JP2006347868A - Apparatus and method of fixing seed crystal - Google Patents
Apparatus and method of fixing seed crystal Download PDFInfo
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- JP2006347868A JP2006347868A JP2006063036A JP2006063036A JP2006347868A JP 2006347868 A JP2006347868 A JP 2006347868A JP 2006063036 A JP2006063036 A JP 2006063036A JP 2006063036 A JP2006063036 A JP 2006063036A JP 2006347868 A JP2006347868 A JP 2006347868A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
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Abstract
Description
本発明は、反応容器の種結晶配置部に接着剤を介して種結晶を固定するための種結晶固定装置及び種結晶の固定方法に関する。 The present invention relates to a seed crystal fixing device and a seed crystal fixing method for fixing a seed crystal to a seed crystal arrangement part of a reaction vessel via an adhesive.
炭化ケイ素は、ケイ素に比し、バンドギャップが大きく、絶縁破壊特性、耐熱性、耐放射線性等に優れることから、小型で高出力の半導体等の電子デバイス材料として注目されている。また、光学的特性に優れることから光学デバイス材料としても注目されてきている。かかる炭化ケイ素の結晶の中でも、炭化ケイ素単結晶は、炭化ケイ素多結晶に比し、ウェハ等のデバイスに応用した際にウェハ内特性の均一性等に特に優れるという利点がある。 Silicon carbide is attracting attention as a small and high-power electronic device material such as a semiconductor because it has a larger band gap and is superior in dielectric breakdown characteristics, heat resistance, radiation resistance, and the like. In addition, it has attracted attention as an optical device material because of its excellent optical characteristics. Among such silicon carbide crystals, a silicon carbide single crystal has an advantage that it is particularly excellent in uniformity of characteristics within a wafer when applied to a device such as a wafer, compared to a silicon carbide polycrystal.
この炭化ケイ素単結晶の製造方法の1つとして、反応容器(坩堝)内の第一端部に昇華用原料を収容し、上記反応容器内の昇華用原料に略対向する第二端部(種結晶配置部)に炭化ケイ素単結晶の種結晶を配置し、昇華させた昇華用原料を上記種結晶上に再結晶させて炭化ケイ素単結晶を成長させる改良レイリー法がある。 As one method for producing this silicon carbide single crystal, a sublimation raw material is accommodated in a first end portion in a reaction vessel (crucible), and a second end portion (seed) that substantially faces the sublimation raw material in the reaction vessel. There is an improved Rayleigh method in which a silicon carbide single crystal seed crystal is arranged in the crystal arrangement portion), and the sublimated raw material for sublimation is recrystallized on the seed crystal to grow a silicon carbide single crystal.
改良レイリー法において、種結晶配置部に種結晶が完全に接着していない状態で種結晶を成長させると、完全に接着していない部分の種結晶配置部側から種結晶を貫通して成長結晶内にまでマクロ欠陥(空洞欠陥)が発生しウェハの品質を損ねる傾向があった。また接着剤が高温下ではガス化してこれが気泡として接着剤層内に残留することも品質の低下の発生原因として考えられていた。 In the modified Rayleigh method, when a seed crystal is grown in a state where the seed crystal is not completely adhered to the seed crystal arrangement portion, the crystal grown through the seed crystal from the seed crystal arrangement portion side of the portion not completely adhered There was a tendency for the macro defect (cavity defect) to occur inside and to deteriorate the quality of the wafer. Further, it has been considered that the adhesive is gasified at a high temperature and remains as bubbles in the adhesive layer as a cause of the deterioration of quality.
上記課題を解決する手段としていくつかの技術が提案されている(例えば、特許文献1、2参照。)。例えば特許文献1には、所定の圧力をかけて固定する固定方法が開示されている。また特許文献2には重石を種結晶の上に載せて圧着する固定方法が開示されている。 Several techniques have been proposed as means for solving the above problems (see, for example, Patent Documents 1 and 2). For example, Patent Literature 1 discloses a fixing method in which a predetermined pressure is applied for fixing. Patent Document 2 discloses a fixing method in which a weight is placed on a seed crystal and pressure-bonded.
