JP2010090015A - Production apparatus and production method of silicon carbide single crystal - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a more practical production apparatus of a silicon carbide single crystal by which a silicon carbide single crystal with high growth efficiency and higher quality can be obtained, and to provide a production method thereof. <P>SOLUTION: The production apparatus of the silicon carbide single crystal is equipped with: a crucible 10 having a supply port 13 (14, 15) for supplying a sublimation raw material fine powder 5 together with a carrier gas 3 into the crucible, a crucible body 11 having a flow passage for supplying a gas produced by heating and sublimating the sublimation raw material fine powder 5 onto a silicon carbide seed crystal 2, and a discharge port 16 of the carrier gas 3; a silicon carbide seed crystal disposition part 12 placed inside the crucible 10 and close to the discharge port 16 so as to dispose a silicon carbide seed crystal 2; and an induction heating coil (heating means) 32 placed in the periphery of the crucible 10 and heating the crucible 10 to sublimate the sublimation raw material fine powder 5. Wherein, a silicon fine powder and a carbon fine powder are used as the sublimation raw material fine powder 5. <P>COPYRIGHT: (C)2010,JPO&INPIT

Description

  The present invention relates to a manufacturing apparatus and manufacturing method for a silicon carbide single crystal, and more particularly, a silicon carbide single crystal having a high growth efficiency and capable of obtaining a higher quality silicon carbide single crystal. Regarding the method.

  Silicon carbide is attracting attention as a small and high-power electronic device material such as a semiconductor because it has a larger band gap and is superior in dielectric breakdown characteristics, heat resistance, radiation resistance, and the like. In addition, silicon carbide has been attracting attention as an optical device material because it has excellent bonding properties with other compound semiconductors having excellent optical characteristics. Among such silicon carbide crystals, a silicon carbide single crystal has an advantage that it is particularly excellent in uniformity of characteristics in a wafer when applied to a device such as a wafer, compared to a silicon carbide polycrystal.

A sublimation method is used as a method for producing a silicon carbide single crystal. For example, in the modified Rayleigh method, the raw material powder and the seed crystal are placed in a graphite crucible at a position facing each other, heated to a high temperature of 2000 [° C.] or higher, and further reduced in pressure to 13332 [Pa] or lower. To recrystallize silicon carbide on the seed crystal. The important parameters in crystal growth are the temperature of the crystal to be grown, the supply amount of the source gas (sublimation gas: Si, Si ₂ C, SiC ₂ etc.), the pressure of the growth atmosphere, etc. There is no method for observing the inside of the crucible, and the temperature of the grown crystal can only be estimated by measuring the temperature of the outer surface of the graphite crucible at a position as close as possible to the grown crystal. Further, the supply amount of the source gas and the atmospheric pressure can only be inferred from the temperature of the outer surface of the graphite crucible at a position close to the raw material powder and the atmospheric pressure outside the crucible.

  Since the crucible is in a semi-closed state, the sublimation gas hardly leaks outside the crucible, and at the same time, there are significant differences in pressure and gas components inside and outside the crucible, making it difficult to understand the environment inside the crucible. It has become possible to estimate the inside of the crucible that has become a black box by utilizing a computer simulation or the like, but sufficient accuracy has not been obtained.

  Further, the raw material powder is enclosed in the graphite crucible and heated, but it is difficult to make the temperature of the raw material powder filling portion uniform, and in reality, a temperature distribution is generated in the raw material powder filling portion. Therefore, there is a problem that the sublimation from the high temperature portion is fast, the supply amount of the raw material gas is large at the initial stage of growth, and the supply amount of the raw material gas is reduced as the raw material in the high temperature part is reduced. Therefore, it is difficult to grow a uniform crystal because it is difficult to grow a crystal at a uniform speed. In addition, recrystallization occurs at a relatively low temperature portion of the raw material powder filling portion, which may prevent the raw material from being efficiently transported to the seed crystal, which hinders improvement in yield.

