inner wall of the crucible is actually desirable because it increases the volume deposition rate due to the addition of deposition surface area. The crucible itself is disposed within the cartridge reactor, which can have a heat shield between the crucible and the reactor wall to significantly reduce radiant energy losses. Typically, 60-70% of the energy used by the Siemens reactor is their loss to the shieldless water-cooled wall.

Additionally, the ratio of the deposition surface area to the cavity volume in the crucible is much higher than the ratio of the total cavity volume to the load deposition surface area in the Siemens reactor, resulting in a higher contact percentage of gas molecules with the deposition surface. This results in a very high actual conversion rate of the material in the gas to the material on the deposition surface.

Figure 1 shows a front view of one preferred embodiment of the main components of a cartridge reactor.
Figure 2 shows a top view of one preferred embodiment of the main components of the cartridge reactor.
Figure 3 shows a perspective view of one preferred embodiment of a deposition cartridge for a cartridge reactor.
Figure 4 shows a front view of one preferred embodiment of a cartridge reactor in which the lower assembly is lowered and the crucible is loaded.
Figure 5 shows a front view of one preferred embodiment of a cartridge reactor in which the lower assembly rises and the reactor is pressurized with an inert gas.
Figure 6 shows a front view of one preferred embodiment of a cartridge reactor in which the crucible is raised and the deposition cartridge is preheated.
Figure 7 shows a front view of one preferred embodiment of a cartridge reactor during a deposition sequence.
Figure 8 shows a front view of one preferred embodiment of a cartridge reactor during directional solidification into an inert gas in the reactor
Figure 9 shows a front view of one preferred embodiment of a cartridge reactor during cooling and edge purging.
Figure 10 shows a front view of one preferred embodiment of a cartridge reactor in which the lower assembly is lowered and the crucible is unloaded.
Figure 11 shows a side elevational view of one preferred embodiment of a reactor top assembly.
Figure 12 shows a front view of one preferred embodiment of a reactor top assembly.
Figure 13 shows a top view (as viewed) of one preferred embodiment of the reactor top assembly.
Figure 14 shows a side elevational view of one preferred embodiment of a crucible during deposition showing a gas flow pattern.
Figure 15 shows a top view of one preferred embodiment of a crucible after deposition showing a material crust.

The main components of one preferred embodiment of the cartridge reactor 50 for the production of materials via CVD processing are shown in Fig. In this embodiment, the reactor top assembly 1 comprises a deposition cartridge 2 (which is described in the '148 and' 145 patent application and co-pending 'deposition cartridge for the production of materials through chemical vapor deposition' application) To distribute the deposition gas mixture on the deposition surface of the deposition cartridge 2, to remove the vent gas, and to affect the heat exchange between the vent gas and the deposition gas mixture. The array of deposition cartridges 2 preferably have a circular planar section if the final product required is a multicrystalline material and preferably a circular planar section if the final product required is a monocrystalline material. The reactor top assembly 1 is attached to the reactor intermediate assembly 3 by a reactor flange 9 comprising an airtight seal. The reactor intermediate assembly 3 houses the crystallization heater 4. The reactor lower assembly 6, which can be raised and lowered from the reactor intermediate assembly 3, has a lower cooler 10 for cooling the crucible during directional solidification and houses a vertically movable crucible pedestal 5. All assemblies in the reactor include a heat shield 13 to minimize radiant energy losses.

2, the reactor walls 35 of the reactor top assembly 1, the reactor intermediate assembly 3, and the reactor bottom assembly 6 are preferably circular in planar section and they are also preferably water cooled . The planar sections of the heat shield 13, the array of deposition cartridges 2, the crystallization heater 4 and the bottom cooler 10 are preferably square if a polycrystalline material is required and preferably circular if a single crystal material is required.

Figure 3 shows a perspective view of one preferred embodiment of an array of deposition cartridges 2 being fitted to a reactor top assembly. The deposition cartridge 2 is connected to the distribution bar 32 by an electrode bracket 57 by these electrode tabs 53. [ There are 16 deposition cartridges 2 spaced about 5 cm apart and about 42 cm high and about 75 cm long. Assuming a deposition crest thickness of about 2 cm on the deposition cartridge 2 and on the inner wall of the crucible, the array of deposition cartridges 2 in this preferred embodiment includes, but is not limited to, crystallization of the deposition material, Lt; RTI ID = 0.0 > 85 cm x 85 cm < / RTI >

This preferred embodiment of the cartridge reactor 50 operates in the following seven preferred steps:

1. The crucible-loading phase is shown in FIG. Preferably, the reactor lower assembly 6 descends, and preferably the crucible 11, which is preferably quartz, is placed exactly on the crucible pedestal 5.

