JPH01305898A - Method and apparatus for production of silicon carbide single crystal - Google Patents
Method and apparatus for production of silicon carbide single crystalInfo
- Publication number
- JPH01305898A JPH01305898A JP13673688A JP13673688A JPH01305898A JP H01305898 A JPH01305898 A JP H01305898A JP 13673688 A JP13673688 A JP 13673688A JP 13673688 A JP13673688 A JP 13673688A JP H01305898 A JPH01305898 A JP H01305898A
- Authority
- JP
- Japan
- Prior art keywords
- silicon carbide
- seed crystal
- substrate
- crystal substrate
- single crystal
- 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 99
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- 239000000758 substrate Substances 0.000 claims abstract description 40
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 21
- 239000010439 graphite Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001953 recrystallisation Methods 0.000 claims description 4
- 238000000859 sublimation Methods 0.000 claims description 4
- 230000008022 sublimation Effects 0.000 claims description 4
- 239000012298 atmosphere Substances 0.000 claims description 3
- 239000011261 inert gas Substances 0.000 claims description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 abstract description 4
- 238000005530 etching Methods 0.000 abstract description 4
- 229910003460 diamond Inorganic materials 0.000 abstract description 3
- 239000010432 diamond Substances 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 229910052786 argon Inorganic materials 0.000 abstract description 2
- 238000005520 cutting process Methods 0.000 abstract description 2
- 238000004381 surface treatment Methods 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- XUIMIQQOPSSXEZ-IGMARMGPSA-N silicon-28 atom Chemical compound [28Si] XUIMIQQOPSSXEZ-IGMARMGPSA-N 0.000 description 1
- 235000012431 wafers Nutrition 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Abstract
Description
【発明の詳細な説明】
(産業上の利用分野)
本発明は炭化珪素(SiC)単結晶製造方法および装置
に関するものである。さらに詳しく述べると、本発明は
青色発光グイオードや高温電子装置等への応用面に有用
な大面積の炭化珪素を効率良く成長させる炭化珪素単結
晶製造方法および装置に関する。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method and apparatus for producing a silicon carbide (SiC) single crystal. More specifically, the present invention relates to a method and apparatus for producing a silicon carbide single crystal for efficiently growing a large area of silicon carbide useful for applications such as blue light-emitting diodes and high-temperature electronic devices.
(従来の技術)
従来の炭化珪素単結晶製造方法においては、特公昭59
−48792号公報に開示されているように、不活性〃
ス雰囲気中で炭化珪素粉末原材料を加熱昇華させる昇華
再結晶法が大型炭化珪素単結晶を得る有力な方法となっ
ている。第4図に、実開昭60−136134号公報に
開示されている昇華再結晶法における従来の装置を示す
、開口した黒鉛製るつぽ21に原材料の炭化珪素粉末2
2が設置され、上部の蓋体23内面側の略中央より垂下
した種結晶載置部23mに炭化珪素機結晶基板24が固
定されている。固定手段として、従来は第5図に示すよ
うに黒鉛製L″r−r一部材用いて種結晶基板24を保
持するか、または第6図(、)、(b)に示すように炭
化珪素種結晶基板24と種結晶載1ff1部23cの間
にシリコン28もしくは炭化珪素29を挿入し、これを
熱処理することによって固着する方法が提案されている
。(Prior art) In the conventional silicon carbide single crystal manufacturing method,
As disclosed in Publication No. 48792, inert
The sublimation recrystallization method, in which silicon carbide powder raw material is heated and sublimated in a gas atmosphere, is an effective method for obtaining large silicon carbide single crystals. FIG. 4 shows a conventional apparatus for the sublimation recrystallization method disclosed in Japanese Utility Model Application No. 60-136134, in which raw material silicon carbide powder 2 is placed in an open graphite crucible 21.
2 is installed, and a silicon carbide organic crystal substrate 24 is fixed to a seed crystal mounting portion 23m that hangs down from approximately the center of the inner surface side of the upper lid body 23. Conventionally, as a fixing means, the seed crystal substrate 24 is held using a graphite L''r member as shown in FIG. 5, or silicon carbide is used as shown in FIGS. A method has been proposed in which silicon 28 or silicon carbide 29 is inserted between seed crystal substrate 24 and seed crystal support 1ff1 portion 23c and fixed by heat treatment.
