JPS63156095A - Liquid phase epitaxy of sic single crystal - Google Patents
Liquid phase epitaxy of sic single crystalInfo
- Publication number
- JPS63156095A JPS63156095A JP30491786A JP30491786A JPS63156095A JP S63156095 A JPS63156095 A JP S63156095A JP 30491786 A JP30491786 A JP 30491786A JP 30491786 A JP30491786 A JP 30491786A JP S63156095 A JPS63156095 A JP S63156095A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- growth
- sic
- crystal
- sic single
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 45
- 238000004943 liquid phase epitaxy Methods 0.000 title 1
- 239000000758 substrate Substances 0.000 claims abstract description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 14
- 239000010439 graphite Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims description 15
- 239000007791 liquid phase Substances 0.000 claims description 7
- 238000007796 conventional method Methods 0.000 abstract description 5
- 239000000155 melt Substances 0.000 abstract description 4
- 238000000407 epitaxy Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、ＳｉＣ単結晶基板上に５ｔｃｆａ結晶層を液
相エピタキシャル成長せしめる方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for liquid phase epitaxial growth of a 5tcfa crystal layer on a SiC single crystal substrate.
ＳｉＣ結晶は、その禁制帯幅が２．３９ ｅ Ｖ 〜３
．３３ ｅ Ｖと広範囲であり、またｐｎ接合の形成が
可能であるので、赤色から青色までのすべての波長範囲
の可視光を発する発光ダイ第一ドの材料として利用され
ている。とりわけ、室温において約３ｅｖの禁制帯幅を
有するα型６Ｈ（ヘキサゴナール）タイプのＳｉＣ結晶
は、青色発光ダイオードの材料として用いられている。The SiC crystal has a forbidden band width of 2.39 eV ~ 3
．． Since it has a wide range of 33 eV and can form p-n junctions, it is used as a material for light-emitting diodes that emit visible light in the entire wavelength range from red to blue. In particular, α-type 6H (hexagonal) type SiC crystal, which has a forbidden band width of about 3 ev at room temperature, is used as a material for blue light-emitting diodes.
ところで、この青色発光ダイオードは、６Ｈ型の結晶基
板に、同じ＜６８型ＳｉＣ結晶のｎ型層。By the way, this blue light emitting diode has an n-type layer of the same <68-type SiC crystal on a 6H-type crystal substrate.
ｐ型層をエピタキシャル成長させて製造される。It is manufactured by epitaxially growing a p-type layer.
そして、このエピタキシャル成長は主に以下の如き液相
エピタキシャル成長方法にて行われていた。This epitaxial growth was mainly carried out by the following liquid phase epitaxial growth method.
即ち、黒鉛るつぼにＳｉを満たし、これを加熱する。こ
の黒鉛るつぼ内に、支持棒に固定されたＳｉＣ結晶基板
を一定時間保持する。するとＳｉ融液中に加熱されたる
つぼ壁からＣが溶は込み、Ｓｉと反応して前記結晶基板
上にＳｉＣ結晶が成長する。That is, a graphite crucible is filled with Si and heated. A SiC crystal substrate fixed to a support rod is held in this graphite crucible for a certain period of time. Then, C melts into the Si melt from the heated crucible wall, reacts with Si, and grows SiC crystals on the crystal substrate.
ところが、上述した従来の成長方法では、結晶性が十分
でなく欠陥結晶が多いという問題点があった。そしてそ
の結果、これらの結晶を用いて製造された青色発光ダイ
オードには、通電による発光波長の長波長化または低輝
度化をきたす等品質が劣悪なものが含まれており、製品
の歩留りが悪いという問題点があった。However, the conventional growth method described above has a problem in that the crystallinity is not sufficient and there are many defective crystals. As a result, some of the blue light emitting diodes manufactured using these crystals are of poor quality, such as emitted light having a longer wavelength or lower brightness when energized, resulting in poor product yields. There was a problem.