2. An inert gas purge step is shown in FIG. Preferably, the reactor lower assembly 6 is elevated and the closed reactor flange 6 of the reactor lower assembly and reactor intermediate assembly 3 is sealed. The reactor cavity is purged with an inert gas, preferably nitrogen, using the reactor gas inlet 18 and the reactor top assembly 1 inlet and outlet. Preferably, the cartridge reactor 50 also reaches operating pressure (preferably in the range of 6 bar).

3. The preheating step is shown in Fig. Preferably, the crucible pedestal 5 rises so that the upper edge of the crucible 11 presses against the gas seal 19 to form a hermetic seal. Preferably, the deposition cartridge 2 is electrically preheated to an optimal deposition temperature, which is preferably in the range of 850 캜 to 1,150 캜 when the deposition material is polysilicon. The heat shield 13 in the cartridge reactor 50 minimizes radiant energy loss and minimizes the cooling duty of the water-cooled reactor wall 35.

4. The deposition sequence step is shown in Fig. Preferably, the deposition gas mixture, which is preferably trichlorosilane and hydrogen or monosilane when the deposition material is polysilicon, is pumped into the crucible 11 from the gas inlet of the reactor top assembly 1, The inert gas is retained in the remainder of the reactor cavity outside the crucible. Preferably, for safety reasons, the inert gas is at a somewhat higher pressure than the deposition gas, and the probability that leakage of gas from the gas seal 19 is low, rather than the leakage of the combustible deposition gas mixture out of the crucible 11 Rather, the inert gas will leak into the crucible 11.

Alternatively, in this preferred embodiment, if there is a leak in the reactor flange 9, the inert gas will leak out of the cartridge reactor 50 rather than the combustible deposition gas mixture leaking out of the cartridge reactor 50 , Which is an additional safety improvement over the Siemens reactor. The gas seal 19 preferably is selected to withstand a relatively high temperature, and while there is a preferred seal material such as a carbon-based material for it, the gas seal preferably experiences a relatively small differential pressure. Preferably, the deposition gas mixture pumped into the crucible 11 is brought into contact with the heated deposition surface of the deposition cartridge 2, undergoes a deposition reaction, is converted to a vent gas and passes through a gas outlet in the reactor top assembly 1 Removed. In this preferred embodiment, the process continues until the material crust 14 has accumulated on the deposition surface such that most of the empty volume inside the crucible 11 is filled. At this point, the inside and the outside of the crucible 11 are all purged with a suitable inert gas, preferably argon, and preferably a vacuum is drawn inside and outside the crucible 11. The deposition surface is then further heated to or above the melting point of the material so that the thin layer of material at the deposition surface of the deposition cartridge 2 is liquefied so that the material crust is separated from the deposition cartridge 2. [

5. The crystallization step is shown in Fig. Preferably, the crucible 11 and the crucible pedestal 5 supporting the material crust 14 descend into the reactor intermediate assembly 3 and the material crust 14 is heated by the crystallization heater 14 until it is the liquid material 15 (4). Preferably, the heat shield 13 may include a reflective layer that minimizes radiant energy loss and an insulating layer outside the reflective layer to minimize convective and conductive energy losses. In this preferred embodiment, the directional solidification is accomplished through one or more means including activation of the lower cooler 10, control of the crystallization heater 4, and / or movement of the crucible pedestal 5 leaving the crystallization heater 4 do. During this crystallization step, the rotary heat shield 12 is closed to provide insulation through the top of the crucible 11 to minimize energy loss. The solidification front 16 moves upward through the liquid material 15 and forms a crystalline material ingot 17 thereafter. In another preferred embodiment of the above crystallization step, the material crust 14 can be completely melted by the deposition cartridge 2, while still the crucible 11 is in a fully raised position. Next, the crucible 11 can be lowered in a controlled manner, while the deposition cartridge 2 continues to heat the liquid silicon and the lower cooler 10 is activated to initiate directional solidification. This preferred embodiment produces crystalline silicon of high quality by maintaining the flattened solidification front 16 as well as having a potential to accelerate the crystallization process. The preferred embodiments of both described above result in the production of a polycrystalline material and a square planar geometry is preferred for the array of deposition cartridges 2, the crucible 11, and the bottom cooler 10.

