JP2007126335A - Manufacturing facility for manufacturing silicon carbide single crystal by means of solution method - Google Patents

Manufacturing facility for manufacturing silicon carbide single crystal by means of solution method Download PDF

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JP2007126335A
JP2007126335A JP2005321260A JP2005321260A JP2007126335A JP 2007126335 A JP2007126335 A JP 2007126335A JP 2005321260 A JP2005321260 A JP 2005321260A JP 2005321260 A JP2005321260 A JP 2005321260A JP 2007126335 A JP2007126335 A JP 2007126335A
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crucible
silicon carbide
single crystal
solution
carbide single
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Yukio Terajima
由紀夫 寺島
Hidemitsu Sakamoto
秀光 坂元
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Toyota Motor Corp
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Toyota Motor Corp
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<P>PROBLEM TO BE SOLVED: To provide a manufacturing facility for manufacturing a silicon carbide single crystal which inhibits the production of a silicon carbide polycrystal in a method for manufacturing silicon carbide single crystal by means of a solution method. <P>SOLUTION: The manufacturing facility 10 for manufacturing silicon carbide single crystal by means of the solution method comprises a crucible 2 for holding a solution containing silicon and carbon, a heating device 3 for heating the crucible, and a seed crystal holding part 6 for holding a seed crystal 5, wherein, during at least manufacturing the silicon carbide single crystal, a part 2a which is brought into contact with the liquid level of the solution of an internal surface of the crucible has a degree of surface roughness Ra of ≤2.0 μm. <P>COPYRIGHT: (C)2007,JPO&INPIT

Description

本発明は、いわゆる溶液法による炭化ケイ素単結晶の製造のための製造設備に関する。   The present invention relates to a production facility for producing a silicon carbide single crystal by a so-called solution method.

炭化ケイ素は、熱的、化学的に非常に安定であり、且つ耐熱性及び機械的強度に優れていることから、耐環境性半導体材料として期待されている。また特に炭化ケイ素単結晶は、高周波高耐電圧電子デバイスのためのウェハ、青色発光ダイオードの発光素子材料、高速半導体素子材料等の用途に関して期待されている。   Silicon carbide is expected to be an environmentally resistant semiconductor material because it is very thermally and chemically stable and has excellent heat resistance and mechanical strength. In particular, silicon carbide single crystals are expected for applications such as wafers for high-frequency, high-voltage electronic devices, light-emitting element materials for blue light-emitting diodes, and high-speed semiconductor element materials.

このような炭化ケイ素単結晶の成長方法としては、気相成長法、アチソン法、及び溶液成長法が知られている。   As such a silicon carbide single crystal growth method, a vapor phase growth method, an atchison method, and a solution growth method are known.

しかしながら気相成長法及びアチソン法は、得られる単結晶の欠陥、純度、生成速度等に関する問題があることが知られている。従って、溶液法が有望な炭化ケイ素単結晶の製造方法であると考えられる。ここでこの溶液法は、るつぼ内に保持されているケイ素と炭素とを含有する溶液に、炭化ケイ素単結晶からなる種結晶を接触させて、種結晶上に炭化ケイ素単結晶を成長させるものである。   However, it is known that the vapor phase growth method and the Atchison method have problems related to defects, purity, production rate and the like of the obtained single crystal. Therefore, the solution method is considered to be a promising method for producing a silicon carbide single crystal. In this solution method, a silicon carbide single crystal is grown on a seed crystal by bringing a seed crystal made of the silicon carbide single crystal into contact with a solution containing silicon and carbon held in a crucible. is there.

この溶液法に関し、特許文献１では、炭化ケイ素単結晶製造のためのケイ素及び炭素を含有する溶液に、遷移金属のうちの少なくとも１種の元素を更に含有させ、液相と炭化ケイ素固相との平衡が存在する相を提供することを開示している。この特許文献１では、このような遷移金属の添加によって、原料溶液中に含有される炭素の量を増加させることができ、従って炭化ケイ素単結晶の成長速度を大きくできるとしている。   With regard to this solution method, Patent Document 1 discloses that a solution containing silicon and carbon for producing a silicon carbide single crystal further contains at least one element of a transition metal, and a liquid phase and a silicon carbide solid phase. Providing a phase in which an equilibrium exists. In this Patent Document 1, it is stated that the amount of carbon contained in the raw material solution can be increased by adding such a transition metal, and therefore the growth rate of the silicon carbide single crystal can be increased.