(発明が解決しようとする課題)
然るに黒鉛!!L’?一部材等を用いた保持法では、該
部材が種結晶基板の表面に当接していることから該部材
上に炭化珪素の多結晶が成長し、種結晶表面に成長しよ
うとする単結晶部分に食い込んでしまい、断面積の大き
な炭化珪素単結晶を得るのに不都合である。また、シリ
コン等を用いた固着法は固着のための作業が複雑であり
、固着により不必要な歪みを生じさせる危惧があるとい
う問題点があった。(Problem to be solved by the invention) But graphite! ! L'? In the holding method using a single member, since the member is in contact with the surface of the seed crystal substrate, silicon carbide polycrystals grow on the member, and the single crystal portion that is about to grow on the seed crystal surface grows. This is inconvenient for obtaining a silicon carbide single crystal with a large cross-sectional area. Furthermore, the fixing method using silicone or the like has the problem that the fixing work is complicated, and there is a risk that unnecessary distortion may occur due to the fixing.
本発明は炭化珪素種結晶基板を容易に種結晶載W1f!
Sに固定し、かつ種結晶基板周辺の多結晶の発生を抑制
して炭化珪素単結晶のみを成長させ、断面積の大きな良
質の炭化珪素単結晶を得る方法および装置を提供するこ
とを目的とする。The present invention makes it easy to mount a silicon carbide seed crystal substrate on a seed crystal W1f!
The purpose of the present invention is to provide a method and apparatus for obtaining high-quality silicon carbide single crystals with a large cross-sectional area by fixing the silicon carbide in S and suppressing the generation of polycrystals around the seed crystal substrate to grow only silicon carbide single crystals. do.
(課題を解決するための手段)
本発明は、黒鉛製るつぼ内に炭化珪素粉末を装填し不活
性気体雰囲気中で昇華させ、前記黒鉛製るつぼの蓋体内
面側中央部に垂下した種結晶載置部に設置した炭化珪素
種結晶基板上に炭化珪素単結晶を成長させる昇華再結晶
法において、前記種結晶載置部に少なくとも一条の凸部
を設け、炭化珪素種結晶基板裏面に前記凸部に合致すべ
く形成した少なくとも一条の溝に該凸部を挿入すること
によって該炭化珪素種結晶基板を保持することを特徴と
する炭化珪素単結晶!!遣方法、および、黒鉛製るつぼ
と蓋体と加熱部とから成り、該蓋体の内面側中央部に垂
下する種結晶載置部を設置し、該種結晶載置部に少なく
とも一条の凸部を設けたことを特徴とする炭化珪素単結
晶91逍装置である。(Means for Solving the Problems) The present invention involves loading silicon carbide powder into a graphite crucible, sublimating it in an inert gas atmosphere, and placing a seed crystal hanging down at the center of the inner surface of the lid of the graphite crucible. In a sublimation recrystallization method in which a silicon carbide single crystal is grown on a silicon carbide seed crystal substrate placed in a placing part, at least one convex part is provided in the seed crystal placing part, and the convex part is provided on the back surface of the silicon carbide seed crystal substrate. A silicon carbide single crystal characterized in that the silicon carbide seed crystal substrate is held by inserting the convex portion into at least one groove formed to match the above! ! It consists of a graphite crucible, a lid body, and a heating part, and a seed crystal placement part that hangs down is installed at the center of the inner surface of the lid body, and at least one convex part is provided on the seed crystal placement part. This is a silicon carbide single crystal 91 application device characterized by being provided with.
前記製造方法においては、種結晶載置部の断面寸法より
大きな断面形状を有する炭化珪素種結晶基板を用いるこ
とが好ましい。In the manufacturing method, it is preferable to use a silicon carbide seed crystal substrate having a cross-sectional shape larger than the cross-sectional dimension of the seed crystal mounting portion.
