JP2001226198A - Method and device for producing silicon carbide single crystal - Google Patents
Method and device for producing silicon carbide single crystalInfo
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- JP2001226198A JP2001226198A JP2000041426A JP2000041426A JP2001226198A JP 2001226198 A JP2001226198 A JP 2001226198A JP 2000041426 A JP2000041426 A JP 2000041426A JP 2000041426 A JP2000041426 A JP 2000041426A JP 2001226198 A JP2001226198 A JP 2001226198A
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- silicon carbide
- single crystal
- raw material
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- silicon
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- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、半導体や発光ダイ
オードなどの素材に利用することができる炭化珪素（以
下、ＳｉＣという）単結晶の製造方法及びその製造装置
に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a silicon carbide (hereinafter referred to as SiC) single crystal which can be used for a material such as a semiconductor or a light emitting diode, and a production apparatus therefor.
【０００２】[0002]
【従来の技術】従来、ＳｉＣ単結晶を成長させる方法と
して、昇華再結晶法が広く用いられている。この昇華再
結晶法は、黒鉛製るつぼ内に配置した黒鉛台座に種結晶
を接合すると共に、るつぼ底部に配したＳｉＣ原料を加
熱昇華させ、その昇華ガスを種結晶に供給することによ
って種結晶上にＳｉＣ単結晶を成長させるものである。2. Description of the Related Art Conventionally, a sublimation recrystallization method has been widely used as a method for growing a SiC single crystal. In this sublimation recrystallization method, a seed crystal is joined to a graphite pedestal arranged in a graphite crucible, and the SiC raw material arranged at the bottom of the crucible is heated and sublimated, and the sublimation gas is supplied to the seed crystal to thereby form a seed crystal. For growing a SiC single crystal.
【０００３】このような昇華再結晶法を用いたＳｉＣ単
結晶の製造において、るつぼ構造や原料供給方法等を工
夫することによりＳｉＣ単結晶の成長面の温度を安定化
させる方法が種々提案されている。これらの方法により
高い確率で高品質、長尺のＳｉＣ単結晶を得ることが可
能である。In the production of a SiC single crystal using such a sublimation recrystallization method, various methods have been proposed for stabilizing the temperature of the growth surface of the SiC single crystal by devising a crucible structure, a raw material supply method, and the like. I have. By these methods, it is possible to obtain a high-quality, long SiC single crystal with a high probability.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、るつぼ
内部に配置されたＳｉＣ原料の昇華の状態が、ＳｉＣ単
結晶の成長過程で微妙に異なってくるために、得られた
ＳｉＣ単結晶がしばしば不良になるという問題がある。However, since the state of sublimation of the SiC raw material disposed inside the crucible is slightly different during the growth process of the SiC single crystal, the obtained SiC single crystal often becomes defective. Problem.
【０００５】本発明は上記点に鑑みて、ＳｉＣ原料の昇
華の状態が一定にできるようにし、確実に高品質、長尺
のＳｉＣ単結晶が製造できるようにすることを目的とす
る。SUMMARY OF THE INVENTION In view of the foregoing, it is an object of the present invention to make the state of sublimation of a SiC raw material constant and to surely produce a high-quality and long SiC single crystal.
【０００６】[0006]
【課題を解決するための手段】上記目的を達成すべく、
本発明者らは以下の検討を行なった。In order to achieve the above object,
The present inventors have conducted the following studies.
【０００７】上記問題は、ＳｉＣ原料の昇華の状態が経
時変化等によって不安定になるために、ＳｉＣガスの過
飽和度が不安定になり、それが原因となって発生すると
考えられる。このため、ＳｉＣ原料の昇華の状態を検出
できるようにすれば、上記問題を解決することができる
と言える。[0007] The above problem is considered to occur because the sublimation state of the SiC raw material becomes unstable due to aging or the like, so that the degree of supersaturation of the SiC gas becomes unstable. For this reason, it can be said that the above problem can be solved if the sublimation state of the SiC raw material can be detected.
【０００８】そこで、本発明者らは、ＳｉＣ原料の昇華
の状態を検出する手段として、Ｘ線を用いることを見出
した。Therefore, the present inventors have found that X-rays are used as means for detecting the state of sublimation of the SiC raw material.
【０００９】ＳｉＣ原料にＸ線を照射すると、ＳｉＣ原
料の昇華が進行した箇所の方が昇華していない箇所より
もＸ線が透過し易い。これは、昇華が進行した箇所では
Ｓｉ成分が抜けたために、Ｘ線の吸収率が変化するから
である。なお、昇華が進行した箇所を組成分析した結
果、Ｃ成分はほとんど抜けていなかったことから、上記
現象はＳｉ成分の抜けが原因であると説明できる。When the SiC raw material is irradiated with X-rays, the X-rays are more likely to pass through the sublimated portion of the SiC raw material than in the non-sublimated portion. This is because the Si component escapes at the place where sublimation has progressed, so that the X-ray absorption rate changes. In addition, as a result of analyzing the composition of the portion where sublimation has progressed, the C component was hardly removed, and thus the above phenomenon can be explained as being caused by the loss of the Si component.
【００１０】Ｘ線を物質に照射して透過させる時、入射
Ｘ線強度と透過Ｘ線強度との間には、次のような関係式
が成り立つ。When irradiating a substance with X-rays for transmission, the following relational expression holds between the incident X-ray intensity and the transmitted X-ray intensity.
【００１１】[0011]
【数１】 但し、Ｉxは透過Ｘ線強度、Ｉ0は入射Ｘ線強度、μは線
吸収係数、ρは密度、ｘはＸ線が物質を透過した距離を
表している。(Equation 1) Here, I x is the transmitted X-ray intensity, I 0 is the incident X-ray intensity, μ is the line absorption coefficient, ρ is the density, and x is the distance that the X-ray has passed through the substance.
【００１２】なお、μ／ρは質量吸収係数と呼ばれ、物
質固有の値であり、次の関係式を満たす。Note that μ / ρ is called a mass absorption coefficient and is a value inherent to a substance, and satisfies the following relational expression.
【００１３】[0013]
【数２】μ／ρ＝ω1（μ／ρ）1＋ω2（μ／ρ）2＋…Μ / ρ = ω 1 (μ / ρ) 1 + ω 2 (μ / ρ) 2 + ...
【００１４】[0014]
【数３】μ／ρ＝ｋλ3Ｚ3 但し、ｎ（ｎ＝１、２…）を成分の種類とすると、ωn
は成分ｎの重量比、（μ／ρ）nは成分ｎの重量吸収係
数、ｋは定数、Ｚは原子番号、λはＸ線の波長を表して
いる。Μ / ρ = kλ 3 Z 3 where n (n = 1, 2,...) Is the type of component, and ω n
Is the weight ratio of component n, (μ / ρ) n is the weight absorption coefficient of component n, k is a constant, Z is the atomic number, and λ is the wavelength of X-rays.