  As means for improving such problems, for example, in Japanese Patent Laid-Open No. 2001-233697 “Silicon carbide single crystal”, silicon dioxide ultrafine particles and carbon fine particles are supplied together with a carrier gas into a crucible provided with a silicon carbide single crystal. Thus, a method for growing a silicon carbide single crystal on a silicon carbide seed crystal has been proposed.

Japanese Patent Laid-Open No. 2002-154899 “Silicon Carbide Single Crystal Manufacturing Method and Manufacturing Device” supplies silane gas and propane gas into a crucible including a silicon carbide seed crystal, and silicon carbide is formed on the silicon carbide seed crystal. A method capable of growing a single crystal has been proposed.
JP 2001-233697 A JP 2002-154899 A

  In general, in the modified Rayleigh method of the sublimation method, it is only possible to indirectly estimate the crystal growth temperature and the pressure inside the crucible, and it is difficult to make the supply amount (sublimation amount) of the raw material constant throughout the growth process. However, there is a problem that it is difficult to keep the components of the sublimation gas constant throughout the growth process.

  In the technique disclosed in Patent Document 1 proposed to improve such a problem, there is an advantage that the supply amount of the raw material and the heating atmosphere are relatively easy to control, but oxygen is contained in the raw material. Thus, there is a possibility that impurities are taken into the silicon carbide single crystal. In addition, oxygen in the raw material may react with the graphite crucible, and the crucible may be severely damaged.

  The technique disclosed in Patent Document 2 also has an advantage that it is relatively easy to control the supply amount of raw materials and the heating atmosphere, but the problem is that the yield is poor because of the chemical reaction between silane gas and propane gas. was there.

  As described above, the modified Rayleigh method generally used in the single crystal growth of silicon carbide has a problem that it is difficult to control the environment such as temperature, pressure, and gas components because the crucible is used. A more practical silicon carbide single crystal production apparatus and production method capable of growing a single crystal at a predetermined rate (temperature, pressure and gas components) have been desired.

  The present invention has been made in view of the above-described conventional circumstances, has a high growth efficiency, can obtain a higher quality silicon carbide single crystal, and a more practical silicon carbide single crystal production apparatus and production It aims to provide a method.

  In order to achieve the above object, the silicon carbide single crystal production apparatus of the present invention comprises a supply port for supplying a sublimation raw material fine powder into a crucible together with a carrier gas, and a gas obtained by heating and sublimating the sublimation raw material fine powder. A crucible body having a flow path for supplying the silicon carbide seed crystal onto the silicon carbide seed crystal, a crucible having the carrier gas discharge port, and the silicon carbide seed crystal disposed on the discharge port side inside the crucible In the silicon carbide single crystal manufacturing apparatus, comprising: a silicon carbide seed crystal disposing portion; and a heating means disposed on an outer periphery of the crucible and heating the crucible to sublimate the raw material powder for sublimation. Silicon fine powder and carbon fine powder are used as the raw material fine powder. In addition, the silicon carbide seed crystal arrangement portion rotates about the longitudinal axis of the crucible.

  The method for producing a silicon carbide single crystal of the present invention includes a first step of supplying a sublimation raw material fine powder into a crucible in which a silicon carbide seed crystal is installed together with a carrier gas, and heating the sublimation raw material fine powder. And a third step of supplying the sublimated gas onto the silicon carbide seed crystal to grow the silicon carbide single crystal on the silicon carbide seed crystal. In the production method, silicon fine powder and carbon fine powder are used as the sublimation raw material fine powder. In addition, a silicon carbide single crystal is grown on the silicon carbide seed crystal while rotating the silicon carbide seed crystal about a crystal growth direction axis.

  According to the silicon carbide single crystal production apparatus and production method of the present invention having the above characteristics, since it is a partially open type furnace having a supply port with respect to a conventional closed type furnace, for example, a radiation thermometer Thus, the surface temperature of the silicon carbide seed crystal and the grown crystal can be measured, and a high-quality silicon carbide single crystal can be obtained by accurately grasping the sublimation atmosphere in the furnace. Further, by adjusting the supply amount of the sublimation raw material fine powder, the supply amount of the sublimation gas can be easily adjusted, and the growth rate of the silicon carbide single crystal can be controlled to be constant. In addition, since the raw material fine powder for sublimation can be continuously supplied, the length of the silicon carbide single crystal can be increased.

