• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    The present invention provides a process for the production of silicon and a production system for the production and extraction of silicon by grinding silicon carbide and quartz, mixing them in a predetermined ratio after purifying them, holding them in a crucible, heating them with a heating unit to cause them to react, oxidize the silicon carbide with the quartz and further reduce the quartz with the silicon carbide. The present invention further provides a process for the simultaneous production of silicon and silicon carbide and a production system for forming silicon carbide by forming a silicon carbide film by vapor phase epitaxy using active gas generated upon heating as a reaction material and recycling the silicon carbide film.
    公开号:SE1150277A1
    申请号:SE1150277
    申请日:2011-03-30
    公开日:2011-10-07
    发明作者:Takashi Tomita
    申请人:Takashi Tomita；
    IPC主号:
    专利说明:

    15 20 25 30 quartz stone as material is introduced from an upper part of the furnace due to the structure of the arc furnace, impurities whose vapor pressure is high will evaporate, and substances such as iron and nickel whose vapor pressure is low from the carbon electrodes, coke and quartz stone as material to gradually concentrated and incorporated into metallic silicon. It is clear that although phosphorus and other substances whose vapor pressure is high once evaporated during the reaction, they get stuck in an area whose temperature is low in the arc furnace and are returned to the original materials.
    An extremely important condition for silicon used for a semiconductor is that it contains few impurities. To ensure high purity, a leaching method is used in which calcium carbonate is mixed with remelted metallic silicon, dissolving the calcium silicate thus formed with acid, and dissolving and removing impurities absorbed in the calcium silicate. The degree of impurities as a result is equal to about 1 to 3 N at most, and no semiconductor properties are shown either. Hitherto, therefore, a process, the Siemens method, has been used for dissolving and evaporating silicon with high temperature hydrochloric acid, producing silicon tetrachloride or silicon trichloride, distilling and purifying it several times, producing highly purified silicon tetra- or highly purified silicon trichloride and silicon trichloride. further thermal decomposition of this with an electrified silicon wire and facilitating vapor phase epitaxy of silicon. As a result, a lot of electrical energy was consumed. Alternatively, a metallurgical process using oxidative vapor plasma silicon and removal of boron, keeping the metallic silicon in a vacuum and removing phosphorus, and finally slow cooling of the metallic silicon by one-way freezing and removal of impurities such as iron and nickel.
    H: DOCWORK Applicationlcxt, docx. 201 1-05-09 l IOO I 3EN 10 15 20 25 30 One reason why impurities are incorporated in silicon purified in the arc furnace is that not only impurities included in the quartz stone and coke as materials but also impurities in a furnace wall and the carbon electrode are mixed into the silicon as a product. As for the quartz stone and the coke, highly purified ones can be chosen for use, but the cost is then increased, of course.
    When these are ground to fine particles where sufficient cleaning effect is required, however, it is difficult to introduce the materials themselves into the arc furnace in which strong convection occurs. In addition, there is a risk that a metallic component such as iron is intentionally mixed in, especially in carbon for the electrode to prevent breakage when used at high temperature, and the contaminant is then passed further into the silicon.
    In order to effectively reduce the supply of electric power, a condition in which quite a lot of oxygen is available is desirable, and since silicon monoxide is also released gaseously when carbon monoxide generated in a reaction process is released from the furnace, the silicon monoxide outside the furnace is oxidized and regenerated. to silica. Since this amount accounts for 20 to 30% in normal commercial production, a heat recovery system is also required, as well as the removal of a bag filter and the investment amount for plant and equipment increases.
    The arc furnace is normally open, but since convection occurs, fine particles cannot be used in the supply of materials such as coke and quartz stone, but only solid material with a certain dimension can be added. Therefore, impurities included in the solid material cannot be so easily removed.
    In addition, the silicon formed is not required to be extracted continuously but intermittently.
    H: DOCWORK ApplicationEext.docx. 201 1-05-09 I 100 ISSE 10 15 20 25 30 The above-mentioned leaching process has disadvantages such as that highly purified calcium carbonate is required, energy for remelting silicon is required, and furthermore grinding of silicon, dissolution and removal of calcium silicate with acid is required, electrical energy is required , further silicon is lost and in addition acid and calcium carbonate are required. On the other hand, the Siemens method has an advantage in that the included pollutants can be reduced to a degree equivalent to about 9 to 11 N such as silane tetrachloride and silane trichloride and the silicon can be heavily purified, however, the Siemens method has a problem that the silicon becomes expensive on due to the high cost of the devices required for the use of chlorine and a large amount of electrical energy is required for the vapor phase epitaxin.
    The present invention has been made in view of the above problems. Fig. 1 is a schematic diagram for explaining the principle of a process for producing silicon and silicon carbide according to the present invention. Coke 51 and quartz sand (quartz) 52 as material are ground to about a few mm or less in advance. These are cleaned with an aqueous solution containing acid or alkali, and contaminants whose vapor pressure is low and moisture are removed. After coke 1 and quartz 2 have been prepared as described above, they are kneaded 53 in a predetermined ratio, to 1500 to 3000 degrees, and they are heated and silicon carbide 54 is obtained as an intermediate. Resistant heating is used as the heating method. A device that conducts gas is provided to prevent nitrogen in the air from being incorporated into the silicon carbide. This process also facilitates the removal of contaminants whose vapor pressure is high.