そして本発明者は種々の研究の結果、上述した問題点は
結晶成長過程における成長速度（Ｊｏｕｎａｌｏｆ Ａ
ｐｐｌｉｅｄ Ｐｈｙｓｉｃｓ ５０ （１２） 、
Ｄｅｃｅ＋ｍｓ＋ｂｅｒ １９７９゜８２１５〜８２２
５に示されている速度は１５〜３０μｍ／ｈ、またＪｏ
ｕｎａｌ ｏｆ Ａｐｐｌｉｅｄ Ｐｈｙｓｉｃｓ
５３ （１０） ＋０ｃｔｏｂｅｒ １９８２．６９
６２〜６９６７に示されている速度は約５０μｍ ／
ｈ ）に起因することを知見した。As a result of various studies, the present inventor found that the above-mentioned problem can be solved by the growth rate in the crystal growth process (Journal of A
pplied Physics 50 (12),
Dece+ms+ber 1979°8215~822
The speed shown in 5 is 15-30 μm/h, and Jo
unal of Applied Physics
53 (10) +0ctober 1982.69
The speed shown in 62-6967 is approximately 50 μm/
h).
本発明はかかる知見に基づいてなされたものであって、
結晶の成長速度を従来より遅く （５μｍ ／ ｈ以下
）して結晶を成長させることにより、結晶性が向上し、
製造される発光ダイオードが良質のものとなり、歩留り
が向上するＳｉＣ単結晶の液相エピタキシャル成長方法
を提供することを目的とする。The present invention was made based on such knowledge, and
By growing crystals at a slower crystal growth rate than conventional methods (5 μm/h or less), crystallinity is improved,
It is an object of the present invention to provide a method for liquid phase epitaxial growth of SiC single crystal, in which the light emitting diodes manufactured are of good quality and the yield is improved.
本発明に係るＳｉＣ単結晶の液相エピタキシャル成長方
法は、黒鉛るつぼ内のＳｉ融液にＳｉＣ単結晶基板を浸
漬させて、該ＳｉＣ単結晶基板上にＳｉＣ単結晶層を液
相エピタキシャル成長せしめる方法において、前記Ｓｉ
Ｃ単結晶層の成長速度を５μｍ ／ ｈ以下とすること
を特徴とする。The liquid phase epitaxial growth method of SiC single crystal according to the present invention is a method in which a SiC single crystal substrate is immersed in a Si melt in a graphite crucible, and a SiC single crystal layer is liquid phase epitaxially grown on the SiC single crystal substrate. The Si
It is characterized in that the growth rate of the C single crystal layer is 5 μm/h or less.
黒鉛るつぼ内のＳｉ融液にＳｉＣ単結晶基板を浸漬させ
て、該ＳｉＣ単結晶基板上に５ｉＣｆｉｉ晶層をエピタ
キシャル成長させる。この際、ＳｉＣ単結晶層の成長速
度を５μｍ ／ ｈ以下とする。そうすると結晶性の良
好なＳｉＣ単結晶層がＳｉＣ単結晶基板上に成長される
。A SiC single crystal substrate is immersed in a Si melt in a graphite crucible, and a 5iCfii crystal layer is epitaxially grown on the SiC single crystal substrate. At this time, the growth rate of the SiC single crystal layer is set to 5 μm/h or less. Then, a SiC single crystal layer with good crystallinity is grown on the SiC single crystal substrate.
以下、本発明をその実施例を示す図面に基づいて説明す
る。第１図は本発明方法を実施するための装置の断面模
式図であり、図中１は石英製の反応管を示す０反応管１
内には、Ｓｉ融液２を収容した黒鉛るつぼ３が設けられ
ている。また、黒鉛るつぼ３内のＳｉ融液２にその端部
を浸漬させた状態で、円柱状の基板支持棒４が、その長
軸方向を前記反応管１の長軸方向つまり上下方向に一致
させて設けられている。該基板支持棒４のＳｉ融／＆２
に浸漬されない側の端部は図示しない駆動部に接続して
おり、基板支持棒４は該駆動部の作用により、その軸芯
を中心にして回転されるようになってい 。Hereinafter, the present invention will be explained based on drawings showing embodiments thereof. FIG. 1 is a schematic cross-sectional view of an apparatus for implementing the method of the present invention, in which 1 indicates a reaction tube made of quartz.