(作用)
第1図に本発明の実施例の概略を示す、この装置は開口
部を有する黒鉛製るつば3と、その上部に設置された黒
鉛製の蓋体1と、炭化珪素種結晶基板2と、炭化珪素粉
末4と、図示されていない加熱部とから成る。蓋体1の
略中央部には種結晶載置ill! 1 aが垂下してい
る。第2図に示すように種結晶載置部1aにはさらに凸
部1bが加工されている。第3図に炭化珪素種結晶基板
2の裏面の概略を示す、sl結晶基板2には、例えば汎
用のダイヤモンド刃を有する結晶切断機を用いて?j1
2 aが容易に形成できる0種結晶基板2の溝2aの幅
および間隔は種結晶載82部1aの凸部1bの幅および
間隔に合致させて製作されているため、第1図に示すよ
うに種結晶基板2を種結晶載置部1&に容易に固定する
ことができる。また、黒鉛は加工が簡単で比較的弾力制
に富むため、容易に目的の凸部を製作することができる
。なお、ここでは凸部1bが二条ある場合を示したが、
−条でも良く、また必要に応じて三条以上の溝により、
同様の方法で種結晶基板を固定することができる。(Function) Fig. 1 shows an outline of an embodiment of the present invention. 2, silicon carbide powder 4, and a heating section (not shown). A seed crystal is placed approximately in the center of the lid body 1! 1 a is hanging down. As shown in FIG. 2, a convex portion 1b is further machined on the seed crystal mounting portion 1a. FIG. 3 schematically shows the back side of the silicon carbide seed crystal substrate 2, and the SL crystal substrate 2 is cut using, for example, a general-purpose crystal cutting machine with a diamond blade. j1
The width and spacing of the grooves 2a of the 0-seed crystal substrate 2, in which the grooves 2a can be easily formed, are made to match the width and spacing of the convex portions 1b of the seed crystal mounting 82 portion 1a, as shown in FIG. The seed crystal substrate 2 can be easily fixed to the seed crystal mounting portion 1&. In addition, since graphite is easy to process and has relatively high elasticity, desired convex portions can be easily manufactured. In addition, although the case where there are two convex portions 1b is shown here,
- grooves may be used, and if necessary, grooves of three or more grooves may be used.
A seed crystal substrate can be fixed in a similar manner.
さらに、種結晶載置部1aの蓋体外側面に平行な断面は
種結晶基板より僅かに小さく作製しておけば種結晶基板
表面近傍には黒鉛部分が存在せず、黒鉛上に成長する多
結晶の影響を受けずに種結晶上に単結晶のみを成長させ
ることが可能となる。Furthermore, if the cross section of the seed crystal placement part 1a parallel to the outer surface of the lid body is made slightly smaller than the seed crystal substrate, there will be no graphite portion near the surface of the seed crystal substrate, and polycrystals will grow on the graphite. It becomes possible to grow only a single crystal on a seed crystal without being affected by
この装置を使用して、不活性ガス分圧を5〜20 To
rr、種結晶載a!I!51aの温度を2000〜22
00℃、炭化珪素粉末の温度を2100〜2300℃に
3〜4時間保つことによって、直径15mm以上の大型
の炭化珪素単結晶を得ることができる。*た、種結晶基
板を固定する際、不必要な歪みの発生を避けることがで
きるため、成長結晶の品質が向上することとなる。Using this device, the inert gas partial pressure can be adjusted from 5 to 20 To
rr, seed crystal mounted a! I! 51a temperature from 2000 to 22
By maintaining the temperature of the silicon carbide powder at 00°C and 2100 to 2300°C for 3 to 4 hours, a large silicon carbide single crystal with a diameter of 15 mm or more can be obtained. *In addition, since unnecessary distortion can be avoided when fixing the seed crystal substrate, the quality of the grown crystal will be improved.
(実施例)
本発明を第1〜3図の装置を用いて実施した例を説明す
る。平行平板状の厚さ約lll11の炭化珪素種結晶基
板2の略中夫に種結晶載置部の凸部に合致すべく刃厚0
,45m+mのダイヤモンド刃を有する結晶切断機で深
さ約0 、5 aIllの溝2aを2mm隔てて二条形
成した。その後、種結晶基板2に有機洗浄、純水洗浄、
アルカリエツチング、酸エツチング等の表面処理を施し
た。一方、種結晶載置部1aに溝2aに対応した凸部1
bを形成した黒鉛製るつば系をあらかじめ約2400℃
で熱処理しておいた。黒鉛製るつば3に炭化珪素粉末4
を装填し、さらに種結晶基板2を、種結晶載置部1aの
凸部1bt−溝2aに挿入することにより設置した。(Example) An example in which the present invention was implemented using the apparatus shown in FIGS. 1 to 3 will be described. A blade with a thickness of 0 is provided approximately at the center of the parallel plate-shaped silicon carbide seed crystal substrate 2 having a thickness of approximately 1111 to match the convex portion of the seed crystal mounting portion.