    H: DOCWORK Applicationstcxt.docx, 201 l-05-09 l IOOI3EN 10 15 20 25 30 The silicon carbide 54 which is an intermediate product is ground, and the ground silicon carbide 4 is mixed with highly purified quartz produced in it and the ground silicon carbide and the quartz of the above method, is heated to 1500 2000 degrees in a high frequency induction furnace 7 to cause them to react, and liquid molten silicon 55 is extracted. The liquid molten silicon can be crystallized in various ways.
    A process for producing silicon according to the present invention comprises the steps of grinding silicon carbide and quartz sand (quartz), the silicon carbide and the quartz sand (quartz) are mixed with each other in a predetermined ratio after re- (quartz) keeping them, the silicon carbide and quartz sand in a molten crucible for heating, they are heated by means of a heating means to cause them to react, and further the quartz sand (quartz) is reduced with the silicon carbide for the production and extraction of silicon.
    In the process for the production of silicon, the degree of impurity in the silicon carbide is equivalent to a high purity of 3 N or more, and the degree of impurity in the quartz sand is equivalent to a high purity of 3 N or more.
    In the process for producing silicon, the heater is high frequency induction heating.
    In the process for the production of silicon, the heating means is direct resistance heating.
    In the process for producing silicon, the heating crucible is made of silicon carbide.
    A process for the production of a silicon carbide semiconductor according to the present invention based on a silicon production process with the production and extraction of silicon by: mixing silicon carbide and silicon carbide and silicon carbide. quartz) with each other in a predetermined relationship after silicon vessels have been ground and purified; hollow bites and quartz sand (quartz) in silicon carbide and quartz sand (quartz) in a crucible; heating this to make them react; oxidation of the silicon carbide with the quartz sand (quartz); and further reducing the quartz sand (quartz) with the silicon carbide, which has the steps so that a silicon carbide film is formed by the vapor phase epitaxin by using active gas formed during the heating to react the material and recycle.
    A process for producing a silicon carbide semiconductor according to the present invention based on a process for producing and extracting silicon by: grinding carbon mixes with each other in holding them seal carbide and quartz sand (quartz); a predetermined ratio after purifying them; in a crucible for heating; heating this to make them react; oxidation of the silicon carbide with the quartz sand (quartz); and further reducing the quartz sand (quartz) with the silicon carbide, which has the steps of keeping carbon in silicon in a state of supersaturation by absorbing carbon from carbon monoxide and silicon from silica in liquid molten silicon separately produced by using the carbon monoxide and silicon monoxide in active gas formed upon heating of material, a silicon carbide film being formed by slow cooling and facilitating vapor phase epitaxy growth and recovery.
    In the process for producing a silicon carbide semiconductor, the heating crucible is made of silicon carbide.
    In the process for producing silicon, in the heating of the reaction, the crucible for heating is housed in a pressure bell to enable reaction in the case of a pressure-relieved state....................................
    In the process for producing a silicon carbide semiconductor, in the heating of the reaction, the heating crucible is housed in a pressure bell to enable reaction in a pressure-relieved state. The ratio In the process for the production of silicon, between silicon carbide and quartz sand (quartz) is mainly 1: 1, but 10: 1 can also be the maximum and 1:10 be the minimum.
    In the process for producing a silicon carbide semiconductor, the ratio of silicon carbide to quartz sand (quartz) is mainly 1: 1, but 10: 1 can also be the maximum and 1:10 be the minimum.
    In the process for producing silicon, the crucible for heating is housed in a pressure bell to enable reaction in inert gas.
    In the process for producing a silicon carbide semiconductor, the heating crucible is housed in the pressure bell for heating in inert gas.
    In the silicon production process, a crucible for recovery, the crucible for heating and the crucible for extraction are arranged in a cascade formation and are housed in the pressure bell to facilitate the reaction by heating.
    In the process for the production of silicon, a crucible for recovery, the crucible for heating and the crucible for extraction are provided, the crucible for heating and the crucible for extraction being arranged. ../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../../ .. are arranged in a cascade formation, and the molten crucible for recovery is arranged next to and along the crucible for heating, the crucible for recycling being designed so that a transverse dimension is longer and they are housed in the pressure bell to facilitate the reaction by heating.
    In the process for producing a silicon carbide semiconductor, a crucible for recovery, the crucible for heating and the crucible for extraction are provided, the crucible for heating and the crucible for extraction being arranged in a cascade formation, and the crucible for recycling being arranged and along the melting crucible for heating, the crucible for recycling being designed so that a transverse dimension is longer and they are housed in the pressure bell to facilitate the reaction by heating.