However, in another preferred embodiment, if the flat section geometry is circular and a rotating puller rod is introduced into the liquid material 15 from the reactor top assembly 1, then the polycrystalline ingot can also be produced by the Czochralski crystallization process have. Finally, in another preferred embodiment, such a total crystallization step may be omitted and the cartridge reactor 50 may be used to directly produce an amorphous material in the crucible for further processing elsewhere.

6. The cooling and air purging steps are shown in Fig. 9, wherein the vacuum is replaced by a circulating inert gas, preferably argon, for convective cooling. After sufficient cooling of the crucible to facilitate subsequent handling, Is purged with air in preparation for the unsealing and descent of the reactor lower assembly (6). In the preferred embodiment in which the crystallization step is omitted, cooling of the crucible 11 and the material crust 14 can also be omitted, so that the energy consumption in subsequent processing steps can be minimized as applied.

7. The crucible-unloading step is shown in Fig. Preferably, the reactor lower assembly is opened and lowered, and the crucible 11 with the crystalline material ingot 17 is unloaded.

A feature of the preferred embodiment of the cartridge reactor 50 is the effective distribution and preheating of the deposition gas mixture achieved in the reactor top assembly 1. In FIG. 11, which is a side front section of the reactor top assembly 1, the deposition gas mixture enters the deposition gas mixture inlet manifold 29 through the deposition gas mixture inlet 20. In this preferred embodiment, the deposition gas mixture is directed into a plurality of deposition gas mixture inlet nozzles 24 which extend downwardly to the lower surface of the reactor top assembly 1 directly above the deposition cartridge 2 and open. The deposition gas mixture is shot through each of the deposition gas mixing nozzles 24, moves downward between the deposition cartridges 2, and strikes the lower portion of the crucible 11. The blocking effect of the adjacent stream of the deposition gas mixture striking the lower portion of the crucible 11 minimizes the lateral diffusion of the deposition gas mixture and minimizes lateral diffusion of the deposition gas mixture from the deposition gas mixture nozzle 24, , And between the deposition cartridges 2, mostly inverted, preferably in a swirling or turbulent motion (see Figs. 12, 13 and in particular Fig. 14). This turbulent flow preferably leads to more complete contact of the deposition gas mixture with the deposition cartridge 2, and therefore a more complete conversion of the material in the deposition gas mixture to the material on the deposition surface.

In this preferred embodiment, the vent gas continues to move upwardly and is removed through the vent gas outlet annulus 25 surrounding the deposition gas mixture inlet nozzle 24 and only on the escape route. The heated vent gas moving upward through the vent gas outlet annulus 25 heats the deposition gas mixture moving downward through the deposition gas mixing nozzle 24 therein. It also heats the cooling water moving from the vent gas aftercooler 26 to the outside of the vent gas outlet annulus. Other preferred embodiments of the deposition gas mixture distribution pattern include individual alternating inlet and outlet nozzles or rows of alternating inlet and outlet nozzles.

Bent gas is collected in a single stream from the vent gas outlet plurality of vent gas outlet annulus (25) and exits the reactor top assembly through vent gas outlet (22). On the other hand, the cooling water heated in the vent gas after-cooler 26 flows directly into the deposition gas mixture inlet nozzle 24 and flows to the deposition gas mixture preheater 28, which provides initial heating for the deposition gas mixture. This cooling water is then discharged through the cooling water outlet 21 to the reactor top assembly 1.

11 and 13 show one preferred embodiment of the reactor top assembly 1 with the positioning of the deposition gas mixture inlet nozzle 24 just above the gap between the cartridges 2 attached to the distribution bar 32 Respectively. 11 and 13 also show a deposition cartridge 2 that is electrically connected in parallel through the distribution bar 31 and the distribution bar 32 itself is electrically insulated against the sidewalls of the vent gas after- And is connected to an electrical power supply through a distribution bar electrode 31 forming a sealed airtight seal. The electrode tab 53 or the electrode bracket 57 may extend through the upper end of the reactor top assembly 1 through an insulated steel tube and may be located at a point at the top of the reactor top assembly 1 It can be connected to a power supply.