また特許文献２では、溶液法に関し、るつぼの低温部、種結晶を保持する種結晶保持部の周囲等に炭化ケイ素多結晶が析出し、この炭化ケイ素多結晶が意図する炭化ケイ素単結晶の成長を妨げるという問題を認識している。この特許文献２ではこの問題を解決するために、原料溶液を保持しているるつぼを断熱し、且つ原料溶液の上面に加熱手段を提供して、原料融液全体が均温化されるようにしている。   Further, in Patent Document 2, regarding the solution method, a silicon carbide polycrystal is deposited around a low temperature portion of a crucible, around a seed crystal holding portion for holding a seed crystal, and the like, and the growth of the silicon carbide single crystal intended by this silicon carbide polycrystal Recognize the problem of preventing. In order to solve this problem, Patent Document 2 insulates the crucible holding the raw material solution and provides a heating means on the upper surface of the raw material solution so that the temperature of the entire raw material melt is equalized. ing.

特開２０００−２６４７９０号公報JP 2000-264790 A 特開平７−１７２９９８号公報JP-A-7-172998

本発明は溶液法による炭化ケイ素単結晶の製造方法において、特許文献２で指摘されるような炭化ケイ素多結晶の析出に関する問題を解決することを意図している。   The present invention is intended to solve the problem related to precipitation of polycrystalline silicon carbide as pointed out in Patent Document 2 in a method for producing a silicon carbide single crystal by a solution method.

本発明の発明者らは、炭化ケイ素単結晶を製造するための溶液法に関し、図４に示すような従来の炭化ケイ素製造設備４０では、ケイ素と炭素とを含有する溶液４の液面がるつぼ２の内側面と接触している箇所において、炭化ケイ素多結晶４ａが発生していること、及びるつぼ２の内側面の表面粗さがこの炭化ケイ素多結晶４ａの発生に影響を与えていることを見いだして、本発明に想到した。   The inventors of the present invention relate to a solution method for producing a silicon carbide single crystal. In a conventional silicon carbide production facility 40 as shown in FIG. 4, the liquid level of the solution 4 containing silicon and carbon is a crucible. That the silicon carbide polycrystal 4a is generated at a position in contact with the inner surface of the silicon carbide 2 and that the surface roughness of the inner surface of the crucible 2 affects the generation of the silicon carbide polycrystal 4a. As a result, the present invention has been conceived.

溶液法による炭化ケイ素単結晶の製造のための本発明の製造設備は、ケイ素及び炭素を含有する溶液を保持するるつぼ、るつぼを加熱する加熱装置及び種結晶を保持する種結晶保持部を有する製造設備であって、るつぼの内側面のうちの、少なくとも炭化ケイ素単結晶の製造の間に溶液の液面と接触する部分が、２．０μｍ以下、好ましくは１．８μｍ以下、より好ましくは１．６μｍ以下の面粗度Ｒａを有する、溶液法による炭化ケイ素単結晶の製造のための製造設備である。   The manufacturing equipment of the present invention for manufacturing silicon carbide single crystal by a solution method includes a crucible for holding a solution containing silicon and carbon, a heating device for heating the crucible, and a seed crystal holding unit for holding a seed crystal. Equipment, wherein at least the portion of the inner surface of the crucible that contacts the liquid surface of the solution during the production of the silicon carbide single crystal is 2.0 μm or less, preferably 1.8 μm or less, more preferably 1. This is a production facility for producing a silicon carbide single crystal by a solution method having a surface roughness Ra of 6 μm or less.