しかし、機械的圧着法では種結晶表面に微細な凸凹が生じるため、種結晶の全表面を均等に圧着することが困難であった。また、重りによる圧着も同様に均等に圧着させることが困難であった。
種結晶配置部に対して種結晶表面を均等に圧着する種結晶固定方法及び種結晶固定装置が求められていた。 There has been a demand for a seed crystal fixing method and a seed crystal fixing device that uniformly press-bond the seed crystal surface to the seed crystal arrangement portion.
即ち、本発明は、以下の記載事項に関する。
(1)反応容器の種結晶配置部に接着剤を介して種結晶を固定するための種結晶固定装置であって、
上記種結晶配置部を内部に配置可能とし密閉雰囲気を形成するチャンバーと、
上前記チャンバーに接続され前記チャンバー内に減圧雰囲気を形成する吸引機と、
を備えることを特徴とする種結晶固定装置。
(2)上記接着剤を加熱硬化させる加熱体を有する上記(1)記載の種結晶固定装置。
(3)上記チャンバーは、上記種結晶配置部を固定すると共に上記種結晶を固定するガイドを有する上記(1)又は(2)記載の種結晶固定装置。
(4)上記ガイドは、上記種結晶の側面と少なくとも3点で接する上記(3)記載の種結晶固定装置。
(5)接着剤を介して種結晶が設けられた種結晶配置部を密閉雰囲気内に配置する工程と、
上記密閉雰囲気内に減圧雰囲気を形成する工程と、
を含むことを特徴とする種結晶固定方法。
(6)上記減圧雰囲気は300Torr以下である上記(5)記載の種結晶固定方法。
(7)上記減圧工程後、上記接着剤を加熱硬化させる工程を有する上記(5)又は(6)に記載の種結晶固定方法。
(8)加熱温度は100〜1000℃である上記(7)記載の種結晶固定方法。
That is, the present invention relates to the following description items.
(1) A seed crystal fixing device for fixing a seed crystal to the seed crystal arrangement part of the reaction vessel via an adhesive,
A chamber capable of arranging the seed crystal arrangement portion inside to form a sealed atmosphere;
A suction machine connected to the chamber to form a reduced pressure atmosphere in the chamber;
A seed crystal fixing device comprising:
(2) The seed crystal fixing device according to (1), further including a heating body that heats and cures the adhesive.
(3) The seed crystal fixing device according to (1) or (2), wherein the chamber includes a guide for fixing the seed crystal arrangement portion and fixing the seed crystal.
(4) The seed crystal fixing device according to (3), wherein the guide contacts the side surface of the seed crystal at least at three points.
(5) a step of arranging a seed crystal arrangement part provided with a seed crystal through an adhesive in a sealed atmosphere;
Forming a reduced pressure atmosphere in the sealed atmosphere;
A seed crystal fixing method comprising the steps of:
(6) The seed crystal fixing method according to (5), wherein the reduced-pressure atmosphere is 300 Torr or less.
(7) The seed crystal fixing method according to (5) or (6), further including a step of heat-curing the adhesive after the pressure reducing step.
(8) The seed crystal fixing method according to (7), wherein the heating temperature is 100 to 1000 ° C.
種結晶配置部に対して種結晶表面を均等に圧着でき、再現性のある種結晶固定方法及び種結晶固定装置を提供する。 Provided is a reproducible seed crystal fixing method and seed crystal fixing apparatus that can uniformly press-bond a seed crystal surface to a seed crystal arrangement part.
以下に実施形態を挙げて本発明を説明するが、本発明が以下の実施形態に限定されないことはいうまでもない。尚、図中同一の機能用途を有するものについては同一または同様の符号を付して説明を省略する。 Hereinafter, the present invention will be described with reference to embodiments, but it goes without saying that the present invention is not limited to the following embodiments. In addition, about the thing which has the same function use in a figure, the same or similar code | symbol is attached | subjected and description is abbreviate | omitted.