【００１５】これらの関係式、及び原子番号がＣ＜Ｓｉ
であることから、Ｘ線の透過量がＳｉ＜ＳｉＣ＜Ｃとな
ることが判る。従って、Ｘ線を用いることにより、Ｓｉ
Ｃ原料の昇華状態をモニターすることができる。These relational expressions and the atomic number C <Si
Therefore, it can be seen that the transmission amount of X-rays satisfies Si <SiC <C. Therefore, by using X-rays, Si
The sublimation state of the C raw material can be monitored.
【００１６】そこで、上記目的を達成するため、請求項
１に記載の発明では、容器（１）内に、炭化珪素原料
（２）と種結晶となる炭化珪素単結晶基板（３）を配置
し、原料を加熱昇華させて炭化珪素単結晶基板上に炭化
珪素単結晶（４）を成長させる炭化珪素単結晶の製造過
程において、容器外部に備えたＸ線発生源（６）にてＸ
線（８）を炭化珪素原料に照射し、容器外部に備えたＸ
線検出器（７）により容器および炭化珪素原料を透過し
たＸ線を検出し、そのＸ線の透過量から炭化珪素原料の
減少量をモニターし、該減少量が一定となるように容器
内の温度を制御することを特徴としている。Therefore, in order to achieve the above object, according to the first aspect of the present invention, a silicon carbide raw material (2) and a silicon carbide single crystal substrate (3) serving as a seed crystal are arranged in a container (1). In the process of producing a silicon carbide single crystal in which a raw material is heated and sublimated to grow a silicon carbide single crystal (4) on a silicon carbide single crystal substrate, X-rays are generated by an X-ray source (6) provided outside the container.
The silicon carbide raw material is irradiated with the wire (8), and X
X-rays transmitted through the container and the silicon carbide raw material are detected by the X-ray detector (7), and the amount of reduction of the silicon carbide raw material is monitored based on the amount of transmitted X-rays. It is characterized by controlling the temperature.
【００１７】このように、Ｘ線を用いて炭化珪素原料の
昇華状態をモニターし、炭化珪素原料の減少量が一定と
なるように容器内の温度を制御することにより、容器内
の珪素／炭素比を安定化させることができ、確実に高品
質、長尺な炭化珪素単結晶が得られるようにできる。As described above, the sublimation state of the silicon carbide raw material is monitored using X-rays, and the temperature in the container is controlled so that the amount of reduction of the silicon carbide raw material becomes constant, whereby the silicon / carbon in the container is reduced. The ratio can be stabilized, and a high-quality, long silicon carbide single crystal can be reliably obtained.
【００１８】請求項２に記載の発明においては、Ｘ線を
炭化珪素原料の上部に照射し、そのＸ線の透過量が一定
となるようにしつつ炭化珪素単結晶を成長させることを
特徴としている。According to a second aspect of the present invention, a silicon carbide single crystal is grown while irradiating an X-ray to an upper portion of a silicon carbide raw material so as to make the amount of transmission of the X-ray constant. .
【００１９】このように、Ｘ線の透過量が一定となるよ
うにすれば、容器内の珪素／炭素比を定常化することが
でき、請求項１と同様の効果が得られる。As described above, if the amount of transmitted X-rays is made constant, the silicon / carbon ratio in the container can be stabilized, and the same effect as in claim 1 can be obtained.
【００２０】例えば、請求項５に示すように、容器内の
温度の制御を行なう制御装置（１０）による温度制御に
よって、Ｘ線の透過量を一定に制御することができる。
なお、温度制御としては、請求項６に示すように容器内
の温度分布を変化させる制御がある。For example, the amount of X-rays transmitted can be controlled to be constant by temperature control by a control device (10) for controlling the temperature in the container.
As the temperature control, there is control for changing the temperature distribution in the container as described in claim 6.
【００２１】請求項３に記載の発明においては、炭化珪
素原料とは別に、容器内に少なくとも珪素を含む材料
（１１）を配置すると共に、該珪素を含む材料と炭化珪
素原料との間を、珪素ガスを通過させることができる仕
切板（１０）で仕切り、珪素を含む材料から発生させた
珪素ガスを仕切板を通じて炭化珪素単結晶基板に供給さ
せるようにし、炭化珪素原料の上部にＸ線を照射し、そ
のＸ線の透過量が一定となるようにしつつ炭化珪素単結
晶を成長させることを特徴としている。According to the third aspect of the present invention, a material (11) containing at least silicon is disposed in a container separately from the silicon carbide raw material, and the space between the silicon-containing material and the silicon carbide raw material is Partitioning is performed by a partition plate (10) through which silicon gas can pass, and a silicon gas generated from a material containing silicon is supplied to the silicon carbide single crystal substrate through the partition plate. Irradiation is performed so that a silicon carbide single crystal is grown while the amount of transmitted X-rays is constant.
【００２２】このように炭化珪素原料とは別に珪素を含
む材料を配置し、Ｘ線の透過量が一定となるようにさせ
れば、珪素を含む材料から珪素が供給され、容器内の珪
素／炭素比を定常化させることができる。As described above, if a material containing silicon is arranged separately from the silicon carbide raw material so that the amount of transmitted X-rays is constant, silicon is supplied from the material containing silicon and silicon / silicon in the container is removed. The carbon ratio can be stabilized.
【００２３】請求項４に記載の発明においては、炭化珪
素原料とは別に、容器外に珪素を含む材料の供給源とな
る珪素導入部（１２）を備え、容器に形成された開口部
を通じて珪素導入部から珪素を含む材料の導入を行い、
Ｘ線の透過量が一定となるように珪素を含む材料の導入
量を制御することを特徴としている。According to the fourth aspect of the present invention, a silicon introducing portion (12) is provided outside the container as a supply source of a material containing silicon, separately from the silicon carbide raw material, and silicon is introduced through an opening formed in the container. Introduce a material containing silicon from the introduction section,
It is characterized in that the introduction amount of the material containing silicon is controlled so that the transmission amount of X-rays becomes constant.
【００２４】このように容器外に珪素導入部を備え、こ
の珪素導入部によって珪素を含む材料を供給するように
すれば、導入時間を適宜調整でき、例えば導入時間を長
くすることによって長期に渡って容器内を適度な炭化珪
素原料の昇華ガスで満たすことができる。If the silicon introducing section is provided outside the container and the material containing silicon is supplied by the silicon introducing section as described above, the introduction time can be appropriately adjusted. For example, by extending the introduction time, the introduction time can be extended. Thus, the inside of the container can be filled with a sublimation gas of an appropriate silicon carbide raw material.