本発明の製造設備によれば、溶液の液面がるつぼの内表面に接触する箇所における炭化ケイ素多結晶の核生成を抑制して、炭化ケイ素多結晶の混入が少ない炭化ケイ素単結晶、特に炭化ケイ素多結晶の混入が実質的にない炭化ケイ素単結晶を製造することができる。尚、本発明に関して、面粗度Ｒａは、ＪＩＳ０６０１で規定される算術平均粗さＲａを意味する。   According to the production facility of the present invention, a silicon carbide single crystal, particularly a carbonized carbon, in which the silicon carbide polycrystal is less mixed by suppressing the nucleation of the silicon carbide polycrystal at the location where the liquid level of the solution contacts the inner surface of the crucible A silicon carbide single crystal substantially free of silicon polycrystals can be produced. In the present invention, the surface roughness Ra means the arithmetic average roughness Ra defined by JIS0601.

本発明の製造設備では、るつぼの内側面のうちの、少なくとも炭化ケイ素単結晶の製造の間に溶液の液面と接触する部分が、るつぼの内側面のうちの他の部分とは異なる材料で形成されていてもよい。   In the production facility of the present invention, at least a portion of the inner surface of the crucible that contacts the liquid surface of the solution during the production of the silicon carbide single crystal is made of a material different from the other portions of the inner surface of the crucible. It may be formed.

この態様によれば、るつぼの内側面のうちの溶液の液面と接触する部分を、他の部分を形成する材料よりも、小さい面粗度の達成及び／又は維持が容易な材料で形成することができる。従って例えばこの態様によれば、るつぼの内表面のうちの溶液の液面と接触する部分を、比較的耐久性の大きい材料、例えば炭化ケイ素、タングステン等でつくり、且つるつぼの他の部分を、比較的成形が容易な材料、例えばグラファイトで形成することができる。この場合には、グラファイト部分から溶液に対して炭素の供給が可能である点でも好ましい。   According to this aspect, the portion of the inner surface of the crucible that contacts the liquid surface of the solution is formed of a material that can easily achieve and / or maintain a smaller surface roughness than the material that forms the other portion. be able to. Thus, for example, according to this aspect, the portion of the inner surface of the crucible that contacts the liquid surface of the solution is made of a relatively durable material, such as silicon carbide, tungsten, and the other portion of the crucible. It can be formed of a material that is relatively easy to mold, such as graphite. In this case, carbon is preferably supplied to the solution from the graphite portion.

また本発明の製造設備では、るつぼの内側面のうちの、少なくとも炭化ケイ素単結晶の製造の間に溶液の液面と接触する部分が、るつぼの他の部分に対して脱着可能にされていてもよい。   Further, in the production facility of the present invention, at least a portion of the inner surface of the crucible that comes into contact with the liquid surface of the solution during the production of the silicon carbide single crystal is detachable from the other portions of the crucible. Also good.

この態様によれば、るつぼの内側面のうちの溶液の液面と接触する部分の面粗度が大きくなったときに、この部分のみを交換することができる。またこの態様では、上記の態様でのように、るつぼの溶液の液面と接触する部分と他の部分とを異なる材料で作ることが容易になる。   According to this aspect, when the surface roughness of the portion of the inner side surface of the crucible that comes into contact with the liquid level of the solution increases, only this portion can be replaced. Further, in this aspect, as in the above-described aspect, it becomes easy to make the portion that contacts the liquid level of the crucible solution and the other portion with different materials.

また更に本発明の製造設備では、るつぼの内側面のうちの、少なくとも炭化ケイ素単結晶の製造の間に溶液の液面と接触する部分が、るつぼの他の部分に対して脱着可能な炭化ケイ素製の管状体であり、且つるつぼの内表面の他の部分がグラファイト製であってよい。   Still further, in the production facility of the present invention, at least a portion of the inner surface of the crucible that comes into contact with the liquid level of the solution during the production of the silicon carbide single crystal is detachable from other portions of the crucible. The other part of the inner surface of the crucible may be made of graphite.