    A process for the production of silicon for the simultaneous production of silicon and silicon carbide based on a process for the production and extraction of silicon by: grinding silicon carbide and quartz sand (quartz); mixing the silicon carbide and the quartz sand (quartz) with each other in a predetermined ratio after purifying them; holding them in a crucible for heating; heating it by means of a heating means to cause them to react; oxidation of silicon vessels and further reduction of the bit with the quartz sand (quartz); (quartz) with the silicon carbide, silicon carbide film is formed by the quartz sand which has the steps of forming a vapor phase epitaxin using active gas formed upon heating of H: DOCWORK Application textducx. 201 1-05-09 110013513 10 15 20 25 30 reaction of the material, and silicon carbide is formed by recycling the silicon carbide film.
    A process for the production of silicon for the simultaneous production of silicon and silicon carbide based on a process for the production and extraction of silicon by: grinding silicon carbide and quartz sand (quartz); mixing silicon carbide and quartz sand (quartz) with each other in a predetermined ratio after purifying them; holding them in a crucible for heating; heating it by means of a heating means to cause them to react; oxidation of the silicon carbide with the quartz sand (quartz): and further reduction of the quartz sand (quartz) with the silicon carbide, which has the steps of keeping carbon in silicon in a state of supersaturation by absorbing carbon from carbon monoxide and silicon from silica in liquid molten silicon separately prepared by using the carbon monoxide and the silicon monoxide in active gas formed upon heating of material, a silicon carbide film being formed by epitaxial growth by slow cooling, and the silicon carbide being formed by recycling the silicon carbide film.
    In the process for producing silicon, a crucible for recovery, a crucible for heating and a crucible for extraction are provided, the crucible for heating and the crucible for extraction being arranged in a cascade formation, and the crucible for recovery being arranged next to and along with the crucible for heating, the crucible for recycling being designed so that a transverse dimension is longer, and silicon and silicon carbide being produced simultaneously by being housed in a pressure bell to facilitate reaction by heating.
    H: DOCWORK Application text, docx, 20l l-05 ~ 09 ll00l3EN 10 15 20 25 30 10 A system for producing silicon according to the present invention is provided with a heating crucible which contains silicon carbide and quartz sand (quartz) which are ground, purified and mixed, heating means which heat it and a crucible for extraction which contains silicon obtained by oxidizing the silicon carbide with the quartz sand (quartz), and further reducing the quartz sand (quartz) with the silicon carbide.
    A system for producing silicon carbide semiconductors is provided with a heating crucible which contains silicon carbide. and quartz sand purified and mixed, (quartz) which are ground, heating means which heat it, a melting crucible for extraction which contains silicon extracted by oxidizing the silicon carbide with the quartz sand (quartz), and further reducing the quartz sand (quartz) with the silicon carbide, recovery means recovering active gas formed during heating for reaction, and a melting crucible for recovery which recovers a silicon carbide film formed using active gas generated during heating to react material.
    In the silicon production system, a crucible for recovery, the crucible for heating and the crucible for extraction are provided, the crucibles being arranged in cascade formation, means for relieving pressure being provided, and the crucibles and the pressure relief means being housed in a pressure bell.
    In the silicon production system, a crucible for recovery, the crucible for heating and the crucible for extraction are provided, the crucible for heating and the crucible for extraction being arranged in cascade formation, H: DOCWORK Applicationstxx.docx. The melting crucible for recovery is arranged next to and along the melting crucible for heating, the melting crucible for recovery being designed so that a transverse dimension is longer, and the pressure crucibles are pressure relief means. are housed in a pressure clock.
    In the system for producing a silicon carbide semiconductor, the crucible for recovery, the crucible for heating and the crucible for extraction are provided, the crucibles being arranged in a cascade formation, a pressure relief means being provided, and the crucibles and pressure relief means being housed in a pressure cap.
    In the system for producing a silicon carbide semiconductor, the crucible for recovery, the crucible for heating and the crucible for extraction are provided, the crucible for heating and the crucible for extraction being formed in a cascade formation, the crucible for recovery being installed next to and heating, whereby the melting crucible for recycling is designed so that a cross-sectional dimension is longer, pressure relief means are arranged, the melting crucibles and pressure relief means are housed in a pressure bell.
    In the silicon production system, the ratio of silicon carbide to quartz sand (quartz) is 2: 1.
    In the system for producing a silicon carbide semiconductor, the ratio of silicon carbide to quartz sand (quartz) is 2: 1.
    In the silicon production system, heating is performed to effect a reaction under a state in which the pressure is lowered from 1 to 0.01 Pa.
    H: DOCWORK Application tcxt, docx. In the process for producing a silicon carbide semiconductor, heating is carried out to effect a reaction under a state in which the pressure is lowered from 1 to 0.01 Pa. 2A and 2B are Fig. Schematic drawings for explaining the operation of a reactor according to the present invention.
    As shown in Fig. 1, for the reaction products in the above-mentioned reaction process, carbon monoxide 56 and silicon monoxide 57 are generated, which are separately prepared in a container 10, and heat energy and the materials are recovered. For reaction products in the reaction process, SiO gas and carbon monoxide (CO) are dissolved by microwave or induction heating, and the recovery of silicon and carbon can be accelerated. For the recovery of these, liquid molten silicon 58 is used.
    Carbon monoxide 56 and silicon monoxide 57 are purified in the reduction process to be consumed by coke maintained at a high temperature, whereby the silicon monoxide 57 is formed. reacts with carbon and a silicon carbide film To add material, coke 50 may also need to be added.