  In addition, by rotating the silicon carbide seed crystal arrangement portion about the longitudinal axis of the crucible, the sublimation gas can be supplied uniformly to the surface of the silicon carbide seed crystal and the growth crystal, and high quality silicon carbide A single crystal can be obtained. Furthermore, by using silicon fine powder and carbon fine powder as raw material fine powder for sublimation, homogeneous powder with narrow particle size distribution can be used as raw material, which can reduce raw material cost and higher quality silicon carbide single crystal Can be obtained.

  Hereinafter, examples of the manufacturing apparatus and the manufacturing method of the silicon carbide single crystal of the present invention will be described in detail in the order of [Example 1] and [Example 2] with reference to the drawings.

[Example 1]
FIG. 1 is a configuration diagram of a silicon carbide single crystal manufacturing apparatus according to Embodiment 1 of the present invention.

  In this figure, the silicon carbide single crystal manufacturing apparatus 1 of the present embodiment uses a supply port 13 for supplying a sublimation raw material fine powder 5 together with a carrier gas 3 into a crucible 10, and a gas sublimated from the sublimation raw material fine powder 5. A crucible body (graphite cylinder) 11 having a flow path for supplying the silicon carbide seed crystal 2 disposed on the silicon carbide seed crystal disposition portion 12, a crucible 10 having a carrier gas discharge port 16, and the inside of the crucible 10 A silicon carbide seed crystal disposition portion 12 disposed on the carrier gas discharge port 16 side and disposed around the longitudinal axis of the crucible 10 by disposing the silicon carbide seed crystal 2, disposed on the outer periphery of the crucible 10, and the crucible body 11 And an induction heating coil (heating means as defined in the claims) 32 for heating and sublimating the sublimation raw material fine powder 5 in the flow path.

  The supply port 13 includes a carrier gas supply port 14 and a sublimation raw material fine powder supply port 15. The carrier gas supply port 14 is provided at the end in the longitudinal direction of the silicon carbide single crystal manufacturing apparatus 1. In addition, the sublimation raw material fine powder supply port 15 is provided on the side of the crucible body 11 slightly downstream from the carrier gas supply port 14. The carrier gas discharge port 16 is provided at the end in the longitudinal direction opposite to the carrier gas supply port 14 in the silicon carbide single crystal manufacturing apparatus 1.

  Further, in the silicon carbide single crystal manufacturing apparatus 1 of the present embodiment, as a jig related to the crucible 10, heat insulation is sequentially performed between the crucible 10 and the induction heating coil 32 from the outside of the crucible 10 toward the induction heating coil 32. A material (carbon heat insulating material) 30, a quartz bottle 21, a water tank (cooling water tank) 22, and a quartz bottle 23 are provided. Further, flanges 24 and 25 are provided at both ends in the longitudinal direction of the silicon carbide single crystal manufacturing apparatus 1.

  Further, the silicon carbide seed crystal disposing unit 12 is rotated about the longitudinal center axis (crystal growth direction axis of the silicon carbide single crystal) of the crucible 10 by operating a driving means (not shown). In addition, since the silicon carbide single crystal manufacturing apparatus 1 of the present embodiment has a horizontal structure, when the silicon carbide seed crystal 2 is installed in the silicon carbide seed crystal arrangement portion 12, the silicon carbide seed crystal 2 is fixed. It is necessary to use fixing means such as an adhesive. As the adhesive, for example, resin, carbohydrate, heat-resistant fine particles, or the like is used.

  In addition, a radiation thermometer 34 for measuring the surface temperature of the silicon carbide seed crystal 2 and the grown crystal is installed in the vicinity of the longitudinal end of the silicon carbide single crystal manufacturing apparatus 1 on the channel extension of the crucible body 11. ing.