この態様によれば、るつぼの内側面のうちの溶液の液面と接触する部分が比較的耐久性の大きい炭化ケイ素であるによって、小さい面粗度を比較的維持することができ、且つるつぼの他の部分がグラファイト製であることによって、るつぼの製造を比較的容易にすることができる。またこの態様によれば、溶液の液面と接触する部分が、るつぼの他の部分に対して脱着可能であることによって、るつぼの内側面のうちの溶液の液面と接触する部分の面粗度が使用の間に大きくなったときに、この部分のみを交換することができる。   According to this aspect, the portion of the inner surface of the crucible that contacts the liquid level of the solution is relatively durable silicon carbide, so that a small surface roughness can be maintained relatively, and the crucible Since the other parts are made of graphite, the crucible can be manufactured relatively easily. Further, according to this aspect, the portion of the inner surface of the crucible that is in contact with the liquid surface of the solution is roughened by the portion that is in contact with the liquid surface of the solution being removable from the other portion of the crucible. When the degree grows during use, only this part can be replaced.

上述のように炭化ケイ素単結晶の製造のための溶液法は、るつぼ内に保持されているケイ素と炭素とを含有する溶液に、炭化ケイ素単結晶からなる種結晶を接触させて、種結晶上に炭化ケイ素単結晶を成長させるものである。   As described above, the solution method for producing a silicon carbide single crystal is obtained by bringing a seed crystal made of a silicon carbide single crystal into contact with a solution containing silicon and carbon held in a crucible, and then on the seed crystal. To grow a silicon carbide single crystal.

この溶液法によって炭化ケイ素単結晶を製造する場合、使用するケイ素と炭素とを含有する溶液は、最終的に得ることを意図している炭化ケイ素（ＳｉＣ）とは異なる組成を有する。これは、炭化ケイ素は加熱すると、昇華や分解を生じ、意図する組成、すなわちＳｉＣの組成の融液が得られないことによる。   When a silicon carbide single crystal is produced by this solution method, the solution containing silicon and carbon used has a composition different from that of silicon carbide (SiC) that is finally intended to be obtained. This is because when silicon carbide is heated, it undergoes sublimation and decomposition, and a melt having an intended composition, that is, a SiC composition cannot be obtained.

従って溶液法では一般に、意図する炭化ケイ素単結晶よりも炭素濃度が低いケイ素及び炭素の溶液を用い、且つこの溶液が、溶液を入れているるつぼの壁面から種結晶に向かって低下する温度分布を有するようにしている。これによれば、炭化ケイ素（ＳｉＣ）が比較的低温の種結晶部分において析出し、またこの炭化ケイ素の析出によって溶液から失われた炭素成分を補うようにして、溶液内を炭素が種結晶部分に向かって移動する。ここでこの炭化ケイ素の析出によって溶液から失われた炭素成分は、るつぼを炭素含有材料、特にグラファイト又は炭化ケイ素で作ることによってるつぼから供給することができる。   Therefore, the solution method generally uses a silicon and carbon solution having a carbon concentration lower than that of the intended silicon carbide single crystal, and this solution has a temperature distribution that decreases from the wall of the crucible containing the solution toward the seed crystal. To have. According to this, silicon carbide (SiC) precipitates at a relatively low temperature seed crystal portion, and carbon is lost in the solution by the silicon carbide precipitation, so that the carbon is seeded within the solution. Move towards. Here, the carbon component lost from the solution by the deposition of silicon carbide can be supplied from the crucible by making the crucible with a carbon-containing material, in particular graphite or silicon carbide.

炭化ケイ素単結晶の製造のための本発明の製造設備を、図１を参照して説明する。   The manufacturing equipment of the present invention for manufacturing a silicon carbide single crystal will be described with reference to FIG.

図１で示されているように、溶液法による炭化ケイ素単結晶の製造のための本発明の製造設備１０は、ケイ素及び炭素を含有する溶液４を保持するるつぼ２、このるつぼを加熱する加熱装置３及び種結晶５を保持する種結晶保持部６を有する。またこの本発明の製造設備１０では、るつぼ２の内側面のうちの、少なくとも炭化ケイ素単結晶の製造の間に溶液の液面と接触する部分２ａが、２．０μｍ以下の面粗度Ｒａを有する。尚、この図１に示す製造設備１０では、るつぼ２、加熱手段３等は、チャンバー１内に配置されている。   As shown in FIG. 1, the manufacturing equipment 10 of the present invention for manufacturing a silicon carbide single crystal by a solution method includes a crucible 2 for holding a solution 4 containing silicon and carbon, and heating for heating the crucible. A seed crystal holding unit 6 that holds the device 3 and the seed crystal 5 is provided. Further, in the manufacturing equipment 10 of the present invention, the surface roughness Ra of the inner surface of the crucible 2 that is in contact with the liquid surface of the solution at least during the manufacture of the silicon carbide single crystal is 2.0 μm or less. Have. In the manufacturing equipment 10 shown in FIG. 1, the crucible 2, the heating means 3, etc. are arranged in the chamber 1.