【００２５】なお、請求項７に示すように、容器の加熱
にらせん形状高周波誘導コイル（１３）を用いる場合に
は、コイルを挟んで一直線にＸ線発生源とＸ線検出器を
配置し、Ｘ線発生源からのＸ線が、コイルを避けるよう
に照射され、容器及び炭化珪素原料を透過してＸ線検出
器に到達するようにすればよい。When the spiral high-frequency induction coil (13) is used for heating the container, the X-ray source and the X-ray detector are arranged in a straight line with the coil interposed therebetween. X-rays from the X-ray generation source may be irradiated so as to avoid the coil, pass through the container and the silicon carbide raw material, and reach the X-ray detector.
【００２６】この場合、請求項８に示すように、コイル
のらせんに沿って、Ｘ線発生源とＸ線検出器をらせん駆
動させるようにすれば、容器に対して相対的にＸ線発生
源とＸ線検出器とを上下に移動させることができるた
め、原料部全体の昇華状態を確認可能とすることができ
る。In this case, if the X-ray source and the X-ray detector are spirally driven along the spiral of the coil, the X-ray source can be relatively moved with respect to the container. And the X-ray detector can be moved up and down, so that the sublimation state of the entire raw material section can be confirmed.
【００２７】なお、請求項９乃至請求項１６に記載の発
明は、請求項１乃至８に記載の炭化珪素単結晶の製造方
法の実施に使用する製造装置の発明である。The inventions described in claims 9 to 16 are inventions of a manufacturing apparatus used for carrying out the method for manufacturing a silicon carbide single crystal according to claims 1 to 8.
【００２８】なお、上記各手段の括弧内の符号は、後述
する実施形態に記載の具体的手段との対応関係を示すも
のである。The reference numerals in the parentheses of the above means indicate the correspondence with specific means described in the embodiments described later.
【００２９】[0029]
【発明の実施の形態】（第１実施形態）図１に本発明の
第１実施形態で用いる結晶成長装置を示す。この結晶成
長装置の容器として用いられる黒鉛製るつぼ１は、黒鉛
製るつぼ１の底部に備えられたＳｉＣ原料粉末（ＳｉＣ
原料）２を熱処理によって昇華させ、種結晶であるＳｉ
Ｃ単結晶基板３上にＳｉＣ単結晶４を結晶成長させるも
のである。DESCRIPTION OF THE PREFERRED EMBODIMENTS (First Embodiment) FIG. 1 shows a crystal growth apparatus used in a first embodiment of the present invention. The graphite crucible 1 used as a container of the crystal growth apparatus is made of SiC raw material powder (SiC crucible) provided at the bottom of the graphite crucible 1.
The raw material 2 is sublimated by heat treatment, and the seed crystal Si
This is for growing a SiC single crystal 4 on a C single crystal substrate 3.
【００３０】この黒鉛製るつぼ１は、上面が開口してい
る略円筒状のるつぼ本体１ａと、るつぼ本体１ａの開口
部を塞ぐ蓋材１ｂとを備えて構成されている。この黒鉛
製るつぼ１を構成する蓋材１ｂを台座として、台座上に
ＳｉＣ単結晶基板３が接着剤５を介して接合されてい
る。The graphite crucible 1 includes a substantially cylindrical crucible body 1a having an open upper surface, and a lid 1b for closing the opening of the crucible body 1a. The lid 1b constituting the graphite crucible 1 is used as a pedestal, and the SiC single crystal substrate 3 is bonded on the pedestal via an adhesive 5.
【００３１】一方、黒鉛製るつぼ１の外部には、黒鉛製
るつぼ１内に向かってＸ線８を照射するＸ線発生源６が
配置されていると共に、黒鉛製るつぼ１内を透過してき
たＸ線８を検出するためのＸ線検出器７が配置されてい
る。On the other hand, outside the graphite crucible 1, an X-ray source 6 for irradiating the inside of the graphite crucible 1 with X-rays 8 is arranged, and X-rays transmitted through the graphite crucible 1 are arranged. An X-ray detector 7 for detecting a line 8 is arranged.
【００３２】また、Ｘ線検出器７には、制御装置８が接
続されており、Ｘ線検出器７によるＸ線８の検出結果が
制御装置９にフィードバックされ、制御装置９によって
黒鉛製るつぼ１内の温度を制御できるように構成されて
いる。A control device 8 is connected to the X-ray detector 7, and the result of detection of the X-rays 8 by the X-ray detector 7 is fed back to the control device 9, and the graphite crucible 1 is controlled by the control device 9. It is configured to be able to control the temperature inside.
【００３３】なお、図示しないが、黒鉛製るつぼ１は、
アルゴンガスが導入できる真空容器の中で加熱装置によ
り、加熱できるようになっており、例えば、この加熱装
置のパワーを調節することによって種結晶であるＳｉＣ
単結晶基板３の温度がＳｉＣ原料粉末２の温度よりも１
００℃程度低温に保たれるようにすることができる。Although not shown, the graphite crucible 1 is
Heating can be performed by a heating device in a vacuum vessel into which argon gas can be introduced. For example, by adjusting the power of the heating device, the seed crystal SiC can be heated.
The temperature of the single crystal substrate 3 is lower than the temperature of the SiC raw material powder 1 by one.
It can be kept at a low temperature of about 00 ° C.
【００３４】このように構成された結晶成長装置を用い
たＳｉＣ単結晶の製造工程について説明する。The manufacturing process of the SiC single crystal using the crystal growth apparatus having such a configuration will be described.
【００３５】まず、ＳｉＣ原料粉末２の温度を２０００
〜２５００℃に加熱する。そして、加熱装置の調節等に
より、ＳｉＣ単結晶基板３の温度がＳｉＣ原料粉末２の
温度よりも低くなるように、黒鉛製るつぼ１内に温度勾
配を設ける。次に、黒鉛製るつぼ１内の圧力を１３．３
Ｐａ〜２６．７ｋＰａとして、昇華法成長を開始する
と、ＳｉＣ原料粉末２が昇華して昇華ガスとなり、Ｓｉ
Ｃ単結晶３に到達し、ＳｉＣ原料粉末２側よりも相対的
に低温となるＳｉＣ単結晶基板３の表面上にＳｉＣ単結
晶４が成長する。First, the temperature of the SiC raw material powder 2 was set to 2000
Heat to ~ 2500C. Then, a temperature gradient is provided in the graphite crucible 1 such that the temperature of the SiC single crystal substrate 3 is lower than the temperature of the SiC raw material powder 2 by adjusting a heating device or the like. Next, the pressure in the graphite crucible 1 was increased to 13.3.