, 45 m+m diamond blades were used to form two grooves 2a having depths of approximately 0.5 mm and 2 mm apart. After that, the seed crystal substrate 2 is subjected to organic cleaning, pure water cleaning,
Surface treatments such as alkali etching and acid etching were performed. On the other hand, a convex portion 1 corresponding to the groove 2a is provided on the seed crystal mounting portion 1a.
The graphite crucible system forming b is heated to approximately 2400℃ in advance.
It was heat treated. Silicon carbide powder 4 on graphite crucible 3
The seed crystal substrate 2 was installed by inserting the seed crystal substrate 2 into the protrusion 1bt-groove 2a of the seed crystal mounting portion 1a.
然るのち、反応容器中に黒鉛製るつぼ系を設置し、容器
内のアルゴンガス圧力を約10Torrに保ちながら、
炭化珪素粉末4を2300℃程度に加熱し、かつ種結晶
載置部1aの温度を2100〜2200℃となるように
温度勾配を設定して5時間結晶成長を行ったところ、種
結晶基板2上に直径1811厚さ10m+の炭化珪素単
結晶が1&艮した。After that, a graphite crucible system was installed in the reaction vessel, and while maintaining the argon gas pressure in the vessel at approximately 10 Torr,
When silicon carbide powder 4 was heated to about 2300°C and a temperature gradient was set so that the temperature of seed crystal mounting part 1a was 2100 to 2200°C, crystal growth was performed for 5 hours. A silicon carbide single crystal with a diameter of 1,811 mm and a thickness of 10 m+ was placed.
(発明の効果)
本発明によると、比較的簡単に種結晶基板を保持でさ、
かつ種結晶基板表面とその周囲に多結晶生成の原因とな
る黒鉛の露出部分を無くせるので、種結晶基板上に多結
晶の付着していない直径151以上の大断面積の炭化珪
素単結晶インゴットを1&長させることができ、炭化珪
素を用いた青色発光ダイオードや高温電子材料への応用
面に有効な大型炭化珪素単結晶ウェハの供給が可能とな
る。(Effects of the Invention) According to the present invention, the seed crystal substrate can be held relatively easily.
In addition, it is possible to eliminate exposed graphite parts on the seed crystal substrate surface and its surroundings that cause polycrystal formation, so a silicon carbide single crystal ingot with a large cross-sectional area of 151 mm or more in diameter and with no polycrystals attached on the seed crystal substrate can be produced. This makes it possible to supply large silicon carbide single crystal wafers that are effective for applications in blue light emitting diodes and high-temperature electronic materials using silicon carbide.
第1図は本発明の実施例を示す断面図、第2図は実施例
の種結晶載置部を示す斜視図、PIS3図は種結晶基板
裏面を示す斜視図、第4図は従来の装置を示す断面図、
第5図および第6図(a)、(b)は従来の種結晶基板
の固定方法を説明するための斜視図および断面図である
。
1・・・蓋体、1a・・・種結晶載置部、1b・・・凸
部、2・・・炭化珪素種結晶基板、2a・・・溝、3・
・・黒鉛製るつぼ、4・・・炭化珪素粉末、21・・・
黒鉛製るつぼ、22・・・炭化珪素粉末、23・・・長
体、23a・・・種結晶1a置部、24・・・炭化珪素
種結晶基板、25・・・黒鉛製り字部材、28・・・シ
リコン、29・・・炭化珪素。
代理人 弁理士 秋パ政光 他1名
24図
7i6図
(Q) Cb)Fig. 1 is a cross-sectional view showing an embodiment of the present invention, Fig. 2 is a perspective view showing the seed crystal placement part of the embodiment, PIS 3 is a perspective view showing the back side of the seed crystal substrate, and Fig. 4 is a conventional device. FIG. 5 and FIGS. 6(a) and 6(b) are a perspective view and a sectional view for explaining a conventional method of fixing a seed crystal substrate. DESCRIPTION OF SYMBOLS 1... Lid body, 1a... Seed crystal mounting part, 1b... Convex part, 2... Silicon carbide seed crystal substrate, 2a... Groove, 3...