    The silicon carbide film can not only be used as a material for purifying silicon but can epitaxially grow into silicon carbide II for a semiconductor by using carbon, silicon or silicon carbide or sapphire as a substrate.
    To use silicon for a semiconductor, the degree of impurity is adjusted to a sufficiently low level and the content can be increased to a high level equivalent to 6 to 11 N. In addition, H: DOCWORK Application text.docx, 201 1-05-09 110013EN 10 15 20 25 30 13 a considerable amount of energy and materials are saved. Furthermore, the highly purified silicon carbide film can grow.
    Induction heating has been described as a heating means, but it need hardly be mentioned that other electrical resistance heating can also be used.
    Silicon 55 can be stably and continuously purified by using silicon carbide 54 and quartz 52 as the material, supplying energy via an electromagnetic field or microwaves and forming a state shielded from the air. Silicon 55 formed by the process has extremely high purity and quality equivalent to a class of semiconductors can be achieved.
    After carbon monoxide generated at the end can be continuously extracted LN: and also can be used for preheating material, cleaning and purification of coke material and silicon material because heat generated in a carbon monoxide combustion process reduces excess energy and material, and silicon carbide can be extracted.
    Embodiments of the invention will now be described in detail based on the following drawings, in which Fig. 1 is a schematic diagram for explaining the principle of a process for producing silicon and silicon carbide according to the present invention, Figs. 2A and 2B are schematic views showing an induction heating reactor according to the present invention, in which Fig. 2A. is a schematic view showing the construction, and Fig. 2B is a schematic diagram for explaining the temperature distribution, Fig. 3 is a schematic view for illustrating the design of an induction heating 4 is a schematic reactor according to the present invention, Figs. Fig. 5 shows an illustration of the design of an induction heating reactor according to the present invention, and Fig. 5 shows silicon obtained with an induction heating reactor according to the present invention.
    First Embodiment Fig. 1 is a schematic diagram for explaining the principle of a process for producing silicon and silicon carbide according to the present invention. Figs. 2A and 2B are schematic views showing an induction heating reactor used in the present invention.
    Table 1 below shows the content of boron, phosphorus, calcium titanium, iron, nickel and copper which are impurities in coke as material, purified coke, quartz as material, purified quartz, silicon carbide and silicon in ppm units.
    H: DOCWORK Application text, docx, 201 1-05-09 ll00l3SE 15 m @ _ @ vm @ _ov m_ @ OH m. @ GH Hmgmox m @ _ @ v mo_ @ v m_ @ m m_ @ CH HwMuHz m @ _ @vm @. @ v mo OH m_ @ om: Hww mo_ov m @. @ v Ho OH m @ _o m QQHHH mo. @ vm @ _ @ v H om H OH e: HuH @ m mo_ @ vm @ _ @ v H_ @ HH ON HoHwo @ m @ .Ov m @. @ V H. @ m No w Hem UHQMQM .fi wm fl vH Hww fl ß WMOM WMOM HQWHM l fl wm fl M UMCÜM HMHHmwumZ UMGÜM .mGHHMPME mæ fi mcmUmWm m H Hcmum m fl mc Hmmmm m. ükningslexLdocx, 201 1-05-09 10 15 20 25 30 16 Coke as a material 51 ground in units of mm in advance. Table 1 shows the results of the analysis of contaminants in the coke.
    The coke as a material is purified with an aqueous solution. As a cleaning solution, HCN of 0.1 mol is used. After purification, the coke was dried at a temperature of 600 to 1200 ° C. During drying, contaminants whose vapor pressure is high are desorbed and removed from the coke, as in step 1.
    Quartz as a material 52 is ground in advance in units of mm. Table 1 shows the results of the analysis of impurities in the quartz. and the quartz is purified with an aqueous solution, heated and dried.
    The cleaning solution used is HCN of 0.1 mol, as step 2.
    As a cleaning solution, nitric acid, hydrochloric acid and hydrofluoric acid can be used in addition to HCN. The concentration and pH value are not really important for the base reaction, although the reaction time depends on them. Table 1 shows the results of the analysis of contaminants after purification.
    Material 53 obtained by mixing and kneading the quartz as material and coke as material prepared in the steps in a ratio of 1: 1 to 1: 3 is dried. The silicon carbide which is an intermediate product is produced by heating the dried material to activate it. To facilitate the reaction, a high temperature of 1500 to 2500 ° C is required, and for the heating method of the present invention, a resistance heating method is used. As 1500 to 3000 degrees desirable. heating temperature is Sublimation of contaminants H: DOCWORK Applicationstcxt.docx. 201 l-05-09 1 IOOISSE 10 15 20 25 30 17 is facilitated by reacting the dried material at the high temperature, as in step 3.
    In the heating step for activation, however, carbon monoxide and silica are generated, and the temperature can be raised by a reactant to a temperature equal to or exceeding 1500 degrees by oxidizing the dried material in an oxygen atmosphere. A reaction process lasts approximately 10 to 100 hours. Table 1 shows the results of the analysis of impurities in the silicon carbide in this case.