A graphite crucible 3 containing a Si melt 2 is provided inside. Further, with its end immersed in the Si melt 2 in the graphite crucible 3, the cylindrical substrate support rod 4 is aligned so that its long axis direction coincides with the long axis direction of the reaction tube 1, that is, the vertical direction. It is provided. Si melting of the substrate support rod 4/&2
The end portion on the side that is not immersed in the substrate is connected to a drive unit (not shown), and the substrate support rod 4 is rotated about its axis by the action of the drive unit.
る。Ru.
また、基板支持棒４のＳｉ融液２に浸漬される下端部に
は、端面側が底面をなす円錐状の欠損部４ａが端面に達
して形成されている。欠損部４ａには、基板支持棒４の
短軸方向にＳｉＣ成長用基板５が、基板支持４１ｓ４の
欠損部４ａ内に嵌込んだ状態で取付けられている。また
、黒鉛るつぼ３には上Ｍ６が冠着されており、更に、反
応管ｌの外周面には、反応管１内を加熱するための高周
波コイル７が囲繞されている。Further, at the lower end of the substrate support rod 4 that is immersed in the Si melt 2, a conical cutout 4a whose bottom surface is on the end surface side is formed so as to reach the end surface. The SiC growth substrate 5 is attached to the cutout part 4a in the short axis direction of the substrate support rod 4 in a state that it is fitted into the cutout part 4a of the substrate support 41s4. Further, an upper M6 is attached to the graphite crucible 3, and a high frequency coil 7 for heating the inside of the reaction tube 1 is surrounded on the outer peripheral surface of the reaction tube 1.
次に、第１図に示す装置を用いてＳｉＣ単結晶を基板上
に成長させる手順について説明する。Next, a procedure for growing a SiC single crystal on a substrate using the apparatus shown in FIG. 1 will be described.
まず、高周波コイル７に通電して黒鉛るつぼ３を結晶成
長温度（１６５０〜１７００℃）まで加熱する。First, the high frequency coil 7 is energized to heat the graphite crucible 3 to the crystal growth temperature (1650 to 1700°C).
この際、黒鉛るつぼ３の上下方向に、底部側が低温部と
なるように温度勾配を設定する。次に、基板支持棒４に
固定されたＳｉＣ成長用基板５をＳｉ融唆２の低温部に
一定時間保持する。そうすると、加熱された黒鉛るつぼ
３の高温部の内壁面からＳｉ独液液２中Ｃが溶は込み、
これが融液の対流によって低温部に流入され、Ｓｉと反
応してＳｉＣ成長用基板５上にＳｉＣ単結晶が成長する
。なお、結晶成長中にＳｉＣ成長用基板５を回転させる
ことにより、吻−な成長層が形成される。At this time, a temperature gradient is set in the vertical direction of the graphite crucible 3 so that the bottom side becomes the low temperature part. Next, the SiC growth substrate 5 fixed to the substrate support rod 4 is held in the low temperature part of the Si melt 2 for a certain period of time. Then, C in the Si liquid solution 2 penetrates into the solution from the inner wall surface of the high temperature part of the heated graphite crucible 3.
This flows into the low temperature part by the convection of the melt, reacts with Si, and a SiC single crystal grows on the SiC growth substrate 5. Note that by rotating the SiC growth substrate 5 during crystal growth, a rostral growth layer is formed.
そしてこの際、結晶の成長速度を５μｍ／ｈ以下とする
。なお、成長速度を制御する方法は実願＠６１−２４５
２号に詳述した方法を用いる。即ち、黒鉛るつぼの底面
の保温手段としてカーボンフェルトからなる複数の保温
ディスクを着脱自在に装着し、この保温ディスクの枚数
を適宜選択することにより、成長用基板の位置における
温度勾配を調整して結晶の成長速度を制御する。At this time, the crystal growth rate is set to 5 μm/h or less. In addition, the method for controlling the growth rate is disclosed in Jitsugaku@61-245.