(種結晶固定装置)
図1(a)は、接着剤5を介して種結晶9が配置された種結晶配置部3を収納した種結晶固定装置1の概略断面図を示し、図1(b)は下チャンバーの上面図を示す。図1(a)に示すように、実施形態にかかる種結晶固定装置1は、反応容器の種結晶配置部3に接着剤5を介して種結晶9を固定するための種結晶固定装置であって、種結晶配置部3を内部に配置可能とし密閉雰囲気を形成するチャンバー10と、チャンバー10に接続されチャンバー10内に減圧雰囲気を形成する吸引機19と、を備える。種結晶固定装置1は、さらに接着剤を加熱硬化させる加熱体20を有する。
(Seed crystal fixing device)
FIG. 1A shows a schematic cross-sectional view of a seed crystal fixing device 1 in which a seed crystal placement unit 3 in which a seed crystal 9 is placed via an adhesive 5 is housed, and FIG. 1B shows an upper surface of a lower chamber. The figure is shown. As shown in FIG. 1 (a), a seed crystal fixing device 1 according to the embodiment is a seed crystal fixing device for fixing a seed crystal 9 to a seed crystal placement portion 3 of a reaction vessel via an adhesive 5. The chamber 10 includes a chamber 10 in which the seed crystal disposition unit 3 can be disposed, and a sealed atmosphere. The suction device 19 is connected to the chamber 10 and forms a decompressed atmosphere in the chamber 10. The seed crystal fixing device 1 further includes a heating body 20 that heats and cures the adhesive.
チャンバー10は、着脱自在に形成された上チャンバー11と下チャンバー13とからなり、使用の際に上チャンバー11を下チャンバー13の外周に配置されたOリング15を挟んで下チャンバー13に装着することにより密閉雰囲気が形成されるように構成されている。チャンバー10には吸引排気口12が設けられており、密閉雰囲気が形成されたチャンバー10内から吸引機19により空気を吸引することで減圧雰囲気が形成される。また下チャンバー13は、図1(a)(b)に示すように、種結晶配置部3を固定すると共に種結晶9を固定するガイド17を有する。種結晶配置部3を下チャンバー13に収納した後に、ガイド17が下チャンバー13に着脱自在に固定され、そして種結晶9が種結晶配置部3上に配置される。 The chamber 10 includes an upper chamber 11 and a lower chamber 13 that are detachably formed. When the chamber 10 is used, the upper chamber 11 is attached to the lower chamber 13 with an O-ring 15 disposed on the outer periphery of the lower chamber 13 interposed therebetween. Thus, a sealed atmosphere is formed. A suction exhaust port 12 is provided in the chamber 10, and a vacuum atmosphere is formed by sucking air from the inside of the chamber 10 in which a sealed atmosphere is formed by a suction device 19. Moreover, the lower chamber 13 has a guide 17 for fixing the seed crystal 9 and fixing the seed crystal 9 as shown in FIGS. After the seed crystal placement unit 3 is stored in the lower chamber 13, the guide 17 is detachably fixed to the lower chamber 13, and the seed crystal 9 is placed on the seed crystal placement unit 3.
ガイド17は、種結晶9の側面に3点以上の点で接していることが好ましい。種結晶9からはみ出した接着剤5がガイド17に付着固化し、ガイド17から種結晶9が剥がれなくなることを防止するためである。具体的には図5(b)に示すように、ガイド171につめ171a〜171dを設けかかる4点で種結晶9を保持することができる。つめ171a〜171dの形状は図5(b)の上面図に示されるような半円形に限定されない。したがって種結晶9との当接点に向かって先が細くなるような略正三角形状であっても構わない。またガイド17の表面にはフッ素樹脂(テフロン(登録商標))コーティングされているのが好ましい。このテフロン(登録商標)コーティングはガイド17のつめ171a〜171dの表面にのみに施されていればよいが、ガイド17の全面に施されていても構わない。 The guide 17 is preferably in contact with the side surface of the seed crystal 9 at three or more points. This is to prevent the adhesive 5 protruding from the seed crystal 9 from adhering and solidifying to the guide 17 and preventing the seed crystal 9 from peeling off from the guide 17. Specifically, as shown in FIG. 5 (b), the guide 171 is provided with claws 171a to 171d, and the seed crystal 9 can be held at these four points. The shape of the pawls 171a to 171d is not limited to a semicircular shape as shown in the top view of FIG. Therefore, it may be a substantially equilateral triangle shape that tapers toward the contact point with the seed crystal 9. The surface of the guide 17 is preferably coated with a fluororesin (Teflon (registered trademark)). The Teflon (registered trademark) coating may be applied only to the surfaces of the claws 171 a to 171 d of the guide 17, but may be applied to the entire surface of the guide 17.