When the sublimation growth is started at a pressure of Pa to 26.7 kPa, the SiC raw material powder 2 sublimates to become a sublimation gas,
The SiC single crystal 4 grows on the surface of the SiC single crystal substrate 3 which reaches the C single crystal 3 and has a relatively lower temperature than the SiC raw material powder 2 side.
【００３６】その際、ＳｉＣ原料粉末２にるつぼ本体１
の外部からＸ線８をＸ線発生源６を用いて照射し、Ｓｉ
Ｃ原料粉末２とるつぼ本体１を透過したＸ線８をＸ線検
出器７で検出する。そうすることで、ＳｉＣ原料粉末２
の珪素成分は昇華により少なくなるが、炭素成分はその
まま残存することから、成長中にＸ線８の透過量が経時
変化するので、ＳｉＣ原料粉末２の減少量を確認するこ
とが可能となる。なお、Ｘ線検出器７に表示器を備え、
Ｘ線８の透過量若しくは減少量を表示器で表示すれば、
ＳｉＣ原料粉末２の昇華状態を把握することも可能であ
る。例えば、透過量若しくは減少量の検出値を数値化し
てもよく、ＳｉＣ原料粉末２の状態を画像で表すことに
よって昇華状態がイメージしやすくなるようにしてもよ
い。At this time, the crucible body 1 is added to the SiC raw material powder 2.
X-rays 8 are radiated from the outside using the X-ray source 6 and Si
An X-ray 8 transmitted through the C raw material powder 2 and the crucible body 1 is detected by an X-ray detector 7. By doing so, SiC raw material powder 2
Although the silicon component becomes smaller due to sublimation, the carbon component remains as it is, so that the amount of transmission of the X-rays 8 changes over time during growth, so that the amount of decrease in the SiC raw material powder 2 can be confirmed. The X-ray detector 7 has a display,
If the amount of transmission or reduction of X-rays 8 is displayed on a display,
It is also possible to grasp the sublimation state of the SiC raw material powder 2. For example, the detection value of the transmission amount or the reduction amount may be digitized, and the state of the SiC raw material powder 2 may be represented by an image so that the sublimation state may be easily imaged.
【００３７】そして、Ｘ線検出器７からの検出結果を制
御装置９にフィードバックし、制御装置９にて黒鉛製る
つぼ１内の温度を制御することによって、ＳｉＣ原料粉
末２の減少量が一定となるようにさせつつ、ＳｉＣ単結
晶４を結晶成長させる。例えば、加熱装置のパワーを調
整することにより黒鉛製るつぼ１内の温度分布を調整す
ることができる。Then, the detection result from the X-ray detector 7 is fed back to the control device 9 and the temperature in the graphite crucible 1 is controlled by the control device 9 so that the reduction amount of the SiC raw material powder 2 is kept constant. While growing, the SiC single crystal 4 is grown. For example, the temperature distribution in the graphite crucible 1 can be adjusted by adjusting the power of the heating device.
【００３８】このようにすることで、るつぼ１内の珪素
／炭素比を安定化させることができ、ＳｉＣ単結晶４を
確実に高品質、長尺に形成することができる。By doing so, the silicon / carbon ratio in the crucible 1 can be stabilized, and the SiC single crystal 4 can be reliably formed with high quality and long length.
【００３９】（第２実施形態）図２に、本発明の第２実
施形態で用いる結晶成長装置を示す。以下、図２に基づ
いて本実施形態におけるＳｉＣ単結晶の製造について説
明するが、装置構成及びＳｉＣ単結晶の製造工程につい
ては第１実施形態とほぼ同様であるため、異なる点につ
いてのみ説明する。(Second Embodiment) FIG. 2 shows a crystal growth apparatus used in a second embodiment of the present invention. Hereinafter, the manufacturing of the SiC single crystal in the present embodiment will be described with reference to FIG. 2. However, since the device configuration and the manufacturing process of the SiC single crystal are almost the same as those in the first embodiment, only different points will be described.
【００４０】本実施形態では、黒鉛製るつぼ１内に配置
されたＳｉＣ原料粉末２の上部にのみＸ線８を照射し、
制御装置９によって透過したＸ線８の透過量が一定とな
るように黒鉛製るつぼ１内の温度を制御しながらＳｉＣ
単結晶４を成長させた。このようにすれば、黒鉛製るつ
ぼ１内の珪素／炭素比を定常化させることができ、Ｓｉ
Ｃ単結晶４を確実に高品質、長尺に形成することができ
る。In this embodiment, only the upper part of the SiC raw material powder 2 placed in the graphite crucible 1 is irradiated with X-rays 8,
The SiC while controlling the temperature in the graphite crucible 1 so that the transmission amount of the X-rays 8 transmitted by the control device 9 becomes constant.
A single crystal 4 was grown. By doing so, the silicon / carbon ratio in the graphite crucible 1 can be stabilized, and Si
The C single crystal 4 can be reliably formed in high quality and long.
【００４１】（第３実施形態）図３に、本発明の第３実
施形態で用いる結晶成長装置を示す。以下、図３に基づ
いて本実施形態におけるＳｉＣ単結晶の製造について説
明するが、装置構成及びＳｉＣ単結晶の製造工程につい
ては第１実施形態とほぼ同様であるため、異なる点につ
いてのみ説明する。(Third Embodiment) FIG. 3 shows a crystal growth apparatus used in a third embodiment of the present invention. Hereinafter, the manufacture of the SiC single crystal in the present embodiment will be described with reference to FIG. 3. However, since the device configuration and the manufacturing process of the SiC single crystal are almost the same as those in the first embodiment, only different points will be described.
【００４２】るつぼ本体１ａの底部には、仕切板１０が
配置されており、この仕切板１０によって、るつぼ本体
１ａは、ＳｉＣ単結晶基板３が配置されている側のスペ
ースと配置されていない側のスペースに仕切られてい
る。そして、ＳｉＣ単結晶基板３が配置されていない側
のスペースには珪素を含む材料としての珪素粉末１１が
収容され、仕切板１０で珪素粉末１１が囲まれた状態と
なっている。また、ＳｉＣ単結晶基板３が配置されてい
る側には仕切板１０を覆うようにＳｉＣ原料粉末２が充
填されている。なお、珪素粉末１１とＳｉＣ原料粉末２
は仕切板１０によって混合しないようになっている。具
体的には、仕切板１０はポーラスカーボン（多孔質黒
鉛）で構成されており、珪素粉末１１の蒸発ガスが通過
できるようになっている。At the bottom of the crucible main body 1a, a partition plate 10 is disposed. With this partition plate 10, the crucible main body 1a is separated from the space where the SiC single crystal substrate 3 is disposed and the side where the SiC single crystal substrate 3 is not disposed. Is divided into spaces. The space on the side where the SiC single crystal substrate 3 is not disposed contains silicon powder 11 as a material containing silicon, and the partition plate 10 surrounds the silicon powder 11. The side on which the SiC single crystal substrate 3 is disposed is filled with the SiC raw material powder 2 so as to cover the partition plate 10. The silicon powder 11 and the SiC raw material powder 2
Are not mixed by the partition plate 10. Specifically, the partition plate 10 is made of porous carbon (porous graphite) so that the vaporized gas of the silicon powder 11 can pass through.