    As a heating means, any of a heliostat, a heating method by magnetization, microwave heating or induction heating can be used.
    Figs. 2A and 2B are schematic views for illustrating the induction heating reactor of the present invention. Fig. 2A is a schematic view for showing the structure, and Fig. 2B is a schematic diagram for explaining the temperature distribution.
    Fig. 3 is a schematic view for illustrating the design of an induction heating reactor according to the present invention, and Fig. 4 is a schematic view for illustrating the design of another induction heating reactor according to the present invention.
    The silicon carbide 54 generated in the above reaction step is ground, as step 4, mixed with the quartz, and heated up to 1500 to 2500 ° C in the multi-stage reactor 6 by an induction heating method. In the reactor, the quartz and the silicon carbide react with each other, and silicon, carbon monoxide and silicon monoxide are formed. When the silicon 55 is converted to liquid molten silicon, it drips from a melting crucible for heating 7 and is stored in a molten crucible for extraction 8. The silicon is at a stage in which extreme H: DOCWORK Application text.docx, 20l l-05-09 l 1001355 10 15 20 25 30 18 small amounts of contaminants occur. Silicon 55 of 28 is extracted from a total feed of 94 g of silicon carbide and quartz. The reaction is controlled depending on the amount of silicon carbide. silicon according to ICP.
    Table 1 shows the results of the analysis of contaminants in As a result, a highly purified semiconductor can be obtained. In the reactor of the present invention, a ratio of silicon carbide to quartz of 2: 1 is optimal.
    Fig. 5 is a view showing silicon made in accordance with the design of the present invention. In the graphite smelting crucible, silicon 55, silicon carbide 54 and quartz are produced.
    As shown in Fig. 1, the carbon monoxide 56 and the silicon monoxide 57 are introduced into the molten liquid silicon 58 in a recovery crucible 9 with the heat of the carbon monoxide and the silicon monoxide isolated. The carbon monoxide dissolves in the molten liquid silicon and the carbon is eluted. The silica monoxide dissolves in silica and silicon. Silica to about 50% is recycled. The recovery of reacted gas is further facilitated by high-frequency induction heating and pressure relief. In this design, the pressure is reduced from 1 to 0.01 Pa.
    When the silicon carbide substrate 11 is inserted into the melting crucible for recovery 9, the thickness of the substrate is initially increased from 0.25 mm to 0.35 mm. and epitaxial growth is enabled at 1800 degrees. For a growth rate, when the temperature rises in a range from 1500 to 2000 ° C, the thickness of the substrate can be increased and in addition, silicon carbide 59 can be recovered from the exhaust gases. The diameter of the crucible for recycling 9 is set to about 15 cm (6 inches) to enable a semiconductor substrate with a diameter of about 10 cm (4 inches) to be accommodated. The recovery of carbon monoxide further facilitates genonx to increase H: DOCWORK Applicationlcxt.docx. 20l l-05-09 1 l00l3EN 10 15 20 25 30 19 the size of the crucible for recycling 9. The reason is that the solubility of carbon in silicon increases. In this case, when ground coke is added to the molten liquid silicon number in a predetermined quantity, the growth rate can be further increased. discharged from the crucible for recycling 9 (the quartz) recovery 9 and returned to silicon 51, although it is a minimal proportion. At this time, excess heat and materials can be recovered. In the design shown in Fig. 2, the reactor is shaped as a vertical type, but to facilitate productivity and machinability, the reactor can also be designed as a horizontal type.
    Second Embodiment A second embodiment relates to a design for integrating the above-mentioned reaction process to increase the efficiency of the utilization of supplied energy. As shown in Fig. 2A, the basic process is the same as the basic process according to the first embodiment. Heating is accomplished using an induction heating coil 60 according to a high frequency induction method. Silicon carbide 54 is fed into a melting crucible for heating 7 via a conduit 63. Quartz 52 is supplied from the crucible for heating 7 through a conduit 65 to a silicon-holding / solidifying crucible 8 via a silicon extraction hole 61. Silicon 55 is thereby recovered.
    The above reactor is controlled for temperature distribution in three steps. Fig. 2B shows the temperature distribution. A top step is equivalent to a silicon carbide growth reactor 9 and the temperature T2 is 1500 to 2500 ° C. A middle step is equivalent to the molten crucible 7 for heating silicon vessels. H: DOCWORK Application txt.d0cx, 201 1-05-09 110013813 10 15 20 25 30 20 bid and quartz as material and the temperature is TO. Silicon, SiO and carbon monoxide are produced in this area. As a material in an outer wall, a carbonaceous material is used and one is used for an induction heating system heating process. Inside the outer wall, the crucible for carbon or silicon carbide and quartz is arranged. It is effective in reducing excess carbonaceous material from the crucible, so quartz or a ceramic material is further applied to the outside of the material of the outer wall.
    The hole 61 for extracting a silicon product is formed at the bottom of the crucible.
    The silicone 55 extracted through the extraction hole 61 flows into a melting crucible for extraction at the lowest stage of the reactor. It acts to more effectively remove unnecessary carbon and unnecessary silicon carbide so that an atmosphere at the lowest stage is made oxidative. to 1450 ° C.