A preferred embodiment of the crucible 11 after deposition and separation from the deposition cartridge 2 is shown in Fig. The material deposited on the inner wall of the crucible 11 and the deposition surface of the deposition cartridge 12 fill most of the volume of the crucible and the narrow deposition cartridge void 36 remains instead of the deposition cartridge 2. [

The preferred benefits of a cartridge reactor over a Siemens reactor are as follows:

1. A faster volumetric deposition rate due to the higher surface area for deposition.

2. A deposition gas to the material on the deposition surface resulting from more complete contact of the deposition surface and the deposition gas mixture possible by a combination of the deposition surface area relative to the deposition gas mixture receiving volume and the deposition cartridge geometry and the gas inlet nozzle geometry The high actual conversion rate of the material in the mixture.

3. Energy conservation because it minimizes radiant heat losses from the deposition cartridge geometry. Most of the radiant heat emitted from the heated deposition surface is absorbed by the adjacent deposition surface.

4. Energy savings due to minimized radioactive, conductive, convective heat loss to the water-cooled reactor walls. Since the deposition takes place in the sealed crucible, the reactor wall outside the crucible can be blocked by the heat shield 13.

5. Energy saving due to melting rather than the ambient temperature for crystallization of the material from the deposition temperature. Whether crystallization occurs in the cartridge reactor or in a separate crystallization apparatus, the material already exists in the crucible, need not be treated directly, and therefore does not need to be cooled to ambient temperature.

6. Removal of actions for decontamination of materials from handling and reduction of contamination from handling such as acid etching.

7. Removal of movement for pushing material into a chuck of manageable size for loading into the crucible.

8. Faster, higher quality crystallization due to controlled recovery of the deposition cartridge from molten silicon.

9. A more complete conversion of the deposition gas mixture into the vent gas, resulting in a reduction in vent gas for downstream processing in the cartridge reactor.

10. A simplified electrical system comprising a single electrode pair for connecting deposition cartridges in parallel or in series, as compared to individual electrode pairs for each rod pair in a Siemens reactor.

11. Increased safety due to the combustible deposition gas mixture sealed inside the additional wall of the crucible and the inert gas in the reactor cavity maintained at a somewhat higher pressure than the deposition gas mixture in the crucible.

12. Easily scalable design. Simply increasing the planar cross-section of the cartridge reactor to include a large number of deposition gas mixture inlet nozzles and a large number of long deposition cartridges and increasing the height of the deposition cartridge will increase the production capacity of the cartridge reactor without most of the re- Can be significantly increased. An easily scaled, directional solidification, which may be an attempt on an external heating furnace of the molten material, can be achieved through heating and controlled recovery of the deposition cartridge from the molten silicon.

Claims (2)