  In the silicon carbide single crystal manufacturing apparatus 1 of the present embodiment, the sublimation raw material fine powder 5 introduced from the sublimation raw material fine powder supply port 15 is supplied from the carrier gas supply port 14 by the structure as described above. The inside of the crucible body 15 flows along the flow of the carrier gas 3. At that time, the sublimation raw material fine powder 5 is heated by the induction heating coil 32 to be sublimated, and the sublimation gas is supplied onto the silicon carbide seed crystal 2 to grow as a silicon carbide single crystal. The carrier gas 3 is discharged from the carrier gas discharge port 16 to the outside of the silicon carbide single crystal manufacturing apparatus 1.

  Next, the manufacturing method of the silicon carbide single crystal by the silicon carbide single crystal manufacturing apparatus 1 of the present embodiment will be described. First, the silicon carbide seed crystal 2 is installed in the silicon carbide seed crystal arrangement part 12 in the crucible 10, the crucible 10 is heated to a high temperature by the induction heating coil 32, and the sublimation raw material fine powder 5 is supplied from the supply port 13 to the carrier gas. Put on 3 and throw. Then, the fine powder for sublimation 5 is sublimated in the flow path of the crucible body 11 and is transported to the surface of the silicon carbide seed crystal 2 as a sublimation gas, so that the silicon carbide seed crystal 2 is maintained at a slightly lower temperature than the crucible body 11. By doing so, a crystal is grown on the surface of the silicon carbide seed crystal 2.

  That is, the manufacturing method of the silicon carbide single crystal of this example includes (a) a first step of supplying the sublimation raw material fine powder 5 into the crucible 10 in which the silicon carbide seed crystal 2 is installed together with the carrier gas 3; (B) a second step of heating and sublimating the raw material powder 5 for sublimation; and (c) supplying the sublimated gas onto the silicon carbide seed crystal 2 to form a silicon carbide single crystal on the silicon carbide seed crystal 2. A third step of growing. Hereinafter, each step will be described in detail.

  (A) In the silicon carbide single crystal manufacturing apparatus 1, first, the carrier gas 3 is introduced into the crucible 10 from the carrier gas supply port 14, and the sublimation raw material fine powder 5 is introduced into the crucible 10 from the sublimation raw material fine powder supply port 15. Supply.

Here, as the carrier gas 3, it is desirable to use an inert gas that does not affect the sublimation of the sublimation raw material fine powder 5, such as argon gas or nitrogen gas. Here, argon gas is used. The supply amount of the carrier gas 3 is desirably supplied so that the supply amount of the sublimation raw material fine powder 5 is 1 to 5 [g / hour], and more appropriately xxx to yyy [g / hour]. It is particularly preferred to supply

  Further, as a raw material for crystal sublimation in silicon carbide single crystal growth, silicon carbide fine powder is generally used, but here, silicon fine powder and carbon fine powder are used. The weight ratio of the silicon fine powder to the carbon fine powder is preferably silicon fine powder: carbon fine powder = 1: 0.43 to 1: 2. This is because if the weight of the silicon fine powder is lower than the lower limit, it is difficult to increase the partial pressure of silicon gas, and if it is higher than the upper limit, silicon may not be sufficiently sublimated. Further, it is particularly preferable that the weight ratio of the silicon fine powder and the carbon fine powder is more suitably supplied so that the silicon fine powder: carbon fine powder = 1: 0.8 to 1: 1.4. In addition, the effect etc. by using a silicon fine powder and a carbon fine powder as the sublimation raw material fine powder 5 are mentioned later.

  (B) Next, the induction heating coil 32 is operated, and the sublimation raw material fine powder 5 is heated and sublimated. Here, the heating temperature is not particularly limited as long as the sublimation raw material fine powder 5 is sublimated, but is preferably set to 2200 to 2500 [° C.]. This is because if the heating temperature is lower than the lower limit value, the sublimation raw material fine powder 5 is not easily sublimated, and if the heating temperature is higher than the upper limit value, it is not economical and the apparatus is easily damaged. Moreover, it is particularly preferable that the heating temperature is 2300 to 2400 [° C.] more appropriately.