    The temperature T1 is checked Silica once stored in the crucible for extraction can be produced continuously by being led into the solidification crucible via a feed-through pipe. As a solidification method, any of Czochralski's method, a solidification process and a rotary solidification process can be used. The content of oxygen is controlled to be at 10 to 0.1%. The solubility of carbon can be reduced by maintaining the oxidative atmosphere. Since the molten crucible is installed in the lower region 71 of the reactor, purified and discharged liquid molten silicon gradually solidifies and can be extracted in the form of an ingot. To realize this, for a procedure for keeping the temperature at T2, not only high frequency induction heating but also resistance heating can be used.
    A top region 72 of the reactor is used for the growth of silicon carbide. A window opening is arranged between a top H: DOCWORK ApplicationtextLdocx. 201 l-05-09 In IOÛBSE 10 15 20 25 30 21 area 72 and a middle area 71 and the window opening is designed to allow flow of a gas which is a mixture of SiO and CO from. the middle step. At the top step, a crucible 74 is provided. Silica carbide and molten resin can be used as materials in the crucible 74. In this design, its outer wall is made of carbon and the inside is made of silicon carbide or magnesium oxide or alumina.
    Molten silicon 76 is kept inside the melting crucible 74. A surface of the silicon is normally exposed to SiO and CO. As a result, CO is dissolved in the silicon. As a result, some of the silicon evaporates as SiO, however, SiO reacts mutually and separates into silicon and quartz.
    The quartz is deposited on the upper side of the silicon and a hole for supplying carbon 77 is provided and the quartz can be filled in molten liquid silicon. A quartz removal jig 78 is equipped to remove the quartz formed on the surface of the silicon 76 by a mechanical method. An inlet 80 is provided to supply a silicon carbide disk through a lid 79 arranged in an upper part, facilitating and epitaxial growth extraction of which the temperature is increased from T21 to T22, and the solubility of silicon carbide 59 again. carbon in silicon is improved to saturated solubility, deposited on an epitaxial substrate II while slowly cooling to T21, and the temperature is raised again after epitaxy and carbon is refilled. Graphite and silicon carbide can be used as substrates.
    The silicon carbide can continuously grow by repeating this operation (see Fig. 2).
    As shown in Figs. 3 and 4, the loss of silicon can be prevented by the mixing of oxygen and the incorporation of contaminants into silicon carbide by admixture of nitrogen by accommodating the entire multi-stage furnace in a container called pressure bell 75 and HÅDOCWORIO / Ansoksstextx! .Docx. 201 1-05-09 1 10013515 10 15 20 25 30 22 release air with an arranged pump 82. In this case a compressor 83 and opening valves 81, 84 are provided.
    In addition, the rate of the reaction between silicon carbide and quartz which are intermediates can be controlled by filling with inert gas such as argon, and further by controlling the pressure ratio. The rate of silicon generation is successively accelerated by lowering the pressure from 1 to 0.05 Pa and the rate of silicon formation can be successively stopped by increasing the pressure from 1 to 5 Pa.
    Third embodiment In the above-mentioned embodiments, the multi-stage furnace in which the reactors are arranged vertically has been used. However, since the reactive gas is forcibly forced upwards in the reactor to the uppermost stage, the surface of the silicon wafer can be covered with quartz when a silicon wafer for silicon carbide recovery is introduced. To deal with this problem, a multi-stage furnace is provided in which the reactors are arranged side by side. Fig. 4 shows the multi-stage furnace according to the third embodiment. Carbon monoxide and silicon monoxide, respectively, generated in a heating vessel 7 are led in laterally. A surface of a fed silicon wafer can be prevented from being covered with quartz by arranging the reactors side by side. In addition, since the reactor is pulled out laterally, more carbon monoxide and silicon monoxide can be recovered.
    Induction heating is used as the heating means, but it hardly needs to be mentioned that means such as electric resistance heating can also be used.
    In the present invention, highly purified silicon can be easily extracted without passing too many steps, as compared with the prior art.
    H: DOCWORK Applicationtextdocx, 201 1-05-09 110013515 10 15 23 In addition, since the generation temperature can be lowered, energy can be saved. Once impurities are mixed into the silicon, a lot of energy is required, but according to the present invention, impurities can be removed simultaneously in the production of silicon carbide which is the intermediate from materials from which impurities have been removed in advance, and thus the incorporation of impurities can be prevented when silicon is formed.
    In the present invention, in addition to the above-mentioned effects, since reactive gas can be recovered in the form of silicon carbide and the silicon carbide can be recovered at high speed and effectively in the form of a silicon wafer usable as an electronic device, the loss of material is reduced. The present invention can therefore make a significant contribution to the new silicon production technology.
    H: DOCWORK Application tcxt, docx. 20l1-05-09 1 IOOISSE
    权利要求:
    Claims (29)
    [1]
    A process for producing silicon, comprising the steps of: grinding silicon carbide and quartz sand (quartz); mixing silicon carbide and quartz sand (quartz) with each other in a predetermined ratio after purifying them; keep them in a crucible for heating; heat them with a heating device to make them react; and oxidizing the silicon carbide with the quartz sand (quartz); reduce the quartz sand (quartz) with the silicon carbide to produce and extract silicon.