本発明の製造設備１０を用いて炭化ケイ素単結晶を製造する場合例えば、始めにるつぼ２にケイ素、炭素等の原料を充填し、チャンバー１内を真空にした後、アルゴン等の不活性ガスによってチャンバー１内を大気圧又はそれよりも高い圧力に加圧する。尚、るつぼ２としてグラファイト等の炭素含有材料製のるつぼを用いる場合、炭素はこのるつぼ２から溶融してくるため、炭素を原料に添加しないこともできる。   When producing a silicon carbide single crystal using the production facility 10 of the present invention, for example, first, the crucible 2 is filled with raw materials such as silicon and carbon, and the inside of the chamber 1 is evacuated, and then an inert gas such as argon is used. The inside of the chamber 1 is pressurized to atmospheric pressure or higher. When a crucible made of a carbon-containing material such as graphite is used as the crucible 2, carbon melts from the crucible 2, so that it is not necessary to add carbon to the raw material.

その後、加熱装置３によりるつぼ２を加熱し、原料を溶融させ、ケイ素と炭素を含む溶液４を形成する。次いで、種結晶保持部６を下降させ、炭化ケイ素単結晶である種結晶５を溶液４の表面と接触させる。この接触を維持することによって、種結晶５上に単結晶が成長し、炭化ケイ素単結晶を得ることができる。   Thereafter, the crucible 2 is heated by the heating device 3 to melt the raw material to form a solution 4 containing silicon and carbon. Next, the seed crystal holding unit 6 is lowered, and the seed crystal 5 that is a silicon carbide single crystal is brought into contact with the surface of the solution 4. By maintaining this contact, a single crystal grows on the seed crystal 5 and a silicon carbide single crystal can be obtained.

ここでケイ素及び炭素を含有する溶液４の温度は、溶融した状態を維持するのに必要な原料の融点以上の温度であり、例えば１８００℃以上の温度にすることができる。溶液４の温度が２３００℃を超えると、溶液からケイ素が激しく蒸発する問題が生ずるので、溶液の温度は一般に２３００℃以下とすることが好ましい。また安定な結晶成長を確保するためには、溶液４が、種結晶５との接触箇所に向かって１０〜４５℃／ｃｍの温度勾配を有するようにして、溶液４を加熱及び／又は種結晶５を冷却することが一般に好ましい。   Here, the temperature of the solution 4 containing silicon and carbon is equal to or higher than the melting point of the raw material necessary for maintaining the molten state, and can be set to, for example, 1800 ° C. or higher. When the temperature of the solution 4 exceeds 2300 ° C., there is a problem that silicon evaporates violently from the solution. Therefore, the temperature of the solution is generally preferably 2300 ° C. or less. In order to ensure stable crystal growth, the solution 4 is heated and / or seeded so that the solution 4 has a temperature gradient of 10 to 45 ° C./cm toward the contact point with the seed crystal 5. It is generally preferred to cool 5.

本発明の炭化ケイ素単結晶を製造するための本発明の製造設備の各部について以下で具体的に説明する。但し、これらの記載は単に説明のためのものであり、本発明はこれらの記載に限定されるものではない。   Each part of the production facility of the present invention for producing the silicon carbide single crystal of the present invention will be specifically described below. However, these descriptions are merely for explanation, and the present invention is not limited to these descriptions.