  (C) Next, a sublimation gas sublimated by heating is supplied onto the silicon carbide seed crystal 2 to grow a silicon carbide single crystal on the silicon carbide seed crystal 2. Here, the silicon carbide seed crystal 2 is not particularly limited and is appropriately determined according to the purpose of use. For example, various silicon carbide seed crystals such as 6H Rayleigh crystal and 6H Atchison crystal can be used. Here, for example, a 6H Rayleigh crystal (crystal thickness: 0.9 [mm], diameter 20 [mm]) is used.

  When growing the silicon carbide single crystal, the silicon carbide seed crystal 2 is rotated while rotating the silicon carbide seed crystal disposition portion 12 about the longitudinal central axis of the crucible 10 (the crystal growth direction axis of the silicon carbide single crystal). It is desirable to grow a silicon carbide single crystal on top. This is because the sublimation gas is uniformly supplied onto the silicon carbide seed crystal 2 so that a high-quality silicon carbide single crystal can be grown.

  Next, the sublimation raw material fine powder 5 which is a feature of the present invention will be described. As described above, silicon carbide powder is generally used as the sublimation raw material, and silicon carbide fine powder or silicon carbide fine powder to which silicon fine powder is added is used as the sublimation raw material fine powder 5. Is possible. In this case, silicon carbide has a plurality of polymorphs having different crystal structures, and it is difficult to obtain raw material powder composed of a single polymorph. Also, since different types of silicon carbides have different sublimation temperatures and pressures, the temperature of the graphite cylinder of the core, that is, the crucible body 11 is adjusted when using raw material powders mixed with different types of different types of polymorphs. There is a need to.

  Moreover, since silicon carbide is a very hard substance, it is difficult to obtain a fine powder with a very fine particle size. In the unlikely event that grains having a large particle diameter are mixed, they cannot be sublimated completely until they reach the silicon carbide seed crystal 2, and adhere to the surface of the silicon carbide seed crystal 2 as a solid. There is a risk of becoming the nucleus of the crystal. Furthermore, there is a problem that the silicon carbide fine powder is very expensive. Furthermore, many silicon carbide fine powders that can be obtained contain a large amount of nitrogen, and only n-type crystals can be grown by ordinary methods. High purity silicon carbide fine powder with a low nitrogen content is also commercially available, but it is very expensive. There is a circumstance that the particle size is large and the particle size distribution is wide.

  In the silicon carbide single crystal manufacturing apparatus and manufacturing method of the present example, instead of the silicon carbide fine powder or the silicon carbide fine powder to which the silicon fine powder is added as the sublimation raw material fine powder 5, the silicon fine powder and the carbon fine powder are used. Use powder. In the case of carbon fine powder, it is possible to obtain a finer powder that is finer than silicon carbide fine powder, which allows sublimation without leaving carbon fine particles by reaction with silicon gas. Crystal growth similar to that when the fine powder or the fine silicon carbide powder to which the fine silicon powder is added is used as the fine powder 5 for sublimation can be performed.

  Moreover, since silicon fine powder and carbon fine powder having higher purity than silicon carbide fine powder are available, the purity of the grown crystal can be improved. In addition, it is possible to intentionally dope the necessary elements in the growth process, and it becomes possible to freely make n-type, p-type or undoped silicon carbide single crystals. For example, in the case of an n-type silicon carbide single crystal, various techniques such as mixing nitrogen with the carrier gas 3 and in the case of a p-type silicon carbide single crystal, using aluminum fine powder doped with aluminum can be considered.

  Further, when silicon fine powder and carbon fine powder are used, there is no problem of different types of polymorphs unlike silicon carbide fine powder, and the temperature adjustment of the crucible body 11 becomes relatively easy. In addition, silicon fine powder and carbon fine powder are easily available as homogeneous powders with narrow particle size distribution and are much cheaper than silicon carbide fine powder, which can reduce raw material costs and higher quality. The silicon carbide single crystal can be obtained.