The method detailed in No. 2 is used. That is, a plurality of heat-insulating disks made of carbon felt are removably attached as heat-insulating means on the bottom of the graphite crucible, and by selecting the appropriate number of heat-insulating disks, the temperature gradient at the position of the growth substrate is adjusted and crystallization is performed. control the growth rate of
次に、本発明方法の要旨である結晶成長速度の限定理由
について説明する。Next, the reason for limiting the crystal growth rate, which is the gist of the method of the present invention, will be explained.
成長層の成長速度が遅いほど、成長層の結晶性が向上す
ることは以下のようにしてＩｒｉ認した。即ち第１図に
示す装置を用い、成長速度を変化させて成長層を形成し
、各成長層のエツチングによるエッチピット密度を光学
顕微鏡にて調べた。エツチング条件は、ＫＯＨ熔融塩に
て約５００℃、１分間エツチングである。第２図は成長
速度とエッチピット密度との関係を示すグラフであり、
成長速度が５μｍ／ｈ以下ではエッチピント密度が小さ
く、良好な結晶性の成長層が得られている。It was found as follows that the slower the growth rate of the growth layer, the better the crystallinity of the growth layer. That is, using the apparatus shown in FIG. 1, growth layers were formed by varying the growth rate, and the etch pit density due to etching of each growth layer was examined using an optical microscope. The etching conditions were etching with molten KOH at about 500° C. for 1 minute. Figure 2 is a graph showing the relationship between growth rate and etch pit density.
When the growth rate is 5 μm/h or less, the etch focus density is small and a grown layer with good crystallinity is obtained.
従って、５μｍ／ｈ以下の成長速度で結晶成長を行えば
、良好な結晶性の成長層が得られる。Therefore, if crystal growth is performed at a growth rate of 5 μm/h or less, a grown layer with good crystallinity can be obtained.
第３図は、第１図に示す装置を用いて青色発光ダイオー
ドを製造した場合の、エピタキシャル成長層の成長速度
と青色発光ダイオードの発光強度との関係を示したグラ
フである。なお、成長温度は１７００℃で一定としてい
る。成長速度が５μｍ ／ ｈ以下の場合では、発光強
度の強い発光ダイオードが得られており、これは良好な
結晶性の成長層が得られていることを示している。FIG. 3 is a graph showing the relationship between the growth rate of the epitaxial growth layer and the emission intensity of the blue light emitting diode when the blue light emitting diode was manufactured using the apparatus shown in FIG. Note that the growth temperature is kept constant at 1700°C. When the growth rate is 5 μm/h or less, a light emitting diode with strong emission intensity is obtained, which indicates that a grown layer with good crystallinity is obtained.
以上詳述した如く本発明方法では、従来方法より成長速
度を遅くするので、従来より良好な結晶性を有するエピ
タキシャル成長層を形成することができる。そしてその
結果、製造される発光ダイオードが良質となり、歩留り
が向上する等本発明は優れた効果を奏する。As detailed above, in the method of the present invention, the growth rate is slower than in the conventional method, so that an epitaxially grown layer having better crystallinity than in the conventional method can be formed. As a result, the light emitting diodes produced are of good quality, and the present invention exhibits excellent effects such as improved yield.
第１図は本発明を実施するための装置の断面模式図、第
２図はエピタキシャル成長層のエッチピット密度と成長
速度との関係を示すグラフ、第３図は青色発光ダイオー
ドの発光強度とエピタキシャル成長層の成長速度との関
係を示すグラフである。
１・・・反応管 ２・・・Ｓｔ融液 ３・・・黒鉛るつ
ぼ ４・・・基板支持棒 ５・・・ＳｉＣ成長用基板
６・・・上蓋７・・・高周波コイル
特許出願人 三洋電機株式会社
代理人 弁理士 河 野 登 夫
ｊ Ｚ
隼 １ ロ
ＯＳ ＋０ １５ ２００
５ ＋Ｏ＋ｓ ２
０＾長達ｑｔｐ２て几ン
葡 ３ （！］Fig. 1 is a schematic cross-sectional view of an apparatus for carrying out the present invention, Fig. 2 is a graph showing the relationship between the etch pit density and growth rate of the epitaxially grown layer, and Fig. 3 is a graph showing the relationship between the emission intensity of the blue light emitting diode and the epitaxially grown layer. It is a graph showing the relationship between the growth rate and the growth rate. 1... Reaction tube 2... St melt 3... Graphite crucible 4... Substrate support rod 5... SiC growth substrate
6...Top lid 7...High frequency coil patent applicant Sanyo Electric Co., Ltd. agent Patent attorney Noboru Konoj Z Hayabusa 1 RoOS +0 15 200
5 +O+s 2
0＾Nagadatsu qtp2 te Rin Grain 3 (!]