【００４３】このような構成においても、ＳｉＣ原料粉
末２にＸ線８を照射し、制御装置９によって透過したＸ
線８の透過量が一定となるように黒鉛製るつぼ１内の温
度を制御することで、ＳｉＣ原料粉末２及び珪素粉末１
１からの昇華状態を制御し、黒鉛製るつぼ１内の珪素／
炭素比を定常化させることができる。これにより、Ｓｉ
Ｃ単結晶４を確実に高品質、長尺に形成することができ
る。Even in such a configuration, the SiC raw material powder 2 is irradiated with X-rays 8,
By controlling the temperature in the graphite crucible 1 so that the transmission amount of the wire 8 is constant, the SiC raw material powder 2 and the silicon powder 1 are controlled.
1 to control the state of sublimation from silicon,
The carbon ratio can be stabilized. Thereby, Si
The C single crystal 4 can be reliably formed in high quality and long.
【００４４】（第４実施形態）図４に、本発明の第４実
施形態で用いる結晶成長装置を示す。以下、図４に基づ
いて本実施形態におけるＳｉＣ単結晶の製造について説
明するが、装置構成及びＳｉＣ単結晶の製造工程につい
ては第１実施形態とほぼ同様であるため、異なる点につ
いてのみ説明する。(Fourth Embodiment) FIG. 4 shows a crystal growth apparatus used in a fourth embodiment of the present invention. Hereinafter, the production of the SiC single crystal in the present embodiment will be described with reference to FIG. 4. However, since the device configuration and the production process of the SiC single crystal are almost the same as those in the first embodiment, only different points will be described.
【００４５】るつぼ本体１ａの底部には開口部を設けて
あり、この開口部を通じて珪素導入部１２から黒鉛製る
つぼ１内に珪素を含む材料が導入できるようになってい
る。この珪素を含む材料としては、例えば常温で珪素系
化合物ガスや珪素系化合物の液体を用いることができ
る。また、珪素導入部１２は制御装置９に接続されてお
り、制御装置９によって珪素導入部１２による珪素を含
む材料の導入量を制御できるように構成されている。An opening is provided at the bottom of the crucible main body 1a, and a material containing silicon can be introduced into the graphite crucible 1 from the silicon introduction portion 12 through the opening. As the material containing silicon, for example, a silicon-based compound gas or a liquid of a silicon-based compound at room temperature can be used. Further, the silicon introduction unit 12 is connected to the control device 9, and is configured such that the control device 9 can control the introduction amount of the material containing silicon by the silicon introduction unit 12.
【００４６】このような構成により、昇華によりＳｉＣ
原料粉末２から抜けたＳｉ成分を、珪素導入部１２によ
って補うことができる。また、このように珪素導入部１
２を黒鉛製るつぼ１の外部に設けることによって、珪素
を含む材料の導入時間を適宜調整でき、例えば導入時間
を長くすることによって長期に渡って黒鉛製るつぼ１内
を適度なＳｉＣ原料の昇華ガスで満たすことができる。With such a structure, SiC is formed by sublimation.
The Si component that has escaped from the raw material powder 2 can be supplemented by the silicon introduction part 12. Also, as described above, the silicon introduction part 1
2 is provided outside the graphite crucible 1 so that the introduction time of the material containing silicon can be appropriately adjusted. For example, by increasing the introduction time, the sublimation gas of a suitable SiC raw material can be maintained in the graphite crucible 1 for a long time. Can be filled with
【００４７】このため、ＳｉＣ原料粉末２にＸ線８を照
射し、制御装置９によって透過したＸ線８の透過量が一
定となるように珪素導入部１２による珪素を含む材料の
導入量を制御することにより、るつぼ１内の珪素／炭素
比を定常化させることができる。これにより、高品質か
つ長尺のＳｉＣ単結晶４を成長することができる。For this reason, the SiC raw material powder 2 is irradiated with X-rays 8, and the control unit 9 controls the introduction amount of the material containing silicon by the silicon introduction unit 12 so that the transmission amount of the X-rays 8 is constant. By doing so, the silicon / carbon ratio in the crucible 1 can be stabilized. Thereby, a high quality and long SiC single crystal 4 can be grown.
【００４８】（他の実施形態）上記実施形態で説明した
ように、黒鉛製るつぼ１は加熱装置で加熱されるが、例
えば、図５に示すように、らせん形状高周波誘導コイル
１３を加熱装置として用いることができる。この場合、
黒鉛製るつぼ１は、コイル１３に囲まれるように配置さ
れるため、コイル１３によってＸ線８が遮られる。従っ
て、このような場合には、コイル１３を挟んで一直線に
Ｘ線発生源６とＸ線検出器７とを配置し、Ｘ線８がコイ
ル１３を避けて照射されると共に黒鉛製るつぼ１及びＳ
ｉＣ原料粉末２を透過してＸ線検出器７に到達するよう
にすればよい。また、Ｘ線発生源６とＸ線検出器７をら
せん駆動する機構を備えれば、Ｘ線発生源６とＸ線検出
器７を黒鉛製るつぼ１に対して相対的に上下に変位させ
ることも可能である。このようならせん駆動機構を設け
れば、Ｘ線８を照射できる範囲を超えてＳｉＣ原料粉末
２が多量に配置されていても、ＳｉＣ原料粉末２の全体
の減少量を検出することができる。また、ＳｉＣ原料粉
末２の量の変化と共に、Ｘ線発生源６とＸ線検出器７を
上下に変位させることもできる。(Other Embodiments) As described in the above embodiment, the graphite crucible 1 is heated by a heating device. For example, as shown in FIG. 5, a spiral high-frequency induction coil 13 is used as a heating device. Can be used. in this case,
Since the graphite crucible 1 is arranged so as to be surrounded by the coil 13, the X-ray 8 is blocked by the coil 13. Therefore, in such a case, the X-ray source 6 and the X-ray detector 7 are arranged in a straight line with the coil 13 interposed therebetween, so that the X-ray 8 is irradiated while avoiding the coil 13 and the graphite crucible 1 and S
What is necessary is just to make it penetrate the iC raw material powder 2 and reach the X-ray detector 7. If a mechanism for spirally driving the X-ray source 6 and the X-ray detector 7 is provided, the X-ray source 6 and the X-ray detector 7 can be displaced up and down relatively to the graphite crucible 1. Is also possible. If such a spiral drive mechanism is provided, even if a large amount of the SiC raw material powder 2 is arranged beyond the range in which the X-rays 8 can be irradiated, it is possible to detect the total reduction amount of the SiC raw material powder 2. Further, the X-ray source 6 and the X-ray detector 7 can be displaced up and down as the amount of the SiC raw material powder 2 changes.