A method for producing a material through a chemical vapor deposition process,
a. Providing a container that can be sealed from a surrounding free space;
b. Providing a deposition surface that can be heated and placed in a container;
c. Providing a flow of the deposition gas mixture into the container while preventing the flow of the deposition gas mixture in the free space surrounding the container;
d. Providing a flow of vent gas to the exterior of the container while preventing the flow of vent gas in the free space surrounding the container;
e. Placing the deposition surface within the container, sealing the container from the surrounding free space, heating the deposition surface, allowing the deposition gas mixture to flow into the container, and allowing the vent gas to flow out of the container, So as to substantially fill the void volume of the container;
f. Stopping and purging the flow of the deposition gas mixture into the container and continuing the production cycle in one of the following ways:
i. In the case where the deposition surface is made of the same material as the laminate material, the container is simply opened and the container re-covered with a substantially filled crust of material for further processing,
ii. When the deposition surface is made from a material to be produced and a material or combination of materials having a higher melting temperature than the solid product,
1. further heating the deposition surface to a temperature of or above the melting temperature of the material so that the thin layer of material at the deposition surface interface is liquefied to separate the crust of the material,
2. Open the container, isolate the heated deposition surface from the separated crust in the container,
3. It is required to re-cover the container which is almost filled with the crust of material for further processing,
iii. When the deposition surface is made of a material or combination of materials having a higher melting temperature than the material to be produced and the molten product,
1. The deposition surface is further heated to or above the melting temperature of the material, and the deposition surface is maintained in contact with the material until the material is melted.
2. Open the container, isolate the heated deposition surface from the molten material in the container,
3. It is required to re-cover a container that is almost filled with molten material for further processing,
iv. When the deposition surface is made of a material or combination of materials having a melting temperature higher than the material to be produced and the crystalline product,
1. further heating the deposition surface to a temperature at or above the melting temperature of the material, contacting the material until the material is melted to maintain the deposition surface,
2. Open the container and isolate the heated deposition surface from the molten material at a controlled rate so that specific cooling and crystallization of the material occurs,
3. A method of manufacturing a material through a chemical vapor deposition process requiring re-covering of a container substantially filled with a crystallization material for further processing. A method and a reactor for producing a material through a chemical vapor deposition process,
a. Providing a reactor that can be sealed from the surrounding free space;
b. Providing a container which can be placed in the reactor and which can be sealed from the rest of the free space inside the reactor;
c. Providing a deposition surface that can be heated and positioned within the container;
d. Providing a flow of a deposition gas mixture from the exterior of the reactor to the interior of the container in the reactor while preventing the flow of the deposition gas mixture from the rest of the free space inside the reactor;
e. Providing a flow of vent gas from the interior of the container within the reactor to the exterior of the reactor while preventing the flow of vent gas from the rest of the free space inside the reactor;
f. Placing the container in the reactor and sealing the reactor from the surrounding free space;
g. Placing the deposition surface inside the reactor and sealing the container from the rest of the free space inside the reactor;
h. Heating the deposition surface to allow the flow of the deposition gas mixture into the container and allowing the flow of the vent gas to the exterior of the container so that a crust of material is deposited over the deposition surface to substantially fill the void volume of the container;
i. Stopping and purging the flow of the deposition gas mixture into the container and continuing the production cycle in one of the following ways:
i. If the deposition surface is made of the same material as the deposition material, simply open the container, unseal the reactor, re-cover the container which is nearly filled with the crust of material for further processing,
ii. When the deposition surface is made of a material to be produced and a material or combination of materials having a higher melting temperature than the solid product,
1. The deposition surface is further heated to a temperature at or above the melting temperature of the material so that the thin layer of material at the deposition surface interface is liquefied and the crust of the material is separated,
2. Open the container, isolate the heated deposition surface from the crust of discrete material in the container,
3. It is required to open the reactor and re-cover the container which is almost filled with the crust of material for further processing,
iii. When the deposition surface is made of a material or combination of materials having a higher melting temperature than the material to be produced and the molten product,
1. further heating the deposition surface to a temperature at or above the melting temperature of the material, contacting the material until the material is melted to maintain the deposition surface,
2. Open the container, isolate the heated deposition surface from the molten material in the container,
3. It is required to open the reactor and re-cover the container which is almost filled with molten material for further processing,
iv. When the deposition surface is made of a material or combination of materials having a higher melting temperature than the material to be produced and the crystalline product,
1. The deposition surface is further heated to a temperature at or above the melting temperature of the material so that the thin layer of material at the deposition surface interface is liquefied and the crust of the material is separated,
2. Melt the material in one of the following ways,
a. By bringing the material and the heated plate into contact with each other until the melting of the material, melting by the heated deposition plate
b. The following steps:
i. Opening the container, isolating the heated deposition surface from the crust of discrete material in the container,
ii. By melting the material in a container that is external to the container but has a heater internal to the reactor, it is possible to melt the material by a heater external to the container but internal to the reactor,
3. Crystallize the molten material by one of the following methods,
a. The container is opened and the heated deposition surface is isolated from the molten material at a controlled rate to cause specific cooling and crystallization of the material to occur,
b. Providing heating from the heater external to the container but internal to the reactor at a controlled rate such that specific cooling and crystallization of the material occurs,
c. It is external to the container but provides an internal cooler in the reactor and provides cooling from such a cooler at a controlled rate such that specific cooling and crystallization of the material occurs,
d. Providing a rotary pulldower rod that is dewatered into the molten material and pulled from the molten material at a controlled rate to cause crystallization of the material,
4. A method and a reactor for producing a material through a chemical vapor deposition process in which it is required to open the reactor and re-cover the container which is almost filled with crystallization material for further processing.
KR1020147002798A 2011-07-01 2012-07-01 Cartridge reactor for production of materials via the chemical vapor deposition process KR20140082638A (en)

Applications Claiming Priority (5)

Application Number Priority Date Filing Date Title
US201161504148P 2011-07-01 2011-07-01
US201161504145P 2011-07-01 2011-07-01
US61/504,145 2011-07-01
US61/504,148 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

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