種結晶固定装置1に収容される種結晶配置部3としては、例えば後に説明する図3に示す炭化ケイ素単結晶製造装置30の種結晶配置部3を用いることができる。種結晶9としては、使用目的により適宜定まるが、6Hのレーリー結晶、6Hのアチソン結晶等を用いることができる。接着剤5としては、樹脂、炭水化物、耐熱性微粒子が挙げられる。樹脂としては、熱硬化性樹脂、例えばフェノール樹脂、ノボラック樹脂、フルフリルアルコール樹脂等を用いることができる。フェノール樹脂にカーボン粉末を混入したものを用いることもできる。炭水化物としては、糖類、例えばグルコースのような単糖類及びセルロースのような多糖類並びにそれらの誘導体を使用することができる。耐熱性微粒子としては、黒鉛(炭素)の他、炭化ケイ素(SiC)、窒化ホウ素(BN)等の耐熱物や、タングステン、タンタル等の高融点金属及びそれらの化合物例えば炭化物や窒化物を使用することができる。 As seed crystal arrangement part 3 accommodated in seed crystal fixing device 1, for example, seed crystal arrangement part 3 of silicon carbide single crystal manufacturing apparatus 30 shown in FIG. 3 described later can be used. The seed crystal 9 is appropriately determined depending on the purpose of use, but 6H Rayleigh crystal, 6H Atchison crystal, or the like can be used. Examples of the adhesive 5 include resins, carbohydrates, and heat-resistant fine particles. As the resin, a thermosetting resin such as a phenol resin, a novolac resin, a furfuryl alcohol resin, or the like can be used. It is also possible to use a phenol resin mixed with carbon powder. As the carbohydrate, saccharides such as monosaccharides such as glucose and polysaccharides such as cellulose and derivatives thereof can be used. As heat-resistant fine particles, in addition to graphite (carbon), heat-resistant materials such as silicon carbide (SiC) and boron nitride (BN), refractory metals such as tungsten and tantalum, and compounds thereof such as carbides and nitrides are used. be able to.
(種結晶固定方法)
図1の種結晶固定装置を用いた実施形態にかかる種結晶固定方法について、図2(a)〜(g)を用いて説明する。
(Seed crystal fixation method)
A seed crystal fixing method according to the embodiment using the seed crystal fixing device of FIG. 1 will be described with reference to FIGS.
(イ)まず、図2(a)に示すように下チャンバー13を用意する。
(ロ)次に、図2(b)に示すように下チャンバー13内に反応容器の種結晶配置部3を配置する。
(ハ)そして、図2(c)に示すように種結晶配置部3をガイド17で固定する。
(A) First, the lower chamber 13 is prepared as shown in FIG.
(B) Next, as shown in FIG. 2 (b), the seed crystal arrangement part 3 of the reaction vessel is arranged in the lower chamber 13.
(C) Then, as shown in FIG. 2 (c), the seed crystal arrangement part 3 is fixed by the guide 17.
(ニ)図2(d)に示すように接着剤5を種結晶配置部3上に塗布する。塗布量は1μl/cm2〜25μl/cm2が好ましい。
(ホ)次に、図2(e)に示すように種結晶9を接着剤5を介して種結晶配置部3上に配置する。接着性を向上させる観点からは、種結晶9の種結晶配置部3への接触面を研磨しておくことが好ましい。具体的には種結晶9の接触面の表面粗さ(Ra)は0.1μm以下が好ましい。また種結晶配置部3の種結晶9配置面の表面粗さ(Ra)を1.4μm以下とすると接着性が向上する点で好ましい。
(D) As shown in FIG. 2 (d), the adhesive 5 is applied onto the seed crystal arrangement part 3. The coating amount is preferably from 1μl / cm 2 ~25μl / cm 2 .