    [2]
    A process for producing silicon according to claim 1, wherein: the degree of impurities in the silicon carbide is equivalent to high purity of 3 N or more; and the degree of contamination in the quartz sand is equivalent to high purity of 3 N or more.
    [3]
    A method for producing silicon according to claim 1, wherein high-frequency induction heating is used as the heating unit.
    [4]
    A method for producing silicon according to claim 1, wherein DC resistance heating is used as the heating unit.
    [5]
    A process for producing silicon according to claim 1, wherein the heating crucible is made of silicon carbide. H: DOCWORK Applicationtext.docx. 201 I-05-09 I 1001355 10 15 20 25 30 25
    [6]
    Process for the production of a silicon carbide semiconductor based on a process for the production and extraction of silicon by grinding silicon carbide and quartz sand (quartz), mixing silicon carbide and quartz sand (quartz) with each other in a predetermined ratio after purification of holding them in a crucible for heating, heating them with a heating unit to cause them to react, oxidizing the silicon carbide with the quartz sand (quartz), and further reducing the quartz sand (quartz) with the silicon carbide, the method comprising the steps of: forming a silicon carbide film of vapor phase epitaxy using active gas generated upon heating to react material; and recycling the silicon carbide film.
    [7]
    A process for producing a silicon carbide semiconductor based on a process for the production and extraction of silicon by grinding silicon carbide and quartz sand (quartz), mixing silicon carbide and quartz sand (quartz) with each other in a predetermined ratio after purification of holding them in a crucible for heating, heating them with a heating unit to cause them to react, oxidizing the silicon carbide with the quartz sand (quartz), and further reducing the quartz sand (quartz) with the silicon carbide, the method comprising the steps of: holding carbon in silicon in a state of supersaturation by absorbing carbon from carbon monoxide and silicon monoxide in molten liquid silicon produced by using carbon monoxide and silicon monoxide in active gas generated during heating as material; forming a silicon carbide film by epitaxial growth by slow cooling; and recycling the silicon carbide film. H: DOCwOlllOAnsökningslextdocx. 201 l-O5-09 1 IOOBSE 10 15 20 25 30 26
    [8]
    A method of manufacturing a silicon carbide semiconductor according to claim 6 or 7, wherein the heating crucible is made of silicon carbide.
    [9]
    A method for producing silicon according to claims 1 to 5, wherein upon heating for reaction, the crucible for heating is housed in a pressure bell to enable heating for reaction in a pressure-relieved state. of a semiconductor of ki-
    [10]
    A process for producing seal carbide according to claim 6 or 7, wherein upon heating for reaction, the crucible for heating is housed in a pressure bell to enable heating for reaction in a pressure-relieved state.
    [11]
    11. ll. A process for producing silicon according to claims 1 to 5, wherein: the ratio of silicon carbide to quartz sand (quartz) is substantially 1: 1; the ratio is a maximum of 10: 1; and the ratio is at least 1:10.
    [12]
    A process for producing a silicon carbide semiconductor according to claim 6 or 7, wherein: the ratio of silicon carbide to quartz sand (quartz) is substantially 1: 1; the ratio is at most 10: 1; and the ratio is at least 1:10.
    [13]
    A method for producing silicon according to claims 1 to 5, wherein the crucible for heating is housed in a pressure H: DOCWORK Applicationstcxt.docx. 2011-05-09 1 IOOISSE 10 15 20 25 30 27 clock to enable heating for reaction in inert gas.
    [14]
    A process for producing a silicon carbide semiconductor according to claim 6 or 7, wherein the heating crucible is housed in a pressure bell to enable heating for reaction in inert gas.
    [15]
    A method for producing silicon according to claims 1 to 5, wherein: a crucible for recovery, the crucible for heating and a crucible for extraction are provided; the crucible for recovery, the crucible for heating and the crucible for extraction are arranged in cascade formation and to facilitate reaction housed in a pressure bell by heating.
    [16]
    A process for producing silicon according to claims 1 to 5, wherein: a crucible for recovery, the crucible for heating and a crucible for extraction are provided; the crucible for heating and the crucible for extraction are arranged in cascade formation; the crucible for recovery is arranged next to and along the crucible for heating; the crucible for recycling is designed in a side dimension that is longer; and the crucible for recovery, the crucible for heating and the crucible for extraction are housed in a pressure bell to facilitate reaction by heating. production of a semiconductor of ki-
    [17]
    17. l7. A method for seal carbide according to claim 6 or 7, wherein: a melting crucible for heating, the crucible for heating and a melting crucible for heating and a melting crucible for heating. melting crucibles for extraction are provided; the crucible for heating and the crucible for extraction are arranged in cascade formation; the crucible for recovery is arranged next to and along the crucible for heating; the crucible for recycling is designed in a side dimension that is longer; and the crucible for recovery, the crucible for heating and the crucible for extraction are housed in a pressure bell to facilitate reaction by heating.