（るつぼ）
本発明の製造設備で使用されるるつぼ２は、ケイ素及び炭素を含有する溶液４を保持するのに必要な耐熱性及び強度を有する任意の材料で形成することができる。一般的にはこのるつぼは、溶液４に対して炭素を供給することが可能なグラファイト又は炭化ケイ素、特にグラファイトで形成されている。グラファイトは、加工が比較的容易である点で好ましい。また、炭化ケイ素は、比較的耐久性が大きい点で好ましい。 (Crucible)
The crucible 2 used in the production facility of the present invention can be formed of any material having heat resistance and strength necessary for holding the solution 4 containing silicon and carbon. In general, this crucible is made of graphite or silicon carbide, in particular graphite, capable of supplying carbon to the solution 4. Graphite is preferred because it is relatively easy to process. Silicon carbide is preferable in terms of relatively high durability.

るつぼの内側面の面粗度を小さくするためには、任意の研磨方法を用いることができ、例えばバフ研磨を用いることができる。尚、本発明の製造設備において使用されるるつぼ２では当然に、このるつぼ２の内側面のうちの、炭化ケイ素単結晶の製造の間に溶液の液面と接触する部分２ａだけでなく、るつぼ２の内表面全体が比較的小さい面粗度を有するようにすることもできる。   In order to reduce the surface roughness of the inner surface of the crucible, any polishing method can be used, for example, buffing can be used. Of course, in the crucible 2 used in the production facility of the present invention, not only the portion 2a of the inner surface of the crucible 2 that contacts the liquid level of the solution during the production of the silicon carbide single crystal, but also the crucible. The entire inner surface of 2 can also have a relatively small surface roughness.

本発明の製造設備で用いるるつぼ２では、図２に示す製造設備２０でのように、るつぼの内側面のうちの、炭化ケイ素単結晶の製造の間に溶液の液面と接触する部分が、るつぼの内側面のうちの他の部分とは異なる材料２ｂで形成されるようにしてもよい。   In the crucible 2 used in the production facility of the present invention, as in the production facility 20 shown in FIG. 2, the portion of the inner surface of the crucible that contacts the liquid surface of the solution during the production of the silicon carbide single crystal is You may make it form with the material 2b different from the other part of the inner surface of a crucible.

上述のように、本願発明の製造設備で用いるるつぼを形成するための材料としては、グラファイト及び炭化ケイ素を考慮することができ、従って例えばるつぼの内側面のうちの溶液の液面と接触する部分が炭化ケイ素で形成されるようにし、他の部分がグラファイトで形成されるようにしてもよい。尚、この場合には当然に、溶液の液面も接触する部分を、非炭素含有材料、例えばタングステン等の耐熱性金属で作ることもできる。   As described above, graphite and silicon carbide can be considered as the material for forming the crucible used in the manufacturing facility of the present invention, and therefore, for example, the portion of the inner surface of the crucible that contacts the liquid level of the solution. May be formed of silicon carbide, and other portions may be formed of graphite. In this case, as a matter of course, the portion that also contacts the liquid level of the solution can be made of a non-carbon-containing material, for example, a heat-resistant metal such as tungsten.

また本発明の製造設備で用いるるつぼ２では、図３に示す製造設備３０でのように、るつぼの内側面のうちの、炭化ケイ素単結晶の製造の間に溶液の液面と接触する部分が、るつぼの他の部分に対して脱着可能な部分、例えばるつぼ２の内側に挿入されている管状体２ｃによって提供にされていてもよい。   Moreover, in the crucible 2 used in the production facility of the present invention, as in the production facility 30 shown in FIG. 3, the portion of the inner surface of the crucible that contacts the liquid surface of the solution during the production of the silicon carbide single crystal. It may be provided by a part that is detachable with respect to other parts of the crucible, for example a tubular body 2c inserted inside the crucible 2.

この場合、この脱着可能な部分をるつぼ２に対して固定するために、固定手段によってチャンバー１の天井から吊すこと、るつぼ２に対してフランジ等の固定具で固定すること等ができる。尚、当然に、この脱着可能な部分は、るつぼ本体と同じ材料で作ることも、るつぼ本体とは異なる材料で作ることもできる。   In this case, in order to fix this detachable part to the crucible 2, it can be hung from the ceiling of the chamber 1 by a fixing means, or fixed to the crucible 2 with a fixing tool such as a flange. Of course, this detachable portion can be made of the same material as the crucible body or a material different from that of the crucible body.