Claims (1)
させて、該ＳｉＣ単結晶基板上にＳｉＣ単結晶層を液相
エピタキシャル成長せしめる方法において、 前記ＳｉＣ単結晶層の成長速度を５μｍ／ｈ以下とする
ことを特徴とするＳｉＣ単結晶の液相エピタキシャル成
長方法。[Claims] 1. A method for growing a SiC single crystal layer on the SiC single crystal substrate by liquid phase epitaxial growth by immersing the SiC single crystal substrate in a Si melt in a graphite crucible, comprising: A method for liquid phase epitaxial growth of SiC single crystal, characterized in that the growth rate is 5 μm/h or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30491786A JPS63156095A (en) | 1986-12-19 | 1986-12-19 | Liquid phase epitaxy of sic single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP30491786A JPS63156095A (en) | 1986-12-19 | 1986-12-19 | Liquid phase epitaxy of sic single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63156095A true JPS63156095A (en) | 1988-06-29 |
Family
ID=17938860
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP30491786A Pending JPS63156095A (en) | 1986-12-19 | 1986-12-19 | Liquid phase epitaxy of sic single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63156095A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5679153A (en) * | 1994-11-30 | 1997-10-21 | Cree Research, Inc. | Method for reducing micropipe formation in the epitaxial growth of silicon carbide and resulting silicon carbide structures |
| JP2009091222A (en) * | 2007-10-11 | 2009-04-30 | Sumitomo Metal Ind Ltd | PRODUCTION METHOD FOR SiC SINGLE CRYSTAL, SiC SINGLE CRYSTAL WAFER AND SiC SEMICONDUCTOR DEVICE |
| WO2009107188A1 (en) * | 2008-02-25 | 2009-09-03 | 財団法人地球環境産業技術研究機構 | METHOD FOR GROWING SINGLE CRYSTAL SiC |
| JP2011098870A (en) * | 2009-11-09 | 2011-05-19 | Toyota Motor Corp | APPARATUS AND METHOD FOR PRODUCING SiC SINGLE CRYSTAL |
| CN112136203A (en) * | 2018-05-23 | 2020-12-25 | 三菱电机株式会社 | Method for manufacturing SiC epitaxial substrate |
-
1986
- 1986-12-19 JP JP30491786A patent/JPS63156095A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5679153A (en) * | 1994-11-30 | 1997-10-21 | Cree Research, Inc. | Method for reducing micropipe formation in the epitaxial growth of silicon carbide and resulting silicon carbide structures |
| JP2009091222A (en) * | 2007-10-11 | 2009-04-30 | Sumitomo Metal Ind Ltd | PRODUCTION METHOD FOR SiC SINGLE CRYSTAL, SiC SINGLE CRYSTAL WAFER AND SiC SEMICONDUCTOR DEVICE |
| WO2009107188A1 (en) * | 2008-02-25 | 2009-09-03 | 財団法人地球環境産業技術研究機構 | METHOD FOR GROWING SINGLE CRYSTAL SiC |
| JP2011098870A (en) * | 2009-11-09 | 2011-05-19 | Toyota Motor Corp | APPARATUS AND METHOD FOR PRODUCING SiC SINGLE CRYSTAL |
| CN112136203A (en) * | 2018-05-23 | 2020-12-25 | 三菱电机株式会社 | Method for manufacturing SiC epitaxial substrate |
| CN112136203B (en) * | 2018-05-23 | 2024-04-09 | 三菱电机株式会社 | Method for manufacturing SiC epitaxial substrate |
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