【００４９】また、第３実施形態で示した珪素粉末１１
は珪素基板などの固体の珪素でもよいし、窒化珪素、珪
素系化合物を用いることもできる。Further, the silicon powder 11 shown in the third embodiment
May be solid silicon such as a silicon substrate, or may be silicon nitride or a silicon-based compound.
【図１】本発明の第１実施形態における結晶成長装置の
構成を示す図である。FIG. 1 is a diagram showing a configuration of a crystal growth apparatus according to a first embodiment of the present invention.
【図２】本発明の第２実施形態における結晶成長装置の
構成を示す図である。FIG. 2 is a diagram illustrating a configuration of a crystal growth apparatus according to a second embodiment of the present invention.
【図３】本発明の第３実施形態における結晶成長装置の
構成を示す図である。FIG. 3 is a diagram illustrating a configuration of a crystal growth apparatus according to a third embodiment of the present invention.
【図４】本発明の第４実施形態における結晶成長装置の
構成を示す図である。FIG. 4 is a diagram showing a configuration of a crystal growth apparatus according to a fourth embodiment of the present invention.
【図５】他の実施形態で示すらせん形状高周波誘導コイ
ルを加熱装置として用いた場合の結晶成長装置の構成を
示す図である。FIG. 5 is a diagram showing a configuration of a crystal growth apparatus when a spiral high-frequency induction coil shown in another embodiment is used as a heating apparatus.
１…黒鉛製るつぼ、１ａ…るつぼ本体、１ｂ…蓋材、２
…ＳｉＣ原料粉末、３…ＳｉＣ単結晶基板、４…ＳｉＣ
単結晶、５…接着剤、６…Ｘ線発生源、７…Ｘ線検出
器、８…Ｘ線、９…制御装置、１０…仕切板、１１…珪
素粉末、１２…珪素導入部、１３…らせん形状高周波誘
導コイル。DESCRIPTION OF SYMBOLS 1 ... Graphite crucible, 1a ... Crucible main body, 1b ... Lid material, 2
... SiC raw material powder, 3 ... SiC single crystal substrate, 4 ... SiC
Single crystal, 5 adhesive, 6 X-ray source, 7 X-ray detector, 8 X-ray, 9 control device, 10 partition plate, 11 silicon powder, 12 silicon introduction section, 13 Spiral shaped high frequency induction coil.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 廣瀬 富佐雄 愛知県刈谷市昭和町１丁目１番地 株式会 社デンソー内 (72)発明者 恩田 正一 愛知県刈谷市昭和町１丁目１番地 株式会 社デンソー内 ──────────────────────────────────────────────────続 き Continuing from the front page (72) Inventor Hiroo Tosao 1-1-1, Showa-cho, Kariya-shi, Aichi Prefecture Inside DENSO Corporation (72) Inventor Shoichi Onda 1-1-1, Showa-cho, Kariya-shi, Aichi Stock Company Inside DENSO
Claims (17)
種結晶となる炭化珪素単結晶基板（３）を配置し、前記
炭化珪素原料を加熱昇華させて前記炭化珪素単結晶基板
上に炭化珪素単結晶（４）を成長させる炭化珪素単結晶
の製造過程において、 前記容器外部に備えたＸ線発生源（６）にてＸ線（８）
を前記炭化珪素原料に照射し、前記容器外部に備えたＸ
線検出器（７）により前記容器および前記炭化珪素原料
を透過したＸ線を検出し、そのＸ線の透過量から前記炭
化珪素原料の減少量をモニターし、該減少量が一定とな
るように前記容器内の温度を制御することを特徴とする
炭化珪素単結晶の製造方法。1. A silicon carbide raw material (2) and a silicon carbide single crystal substrate (3) serving as a seed crystal are arranged in a container (1), and the silicon carbide raw material is heated and sublimated to form the silicon carbide single crystal substrate. In the process of producing a silicon carbide single crystal on which a silicon carbide single crystal (4) is grown, an X-ray (8) is generated by an X-ray source (6) provided outside the container.
To the silicon carbide raw material, and X
X-rays transmitted through the container and the silicon carbide raw material are detected by a line detector (7), and the reduction amount of the silicon carbide raw material is monitored from the transmission amount of the X-rays so that the reduction amount becomes constant. A method for producing a silicon carbide single crystal, comprising controlling a temperature in the container.
種結晶となる炭化珪素単結晶基板（３）を配置し、前記
炭化珪素原料を加熱昇華させて前記炭化珪素単結晶基板
上に炭化珪素単結晶（４）を成長させる炭化珪素単結晶
の製造過程において、 前記容器外部に備えたＸ線発生源（６）にてＸ線（８）
を前記炭化珪素原料の上部に照射し、前記容器外部に備
えたＸ線検出器（７）により前記容器および前記炭化珪
素原料を透過したＸ線を検出し、そのＸ線の透過量が一
定となるようにしつつ前記炭化珪素単結晶を成長させる
ことを特徴とする炭化珪素単結晶の製造方法。2. A silicon carbide raw material (2) and a silicon carbide single crystal substrate (3) serving as a seed crystal are arranged in a container (1), and the silicon carbide raw material is heated and sublimated to form the silicon carbide single crystal substrate. In the process of producing a silicon carbide single crystal on which a silicon carbide single crystal (4) is grown, an X-ray (8) is generated by an X-ray source (6) provided outside the container.
Is irradiated onto the upper portion of the silicon carbide raw material, and X-rays transmitted through the container and the silicon carbide raw material are detected by an X-ray detector (7) provided outside the container. A method for producing a silicon carbide single crystal, wherein the silicon carbide single crystal is grown while forming the silicon carbide single crystal.