    [18]
    Process for the production of silicon for the simultaneous production of silicon and silicon carbide based on a process for the production and extraction of silicon by grinding silicon carbide and quartz sand (quartz), mixing silicon carbide and quartz sand (quartz) with each other in a predetermined ratio after purifying them, holding them in a crucible for heating, heating them with a heating unit to cause them to react, oxidizing the silicon carbide with the quartz sand (quartz), and further reducing the quartz sand (quartz) with the silicon carbide, the process comprising the steps of: : forming a silicon carbide film of vapor phase epitaxy using active gas generated upon heating to react material; and recovering the silicon carbide film to form silicon carbide.
    [19]
    19. Process for the production of silicon for the simultaneous production of silicon and silicon carbide based on a process for the production and extraction of silicon by grinding silicon carbide and quartz sand (quartz), mixing silicon carbide and quartz sand (quartz) with each other in a predetermined ratio H : DOCWORK Application time: xt, d0cx, 201 1-05-09 l 10013513 10 15 20 25 30 29 after cleaning them, keep them in a crucible for heating, heating them with a heating unit to get them reacting, oxidizing the silicon carbide with the quartz sand (quartz), and further reducing the quartz sand (quartz) with the silicon carbide, the process comprising the steps of: keeping carbon in silicon in a state of supersaturation by absorbing carbon from carbon monoxide and silicon monoxide in molten liquid silicon produced by use of carbon monoxide and silica monoxide in active gas generated during heating as material; forming a silicon carbide film by epitaxial growth by slow cooling; and recovering the silicon carbide film to form silicon carbide.
    [20]
    A silicon production system, comprising: a crucible for heating which. contains silicon carbide and quartz sand (quartz) which has been ground, purified and mixed; a heating unit that heats the crucible for heating; and a melting crucible for extraction containing silicon extracted by oxidizing the silicon carbide with the quartz sand (quartz), and: further reducing the quartz sand (quartz) with the silicon carbide.
    [21]
    A manufacturing system for a silicon carbide semiconductor, comprising: a heating crucible containing silicon carbide and quartz sand (quartz) ground, purified and mixed; a heating unit that heats the crucible for heating; and a melting crucible for extraction containing silicon extracted by oxidation of the silicon carbide with the quartz sand (quartz sand), and further reducing the quartz sand (quartz). ) with the silicon carbide; a recovery unit that recovers active gas generated upon heating for reaction; and a recovery crucible recovering silicon carbide film formed using the recovered active gas as the material.
    [22]
    A silicon production method according to claim 20, comprising: a crucible for recovery; the crucible for heating; the crucible for extraction; and a pressure relief unit, wherein: the crucibles are arranged in cascade formation; and the crucibles and pressure relief unit are housed in a pressure bell.
    [23]
    The silicon production process according to claim 20, comprising: a crucible for recovery; the crucible for heating; the crucible for extraction; and a pressure relief unit, wherein: the crucible for heating and the crucible for extraction are arranged in cascade formation; the crucible for recovery is located next to and along the crucible for heating; the crucible for recycling is designed with a side dimension that is longer; and the crucibles and pressure relief unit are housed in a pressure bell. H: DOCWORK Application lexdocx. 20 I 1-05-09 I 100 BSE 10 15 20 25 30 31
    [24]
    A silicon carbide semiconductor manufacturing system according to claim 21, comprising: a crucible for recycling; the crucible for heating; the crucible for extraction; and a pressure relief unit, wherein: the crucibles are arranged in cascade formation; and the crucibles and pressure relief unit are housed in a pressure bell. silicon carbide
    [25]
    A semiconductor manufacturing system according to claim 21, comprising: the crucible for recovery; the crucible for heating; the crucible for extraction; and a pressure relief unit, wherein: the crucible for heating and the crucible for extraction are arranged in cascade formation; the crucible for recovery is located next to and along the crucible for heating; the crucible for recycling is designed: down a side dimension that is longer; and the crucibles and pressure relief unit are housed in a pressure bell.
    [26]
    A process for producing silicon according to claims 1 to 5, wherein the ratio of silicon carbide to quartz sand (quartz) is 2: 1.
    [27]
    A process for producing silicon carbide according to claim 6 or 7, wherein the ratio of silicon carbide to quartz sand (quartz) is 2: 1. H: DOCWORK Ansökningslext.docx, 20l 105-09 1 1001355 32
    [28]
    A process for producing silicon according to claim 9, wherein heating is performed to effect reaction in a state in which the pressure is reduced from 1 to 0.01 Pa.
    [29]
    A process for producing a silicon carbide semiconductor according to claim 10, wherein heating is performed to effect a reaction in a state in which the pressure is lowered from 1 to 0.01 Pa. H: DOCWORK Application.ngstext.docx. 20l l-05 -09 1 100 ISSE
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    同族专利:
    公开号 | 公开日
    KR20110112223A|2011-10-12|
    NO20110671A1|2011-10-07|
    DE102011006888A1|2011-12-15|
    US20110243826A1|2011-10-06|
    SE1250593A1|2012-06-07|
    JP2011219286A|2011-11-04|
    TW201202139A|2012-01-16|
    CN102211771A|2011-10-12|
    US20120171848A1|2012-07-05|
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    法律状态:
    2015-03-31| NAV| Patent application has lapsed|
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