（加熱装置）
本発明の製造設備１０では、るつぼ２の周囲には加熱装置３が配置されており、この加熱装置によって、るつぼ２内の原料を加熱して溶液の状態に維持する。この加熱装置としては任意の装置を用いることができるが、例えば加熱コイル等の電気加熱装置を用いることができる。 (Heating device)
In the production facility 10 of the present invention, a heating device 3 is disposed around the crucible 2, and the heating device heats the raw material in the crucible 2 and maintains it in a solution state. Although any device can be used as this heating device, for example, an electric heating device such as a heating coil can be used.

（種結晶保持部）
本発明の製造設備１０では、るつぼ２の上方に炭化ケイ素単結晶である種結晶５を保持するための種結晶保持部６が配置されている。ここでこの種結晶保持部６は、随意に回転させながら上方に引き上げることができるようにされており、それによってケイ素及び炭素を含有する溶液４から種結晶５上に炭化ケイ素単結晶を析出させるようにされている。尚、図示していないが、この種結晶保持部６は冷却装置に接続し、それによって種結晶５を所定の温度に冷却できるようにすることができる。 (Seed crystal holding part)
In the production facility 10 of the present invention, a seed crystal holding unit 6 for holding a seed crystal 5 that is a silicon carbide single crystal is disposed above the crucible 2. Here, the seed crystal holding unit 6 is configured to be able to be pulled upward while being arbitrarily rotated, thereby depositing a silicon carbide single crystal on the seed crystal 5 from the solution 4 containing silicon and carbon. Has been. Although not shown, the seed crystal holding unit 6 can be connected to a cooling device so that the seed crystal 5 can be cooled to a predetermined temperature.

図１に示すような製造設備を用いて４８時間にわたって炭化ケイ素単結晶を製造した。ここで、るつぼとしては、内側表面のうちの溶液の液面が接触する部分の面粗度がそれぞれ０．４μｍ、１．０μｍ、１．６μｍ、１．８μｍ、２．６μｍ及び３．４μｍであるグラファイト製るつぼを用いた。またこの製造の間の溶液１１の液面の温度は約１８００℃であった。   A silicon carbide single crystal was produced for 48 hours using a production facility as shown in FIG. Here, as the crucible, the surface roughness of the portion of the inner surface where the liquid level of the solution contacts is 0.4 μm, 1.0 μm, 1.6 μm, 1.8 μm, 2.6 μm and 3.4 μm, respectively. A graphite crucible was used. Further, the temperature of the liquid surface of the solution 11 during the production was about 1800 ° C.

得られた炭化ケイ素単結晶を切断し、光学顕微鏡によって評価を行った。また、るつぼを室温まで放冷し、るつぼ内に残留している材料を固化させ、この固化した材料をるつぼから取り出し、切断し、光学顕微鏡によって評価を行った。   The obtained silicon carbide single crystal was cut and evaluated by an optical microscope. Further, the crucible was allowed to cool to room temperature, the material remaining in the crucible was solidified, the solidified material was taken out from the crucible, cut, and evaluated by an optical microscope.

るつぼの面粗度が０．４μｍ、１．０μｍ及び１．６μｍのときには、得られた炭化ケイ素単結晶において多結晶の混入は観察されなかった。またこのときには、るつぼ内に残留している材料を固化させたものにおいても、多結晶の存在は観察されなかった。   When the surface roughness of the crucible was 0.4 μm, 1.0 μm and 1.6 μm, no inclusion of polycrystals was observed in the obtained silicon carbide single crystal. At this time, the presence of polycrystal was not observed even in the solidified material remaining in the crucible.

るつぼの面粗度が１．８μｍのときには、得られた炭化ケイ素単結晶において小さい多結晶の混入が観察された。またこのときには、るつぼ内に残留している材料を固化させたものにおいても、小さい多結晶の存在が観察された。   When the surface roughness of the crucible was 1.8 μm, small polycrystalline contamination was observed in the obtained silicon carbide single crystal. At this time, the presence of small polycrystals was also observed in the solidified material remaining in the crucible.