種結晶となる炭化珪素単結晶基板（３）を配置し、前記
炭化珪素原料を加熱昇華させて前記炭化珪素単結晶基板
上に炭化珪素単結晶（４）を成長させる炭化珪素単結晶
の製造過程において、 前記炭化珪素原料とは別に、前記容器内に少なくとも珪
素を含む材料（１１）を配置すると共に、該珪素を含む
材料と前記炭化珪素原料との間を、珪素ガスを通過させ
ることができる仕切板（１０）で仕切り、前記珪素を含
む材料から発生させた珪素ガスを前記仕切板を通じて前
記炭化珪素単結晶基板に供給させるようにし、 前記容器外部に備えたＸ線発生源（６）にてＸ線（８）
を前記炭化珪素原料の上部に照射し、前記容器外部に備
えたＸ線検出器（７）により前記容器および前記炭化珪
素原料を透過したＸ線を検出し、そのＸ線の透過量が一
定となるようにしつつ前記炭化珪素単結晶を成長させる
ことを特徴とする炭化珪素単結晶の製造方法。3. A silicon carbide raw material (2) and a silicon carbide single crystal substrate (3) serving as a seed crystal are arranged in a container (1), and the silicon carbide raw material is heated and sublimated to form the silicon carbide single crystal substrate. In the process of producing a silicon carbide single crystal on which a silicon carbide single crystal (4) is grown, a material (11) containing at least silicon is placed in the container separately from the silicon carbide raw material and contains the silicon carbide. The material and the silicon carbide raw material are partitioned by a partition plate (10) through which a silicon gas can pass, and silicon gas generated from the silicon-containing material is passed through the partition plate to the silicon carbide single crystal substrate. X-rays (8) at an X-ray source (6) provided outside the container.
Is irradiated onto the upper portion of the silicon carbide raw material, and X-rays transmitted through the container and the silicon carbide raw material are detected by an X-ray detector (7) provided outside the container. A method for producing a silicon carbide single crystal, wherein the silicon carbide single crystal is grown while forming the silicon carbide single crystal.
種結晶となる炭化珪素単結晶基板（３）を配置し、前記
炭化珪素原料を加熱昇華させて前記炭化珪素単結晶基板
上に炭化珪素単結晶（４）を成長させる炭化珪素単結晶
の製造過程において、 前記炭化珪素原料とは別に、前記容器外に珪素を含む材
料の供給源となる珪素導入部（１２）を備え、前記容器
に形成された開口部を通じて前記珪素導入部から前記珪
素を含む材料の導入を行い、 前記容器外部に備えたＸ線発生源（６）にてＸ線（８）
を前記炭化珪素原料の上部に照射し、前記容器外部に備
えたＸ線検出器（７）により前記容器および前記炭化珪
素原料を透過したＸ線を検出し、そのＸ線の透過量が一
定となるように前記珪素を含む材料の導入量を制御する
ことを特徴とする炭化珪素単結晶の製造方法。4. A silicon carbide raw material (2) and a silicon carbide single crystal substrate (3) serving as a seed crystal are arranged in a container (1), and the silicon carbide raw material is heated and sublimated to form the silicon carbide single crystal substrate. In the manufacturing process of a silicon carbide single crystal on which a silicon carbide single crystal (4) is grown, a silicon introduction part (12) serving as a supply source of a material containing silicon is provided outside the container separately from the silicon carbide raw material. Introducing the silicon-containing material from the silicon introduction portion through an opening formed in the container; and X-rays (8) at an X-ray source (6) provided outside the container.
Is irradiated onto the upper portion of the silicon carbide raw material, and X-rays transmitted through the container and the silicon carbide raw material are detected by an X-ray detector (7) provided outside the container. A method for producing a silicon carbide single crystal, characterized in that the amount of the silicon-containing material to be introduced is controlled so as to be as follows.
置（１０）による温度制御によって、前記前記Ｘ線の透
過量を一定に制御することを特徴とする請求項２乃至４
に記載の炭化珪素単結晶の製造方法。5. The transmission amount of the X-rays is controlled to be constant by temperature control by a control device (10) for controlling the temperature in the container.
3. The method for producing a silicon carbide single crystal according to item 1.
器内の温度分布を変化させる制御であることを特徴とす
る請求項５に記載の炭化珪素単結晶の製造方法。6. The method for producing a silicon carbide single crystal according to claim 5, wherein the temperature control by the control device is a control for changing a temperature distribution in the container.
（１３）に囲まれるように配置し、該コイルによって前
記容器内の温度を制御するようにし、 前記コイルを挟んで一直線にＸ線発生源と前記Ｘ線検出
器を配置し、Ｘ線発生源からのＸ線が、前記コイルを避
けるように照射され、前記容器及び前記炭化珪素原料を
透過して前記Ｘ線検出器に到達するようにすることを特
徴とする請求項１、５又は６に記載の炭化珪素単結晶の
製造方法。7. The container is arranged so as to be surrounded by a helical high-frequency induction coil (13), and the temperature in the container is controlled by the coil. The X-ray detector is arranged so that X-rays from an X-ray source are irradiated so as to avoid the coil, pass through the container and the silicon carbide raw material, and reach the X-ray detector. The method for producing a silicon carbide single crystal according to claim 1, 5, or 6.
前記Ｘ線検出器をらせん駆動させることを特徴とする請
求項７に記載の炭化珪素単結晶の製造方法。8. The method of manufacturing a silicon carbide single crystal according to claim 7, wherein the X-ray source and the X-ray detector are helically driven along the coil.
種結晶となる炭化珪素単結晶基板（３）を配置し、前記
炭化珪素原料を加熱昇華させて前記炭化珪素単結晶基板
上に炭化珪素単結晶（４）を成長させる炭化珪素単結晶
の製造装置において、 前記容器外部に備えられ、前記容器内部に配置された前
記炭化珪素原料に向かってＸ線（８）を照射するＸ線発
生源（６）と、 前記容器外部に備えられ、前記炭化珪素原料を透過した
前記Ｘ線の透過量を検出するＸ線検出器（７）とを備え
ていることを特徴とする炭化珪素単結晶の製造装置。9. A silicon carbide raw material (2) and a silicon carbide single crystal substrate (3) serving as a seed crystal are arranged in a container (1), and the silicon carbide raw material is heated and sublimated to form the silicon carbide single crystal substrate. An apparatus for producing a silicon carbide single crystal on which a silicon carbide single crystal (4) is grown, wherein an X-ray (8) is irradiated toward the silicon carbide raw material provided outside the container and disposed inside the container. An X-ray generation source (6), and an X-ray detector (7) provided outside the container and configured to detect an amount of the X-ray transmitted through the silicon carbide raw material (7). Equipment for manufacturing silicon single crystals.
れ、該検出結果に基づいて前記容器内の温度を制御でき
る制御装置（９）を備えていることを特徴とする請求項
９に記載の炭化珪素単結晶の製造装置。10. The apparatus according to claim 9, further comprising a control device (9) to which a detection result of the X-ray detector is input, and which can control a temperature in the container based on the detection result. For producing silicon carbide single crystal.
ら前記炭化珪素原料の減少量をモニターし、該減少量が
一定となるように前記容器内の温度を制御するものであ
ることを特徴とする請求項１０に記載の炭化珪素単結晶
の製造装置。11. The method according to claim 1, wherein the control device monitors a reduction amount of the silicon carbide raw material from the X-ray transmission amount, and controls a temperature in the container so that the reduction amount becomes constant. The apparatus for producing a silicon carbide single crystal according to claim 10.