Next, the silicon carbide single crystal obtained by the silicon carbide single crystal production apparatus and production method of this example will be described. The silicon carbide single crystal preferably has a crystal defect (pipe defect) of 100 [pieces / cm ² ] or less, more suitably 10 [pieces / cm ² ] or less, which is nondestructive and optically image-detected. Is particularly preferred. The crystal defect can be detected by a well-known technique.

The silicon carbide single crystal obtained by the silicon carbide single crystal production apparatus and production method of the present example was not mixed with different polymorphs, and all consisted of a single polymorph (6H). Moreover, when the micropipe density of the obtained crystal was measured by the above-described method, it was 5 to 10 [pieces / cm ² ] in three trial manufactures, and a high-quality single crystal was obtained. Therefore, it is suitably used for electronic devices excellent in high voltage resistance, dielectric breakdown characteristics, heat resistance, radiation resistance and the like, particularly power devices and light emitting diodes.

  Moreover, when silicon carbide fine powder (commercially available as an abrasive) obtained by adding silicon fine powder to fine powder for sublimation was used, the growth crystal contained 200 to 500 [ppm] N (nitrogen). In the growth crystal using high-purity silicon fine powder and carbon fine powder as the sublimation raw material fine powder, N decreased to 50 ppm or less, and a significant improvement in purity was observed. By reducing the N content attributable to the raw material, it is possible to freely change the electrical conductivity of the grown crystal by mixing nitrogen gas whose flow rate is controlled into the carrier gas density.

  As described above, in the silicon carbide single crystal manufacturing apparatus of the present embodiment, the supply port 13 (14, 15) for supplying the sublimation raw material fine powder 5 together with the carrier gas 3 into the crucible, and the sublimation raw material fine powder. 5, a crucible body 10 provided with a flow path for supplying a gas sublimated by heating 5 onto the silicon carbide seed crystal 2, a discharge port 16 for the carrier gas 3, and a discharge port 16 side inside the crucible 10 And an induction heating coil (heating) that is arranged on the outer periphery of the crucible 10 and that sublimates the raw material powder 5 for sublimation by heating the crucible 10. Means) 32, a silicon fine powder and a carbon fine powder are used as the sublimation raw material fine powder 5. In addition, the silicon carbide seed crystal placement portion 12 rotates about the longitudinal axis of the crucible 10.

  Moreover, in the manufacturing method of the silicon carbide single crystal of the present embodiment, the first step of supplying the sublimation raw material fine powder 5 into the crucible 10 in which the silicon carbide seed crystal 2 is installed together with the carrier gas 3, and the sublimation raw material fine powder. A second step of heating and sublimating the powder 5; and a third step of supplying a sublimated gas onto the silicon carbide seed crystal 2 to grow a silicon carbide single crystal on the silicon carbide seed crystal 2. In the silicon carbide single crystal manufacturing method provided, silicon fine powder and carbon fine powder are used as the sublimation raw material fine powder 5. Further, a silicon carbide single crystal is grown on the silicon carbide seed crystal 2 while rotating the silicon carbide seed crystal 2 around the crystal growth direction axis. Furthermore, the weight ratio of the silicon fine powder to the carbon fine powder is preferably silicon fine powder: carbon fine powder = 1: 0.8 to 1: 1.4.

  Thus, in the silicon carbide single crystal manufacturing apparatus and manufacturing method of the present embodiment, since it is a partially open type furnace provided with the supply port 13 with respect to the conventional closed type furnace, for example, the radiation temperature The surface temperature of the silicon carbide seed crystal 2 and the grown crystal can be measured by a total of 34 and the like, and a high-quality silicon carbide single crystal can be obtained by accurately grasping the sublimation atmosphere in the furnace. Further, by adjusting the supply amount of the sublimation raw material fine powder 5, the supply amount of the sublimation gas can be easily adjusted, and the growth rate of the silicon carbide single crystal can be controlled to be constant. In addition, since the sublimation raw material fine powder 5 can be continuously supplied, the length of the silicon carbide single crystal can be increased.