るつぼの面粗度が２．６μｍ及び３．４μｍのときには、得られた炭化ケイ素単結晶において大きい多結晶の混入が観察された。またこのときには、るつぼ内に残留している材料を固化させたものにおいても、大きい多結晶の存在が観察された。   When the surface roughness of the crucible was 2.6 μm and 3.4 μm, large polycrystalline contamination was observed in the obtained silicon carbide single crystal. At this time, the presence of large polycrystals was also observed in the solidified material remaining in the crucible.

炭化ケイ素単結晶を製造する本発明の製造設備を示す略図である。1 is a schematic diagram showing a production facility of the present invention for producing a silicon carbide single crystal. 炭化ケイ素単結晶を製造する本発明の他の製造設備を示す略図である。It is the schematic which shows the other manufacturing equipment of this invention which manufactures a silicon carbide single crystal. 炭化ケイ素単結晶を製造する本発明の更に他の製造設備を示す略図である。It is the schematic which shows the further another manufacturing equipment of this invention which manufactures a silicon carbide single crystal. 炭化ケイ素単結晶を製造する従来の製造設備を示す略図である。1 is a schematic view showing a conventional production facility for producing a silicon carbide single crystal.

符号の説明Explanation of symbols

１ チャンバー
２ るつぼ
３ 加熱装置
４ ケイ素及び炭素を含有する溶液
５ 種結晶
６ 種結晶保持部
１０，２０，３０ 本発明の炭化ケイ素製造設備
４０ 従来の炭化ケイ素製造設備 DESCRIPTION OF SYMBOLS 1 Chamber 2 Crucible 3 Heating apparatus 4 Solution containing silicon and carbon 5 Seed crystal 6 Seed crystal holding part 10, 20, 30 Silicon carbide production equipment of the present invention 40 Conventional silicon carbide production equipment

Claims (4)

ケイ素及び炭素を含有する溶液を保持するるつぼ、前記るつぼを加熱する加熱装置及び種結晶を保持する種結晶保持部を有する、溶液法による炭化ケイ素単結晶の製造のための製造設備であって、
前記るつぼの内側面のうちの、少なくとも炭化ケイ素単結晶の製造の間に前記溶液の液面と接触する部分が、２．０μｍ以下の面粗度Ｒａを有する、溶液法による炭化ケイ素単結晶の製造のための製造設備。 A production facility for producing a silicon carbide single crystal by a solution method, comprising a crucible for holding a solution containing silicon and carbon, a heating device for heating the crucible, and a seed crystal holding part for holding a seed crystal,
Of the inner surface of the crucible, at least a portion that contacts the liquid surface of the solution during the production of the silicon carbide single crystal has a surface roughness Ra of 2.0 μm or less. Manufacturing equipment for manufacturing. 前記るつぼの内側面のうちの、少なくとも炭化ケイ素単結晶の製造の間に前記溶液の液面と接触する部分が、前記るつぼの内側面のうちの他の部分とは異なる材料で形成されている、請求項１に記載の製造設備。   Of the inner surface of the crucible, at least a portion that contacts the liquid surface of the solution during the production of the silicon carbide single crystal is formed of a material different from the other portions of the inner surface of the crucible. The manufacturing equipment according to claim 1. 前記るつぼの内側面のうちの、少なくとも炭化ケイ素単結晶の製造の間に前記溶液の液面と接触する部分が、前記るつぼの他の部分に対して脱着可能である、請求項１又は２に記載の製造設備。   The inner surface of the crucible, at least a portion that contacts the liquid surface of the solution during the production of the silicon carbide single crystal is detachable from other portions of the crucible. The manufacturing equipment described. 前記るつぼの内側面のうちの、少なくとも炭化ケイ素単結晶の製造の間に前記溶液の液面と接触する部分が、前記るつぼの他の部分に対して脱着可能な炭化ケイ素製の管状体であり、且つ前記るつぼの内表面の他の部分がグラファイト製である、請求項１に記載の製造設備。   Of the inner surface of the crucible, at least a portion in contact with the liquid level of the solution during the production of the silicon carbide single crystal is a tubular body made of silicon carbide that can be detached from the other portion of the crucible. And the other part of the inner surface of the crucible is made of graphite.
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