...Graphite crucible, 4...Silicon carbide powder, 21...
Graphite crucible, 22... Silicon carbide powder, 23... Long body, 23a... Seed crystal 1a placement part, 24... Silicon carbide seed crystal substrate, 25... Graphite shaped member, 28 ...Silicon, 29...Silicon carbide. Agent Patent attorney Masamitsu Akipa and 1 other person 24 Figure 7i6 (Q) Cb)
Claims (3)
体雰囲気中で昇華させ、前記黒鉛製るつぼの蓋体内面側
中央部に垂下した種結晶載置部に設置した炭化珪素種結
晶基板上に炭化珪素単結晶を成長させる昇華再結晶法に
おいて、前記種結晶載置部に少なくとも一条の凸部を設
け、炭化珪素種結晶基板裏面に前記凸部に合致すべく形
成した少なくとも一条の溝に該凸部を挿入することによ
って該炭化珪素種結晶基板を保持することを特徴とする
炭化珪素単結晶製造方法。(1) Silicon carbide powder was loaded into a graphite crucible and sublimated in an inert gas atmosphere, and a silicon carbide seed crystal substrate was placed on a seed crystal placement part hanging down from the center of the inner surface of the lid of the graphite crucible. In a sublimation recrystallization method for growing a silicon carbide single crystal thereon, at least one convex portion is provided on the seed crystal mounting portion, and at least one groove is formed on the back surface of the silicon carbide seed crystal substrate to match the convex portion. A method for manufacturing a silicon carbide single crystal, comprising holding the silicon carbide seed crystal substrate by inserting the convex portion into the silicon carbide single crystal substrate.
する炭化珪素種結晶基板を用いることを特徴とする請求
項1記載の炭化珪素単結晶製造方法。(2) The method for producing a silicon carbide single crystal according to claim 1, characterized in that a silicon carbide seed crystal substrate having a cross-sectional shape larger than the cross-sectional dimension of the seed crystal mounting portion is used.
の内面側中央部に垂下する種結晶載置部を設置し、該種
結晶載置部に少なくとも一条の凸部を設けたことを特徴
とする炭化珪素単結晶製造装置。(3) Consisting of a graphite crucible, a lid body, and a heating part, a seed crystal placement part that hangs down is installed at the center of the inner surface of the lid body, and at least one convex part is provided on the seed crystal placement part. A silicon carbide single crystal manufacturing device characterized by:
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP13673688A JPH01305898A (en) | 1988-06-03 | 1988-06-03 | Method and apparatus for production of silicon carbide single crystal |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP13673688A JPH01305898A (en) | 1988-06-03 | 1988-06-03 | Method and apparatus for production of silicon carbide single crystal |
Publications (1)
Publication Number | Publication Date |
---|---|
JPH01305898A true JPH01305898A (en) | 1989-12-11 |
Family
ID=15182305
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP13673688A Pending JPH01305898A (en) | 1988-06-03 | 1988-06-03 | Method and apparatus for production of silicon carbide single crystal |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPH01305898A (en) |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2001004390A1 (en) * | 1999-07-07 | 2001-01-18 | Siemens Aktiengesellschaft | Seed crystal holder with a lateral border for an sic seed crystal |
JP2001072490A (en) * | 1999-08-30 | 2001-03-21 | Agency Of Ind Science & Technol | Growing apparatus for single crystal and production method |
US7045009B2 (en) | 2003-08-04 | 2006-05-16 | Denso Corporation | Method and apparatus for manufacturing single crystal |
-
1988
- 1988-06-03 JP JP13673688A patent/JPH01305898A/en active Pending
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2001004390A1 (en) * | 1999-07-07 | 2001-01-18 | Siemens Aktiengesellschaft | Seed crystal holder with a lateral border for an sic seed crystal |
US6723166B2 (en) | 1999-07-07 | 2004-04-20 | Siemens Aktiengesellschaft | Seed crystal holder with lateral mount for an SiC seed crystal |
JP2001072490A (en) * | 1999-08-30 | 2001-03-21 | Agency Of Ind Science & Technol | Growing apparatus for single crystal and production method |
JP4509258B2 (en) * | 1999-08-30 | 2010-07-21 | 独立行政法人産業技術総合研究所 | Single crystal growth apparatus and manufacturing method |
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