一定となるように前記容器内の温度を制御することを特
徴とする請求項１０に記載の炭化珪素単結晶の製造装
置。12. The apparatus for producing a silicon carbide single crystal according to claim 10, wherein the control device controls the temperature in the container so that the amount of transmission of the X-rays is constant.
外に珪素を含む材料を前記容器内に導入する珪素導入部
（１２）と、 前記Ｘ線検出器の検出結果が入力され、該検出結果に基
づいて前記珪素導入部による前記珪素を含む材料の導入
量を制御する制御装置（９）とを備えていることを特徴
とする請求項９に記載の炭化珪素単結晶の製造装置。13. A silicon introduction part (12) for introducing a material containing silicon outside the container into the container separately from the silicon carbide raw material, and a detection result of the X-ray detector is input. The apparatus for producing a silicon carbide single crystal according to claim 9, further comprising: a control device (9) for controlling an introduction amount of the material containing silicon by the silicon introduction unit based on a result.
ら前記炭化珪素原料の減少量をモニターし、該減少量が
一定となるように前記珪素を含む材料の導入量を制御す
るものであることを特徴とする請求項１３に記載の炭化
珪素単結晶の製造装置。14. The control device monitors a reduction amount of the silicon carbide raw material from the transmission amount of the X-ray, and controls an introduction amount of the silicon-containing material so that the reduction amount becomes constant. The apparatus for producing a silicon carbide single crystal according to claim 13, wherein:
一定となるように前記珪素を含む材料の導入量を制御す
ることを特徴とする請求項１３に記載の炭化珪素単結晶
の製造装置。15. The production of a silicon carbide single crystal according to claim 13, wherein the control device controls the introduction amount of the silicon-containing material so that the transmission amount of the X-ray becomes constant. apparatus.
容器の加熱を行なうらせん形状高周波誘導コイル（１
３）を有し、 前記Ｘ線発生源からのＸ線が、前記コイルを避けるよう
に照射され、前記容器及び前記炭化珪素原料を透過して
前記Ｘ線検出器に到達するように、前記コイルを挟んで
一直線に前記Ｘ線発生源と前記Ｘ線検出器とが配置され
ており、 前記コイルに沿って、前記Ｘ線発生源と前記Ｘ線検出器
をらせん駆動させる駆動機構が備えられていることを特
徴とする請求項９乃至１５のいずれか１つに記載の炭化
珪素単結晶の製造装置。16. A helical high-frequency induction coil (1) arranged to surround the container and heats the container.
3) wherein the X-rays from the X-ray source are irradiated so as to avoid the coil, and the X-ray is transmitted through the container and the silicon carbide raw material to reach the X-ray detector. The X-ray source and the X-ray detector are arranged in a straight line with a drive mechanism provided between the X-ray source and the X-ray detector in a spiral drive along the coil. The apparatus for producing a silicon carbide single crystal according to any one of claims 9 to 15, wherein:
と種結晶となる炭化珪素単結晶基板（３）を配置し、前
記炭化珪素原料を加熱昇華させて前記炭化珪素単結晶基
板上に炭化珪素単結晶（４）を成長させる炭化珪素単結
晶の製造過程において、 前記容器外部に備えたＸ線発生源（６）にてＸ線を前記
炭化珪素原料に照射し、前記容器外部に備えたＸ線検出
器（７）により前記容器および前記炭化珪素原料を透過
したＸ線を検出し、そのＸ線の透過量から、前記炭化珪
素原料の減少量をモニターする炭化珪素原料の昇華状態
検出方法。17. A silicon carbide raw material (2) in a container (1).
And a silicon carbide single crystal substrate (3) serving as a seed crystal is arranged, and the silicon carbide raw material is heated and sublimated to produce a silicon carbide single crystal (4) on the silicon carbide single crystal substrate. In the process, the X-ray source (6) provided outside the container irradiates the silicon carbide raw material with X-rays, and the X-ray detector (7) provided outside the container provides the X-ray detector (7) with the container and the silicon carbide raw material. A method for detecting the sublimation state of a silicon carbide raw material, comprising detecting X-rays transmitted through the silicon carbide and monitoring the amount of reduction of the silicon carbide raw material from the amount of transmitted X-rays.
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|---|---|---|---|
| JP2000041426A JP4238449B2 (en) | 2000-02-15 | 2000-02-15 | Method and apparatus for producing silicon carbide single crystal |
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| JP4238449B2 JP4238449B2 (en) | 2009-03-18 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004131376A (en) * | 2002-09-19 | 2004-04-30 | Showa Denko Kk | Silicon carbide single crystal, and method and apparatus for producing the same |
| KR20190000618A (en) * | 2017-06-23 | 2019-01-03 | 주식회사 엘지화학 | Manufacturing apparatus for silicon carbide single crystal |
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| CN116676662A (en) * | 2023-07-31 | 2023-09-01 | 北京青禾晶元半导体科技有限责任公司 | Bonding method and application of silicon carbide seed crystal |
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| KR101189372B1 (en) | 2011-01-13 | 2012-10-09 | 엘지이노텍 주식회사 | Holder-seed assembly and method for the same |
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2000
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2004131376A (en) * | 2002-09-19 | 2004-04-30 | Showa Denko Kk | Silicon carbide single crystal, and method and apparatus for producing the same |
| JP4505202B2 (en) * | 2002-09-19 | 2010-07-21 | 昭和電工株式会社 | Method and apparatus for producing silicon carbide single crystal |
| KR20190000618A (en) * | 2017-06-23 | 2019-01-03 | 주식회사 엘지화학 | Manufacturing apparatus for silicon carbide single crystal |
| KR102153519B1 (en) * | 2017-06-23 | 2020-09-08 | 주식회사 엘지화학 | Manufacturing apparatus for silicon carbide single crystal |
| KR20220009142A (en) * | 2020-07-15 | 2022-01-24 | 주식회사 쎄닉 | Monitoring apparatus for monitoring inside of a reaction crucible and method for growing an ingot with a growth apparatus applied the same |
| KR102447492B1 (en) * | 2020-07-15 | 2022-09-26 | 주식회사 쎄닉 | Monitoring apparatus for monitoring inside of a reaction crucible and method for growing an ingot with a growth apparatus applied the same |
| CN116676662A (en) * | 2023-07-31 | 2023-09-01 | 北京青禾晶元半导体科技有限责任公司 | Bonding method and application of silicon carbide seed crystal |
| CN116676662B (en) * | 2023-07-31 | 2023-11-10 | 北京青禾晶元半导体科技有限责任公司 | Bonding method and application of silicon carbide seed crystal |
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