  In addition, by rotating the silicon carbide seed crystal arrangement portion 12 about the longitudinal axis of the crucible, the sublimation gas can be supplied uniformly to the surface of the silicon carbide seed crystal 2 and the growth crystal, and high quality. A silicon carbide single crystal can be obtained. Furthermore, by using silicon fine powder and carbon fine powder as the raw material powder 5 for sublimation, a homogeneous powder having a narrow particle size distribution can be used as the raw material, and the raw material cost can be reduced and higher quality silicon carbide single powder can be used. Crystals can be obtained.

[Example 2]
Next, an apparatus and a method for manufacturing a silicon carbide single crystal according to Example 2 of the present invention will be described. FIG. 2 is a configuration diagram of a silicon carbide single crystal manufacturing apparatus according to Embodiment 2 of the present invention.

  In the figure, the silicon carbide single crystal manufacturing apparatus 101 of the present embodiment carbonizes the gas sublimated from the sublimation raw material fine powder 105, the supply port for supplying the sublimation raw material fine powder 105 together with the carrier gas 103 into the crucible 110. A crucible body (graphite cylinder) 111 having a flow path to be supplied onto the silicon carbide seed crystal 102 installed in the silicon seed crystal placement unit 112, a crucible 110 having a carrier gas discharge port 116, and a carrier inside the crucible 110 The silicon carbide seed crystal 102 is disposed on the gas discharge port 116 side, is disposed on the outer periphery of the crucible 110, and is disposed on the outer periphery of the crucible 110. And an induction heating coil (heating means referred to in the claims) 132 for heating and sublimating the sublimation raw material fine powder 105 in the flow path. There.

  As the supply ports, a carrier gas supply port 114 and a sublimation raw material fine powder supply port 115 are provided, and the carrier gas supply port 114 is an end in the longitudinal direction (upward) of the silicon carbide single crystal manufacturing apparatus 101. The sublimation raw material fine powder supply port 115 is provided on the side of the crucible main body 111 slightly downstream from the carrier gas supply port 114. The carrier gas discharge port 116 is provided at the end in the longitudinal direction (downward) opposite to the carrier gas supply port 114 in the silicon carbide single crystal manufacturing apparatus 101.

  In addition, in the silicon carbide single crystal manufacturing apparatus 101 of the present embodiment, as a jig related to the crucible 110, heat insulation is sequentially performed between the crucible 110 and the induction heating coil 132 from the outside of the crucible 110 toward the induction heating coil 132. A material (carbon heat insulating material) 130, a quartz jar 121, a water tank (cooling water tank) 122, and a quartz jar 123 are provided. Further, flanges 124 and 125 are provided at both ends in the longitudinal direction of the silicon carbide single crystal manufacturing apparatus 2.

  Further, the silicon carbide seed crystal placement unit 112 rotates around the longitudinal center axis (the crystal growth direction axis of the silicon carbide single crystal) of the crucible 110 by operating a driving means (not shown). A radiation thermometer 134 for measuring the surface temperature of the silicon carbide seed crystal 102 and the grown crystal is installed near the longitudinal end of the silicon carbide single crystal manufacturing apparatus 101 on the channel extension of the crucible body 111. ing.

  The apparatus for producing a silicon carbide single crystal of this example has a horizontal structure as the horizontal structure of Example 1, and the details of each component are substantially the same as those of Example 1. In addition, the silicon carbide single crystal manufacturing method by the silicon carbide single crystal manufacturing apparatus 101 of the present embodiment is almost the same as that of the first embodiment. Therefore, the same effect as that of the first embodiment can be achieved in the silicon carbide single crystal manufacturing apparatus and method of the present embodiment.

  In addition, since silicon carbide single crystal manufacturing apparatus 1 of Example 1 has a horizontal structure, silicon carbide seed crystal 2 is fixed when silicon carbide seed crystal 2 is placed in silicon carbide seed crystal placement portion 12. However, since the silicon carbide single crystal manufacturing apparatus 101 of the present embodiment has a vertical structure, the center in the longitudinal direction on the silicon carbide seed crystal arrangement portion 112 must be used. It is only necessary to place the silicon carbide seed crystal 102 on the shaft (rotating shaft), and the use of a fixing means such as an adhesive or a fixing step can be omitted. When silicon carbide seed crystal 102 may move due to carrier gas 103, a groove having a size slightly larger than silicon carbide seed crystal 102 is provided in silicon carbide seed crystal placement portion 112, and seed crystal 102 is placed there. Thus, the silicon carbide seed crystal 102 can be fixed at a predetermined position.

[Modification]
In the silicon carbide single crystal manufacturing apparatus 1 of the first embodiment, the carrier gas supply port 14 and the observation port for measurement by the radiation thermometer 134 are the same, and the silicon carbide single crystal manufacturing apparatus of the second embodiment is used. 101 has a different structure, but the first embodiment can be replaced with the same structure as the second embodiment, and the second embodiment can be replaced with the same structure as the first embodiment. is there.

It is a block diagram of the manufacturing apparatus of the silicon carbide single crystal which concerns on Example 1 of this invention. It is a block diagram of the manufacturing apparatus of the silicon carbide single crystal which concerns on Example 2 of this invention.

Explanation of symbols

DESCRIPTION OF SYMBOLS 1,101 Production apparatus of silicon carbide single crystal 2,102 Silicon carbide seed crystal 3,103 Carrier gas 5,105 Fine powder for sublimation 10,110 Crucible 11,111 Crucible body 12,112 Silicon carbide seed crystal arrangement part 13 Supply Port 14,114 Carrier gas supply port 15,115 Sublimation raw material fine powder supply port 16,116 Carrier gas discharge port 21,121 Quartz jar 22,122 Water tank 23,123 Quartz jar 24,25,124,125 Flange 32, 132 Induction heating coil (heating means)
34,134 Radiation thermometer

Claims (5)

A supply port for supplying the fine powder for sublimation together with a carrier gas into the crucible, a crucible body provided with a flow path for supplying a gas obtained by heating and sublimating the fine powder for sublimation to the silicon carbide seed crystal, and the carrier A crucible comprising a gas outlet;
A silicon carbide seed crystal disposition portion that is disposed on the discharge port side inside the crucible and in which the silicon carbide seed crystal is disposed;
In a silicon carbide single crystal manufacturing apparatus comprising: a heating means disposed on an outer periphery of the crucible, and heating the crucible to sublimate the raw material powder for sublimation.
A silicon carbide single crystal production apparatus using silicon fine powder and carbon fine powder as the sublimation raw material fine powder.   The said silicon carbide seed crystal arrangement | positioning part rotates centering on the longitudinal direction axis | shaft of the said crucible, The manufacturing apparatus of the silicon carbide single crystal of Claim 1 characterized by the above-mentioned. A first step of supplying a fine powder for sublimation into a crucible in which a silicon carbide seed crystal is installed together with a carrier gas;
A second step of heating and sublimating the sublimation raw material fine powder;
A third step of supplying a sublimated gas onto the silicon carbide seed crystal to grow the silicon carbide single crystal on the silicon carbide seed crystal, and a method for producing a silicon carbide single crystal comprising:
A method for producing a silicon carbide single crystal, wherein silicon fine powder and carbon fine powder are used as the sublimation raw material fine powder.   The weight ratio of said silicon fine powder and said carbon fine powder is silicon fine powder: carbon fine powder = 1: 0.43 to 1: 2, The manufacture of the silicon carbide single crystal of Claim 3 characterized by the above-mentioned. Method.   5. The silicon carbide single crystal is grown on the silicon carbide seed crystal while rotating the silicon carbide seed crystal about a crystal growth direction axis. 6. A method for producing a silicon carbide single crystal.

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