(E) Next, as shown in FIG. 2 (e), the seed crystal 9 is arranged on the seed crystal arrangement part 3 through the adhesive 5. From the viewpoint of improving adhesiveness, it is preferable to polish the contact surface of the seed crystal 9 with the seed crystal arrangement portion 3 in advance. Specifically, the surface roughness (Ra) of the contact surface of the seed crystal 9 is preferably 0.1 μm or less. Further, it is preferable that the surface roughness (Ra) of the seed crystal 9 arrangement surface of the seed crystal arrangement part 3 is 1.4 μm or less from the viewpoint of improving the adhesiveness.
(ヘ)図2(f)に示すように下チャンバー13に上チャンバー11を装着して密閉雰囲気を形成する。
(ト)チャンバー10内から吸引機19により空気を吸引して減圧雰囲気を形成する。この減圧雰囲気は300Torr以下であることが好ましい。
(F) As shown in FIG. 2F, the upper chamber 11 is attached to the lower chamber 13 to form a sealed atmosphere.
(G) A vacuum atmosphere is formed by sucking air from the chamber 10 by the suction machine 19. The reduced pressure atmosphere is preferably 300 Torr or less.
(チ)加熱体20により加熱して接着剤5を硬化させる。加熱条件は接着剤(熱硬化性樹脂)の性質等に依るが、100℃〜1000℃、好ましくは100℃〜300℃で、5分〜10分程度である。 (H) The adhesive 5 is cured by heating with the heating body 20. The heating conditions depend on the properties of the adhesive (thermosetting resin) and the like, but are 100 ° C. to 1000 ° C., preferably 100 ° C. to 300 ° C., for about 5 minutes to 10 minutes.
ここで、接着剤5を硬化させる際に生じるガスが種結晶9と種結晶配置部3の間に気泡として残るとそれが原因となって接着ムラが生じるおそれがある。そのため、吸引排気口12に接続された吸引機19を用いてチャンバー10内から大気や接着ムラの原因と考えられるガスを吸引して減圧雰囲気を形成しながら加熱硬化することが好ましい。減圧雰囲気を形成することで種結晶9に荷重される圧力の均一性の向上の効果も得られる。即ち、常に同一の条件で接着することにより接着性の再現性が向上する。この減圧雰囲気は300Torr以下であることが好ましい。以上により種結晶9が種結晶配置部3上に固定される。 Here, if the gas generated when the adhesive 5 is cured remains as bubbles between the seed crystal 9 and the seed crystal disposition portion 3, it may cause adhesion unevenness. Therefore, it is preferable to heat and cure while forming a reduced-pressure atmosphere by sucking air or gas considered to be the cause of adhesion unevenness from the inside of the chamber 10 using the suction device 19 connected to the suction exhaust port 12. By forming the reduced pressure atmosphere, the effect of improving the uniformity of the pressure applied to the seed crystal 9 can also be obtained. That is, the reproducibility of adhesiveness is improved by always bonding under the same conditions. The reduced pressure atmosphere is preferably 300 Torr or less. The seed crystal 9 is fixed on the seed crystal arrangement part 3 by the above.
(炭化ケイ素単結晶の製造方法)
以上種結晶固定方法等について説明してきたが、本発明の別形態として炭化ケイ素単結晶の製造方法が提供される。即ち、昇華用原料を収容する反応容器に昇華用原料を収容し、昇華用原料に略対向して種結晶を配置し、昇華させた昇華用原料を種結晶上に再結晶させて炭化ケイ素単結晶を成長させる炭化ケイ素単結晶の製造方法であって、上記実施形態にかかる種結晶固定方法により種結晶配置部に固定された種結晶上に単結晶を成長させる炭化ケイ素単結晶の製造方法が提供される。
(Method for producing silicon carbide single crystal)
Although the seed crystal fixing method and the like have been described above, a method for producing a silicon carbide single crystal is provided as another embodiment of the present invention. In other words, a sublimation raw material is contained in a reaction vessel containing a sublimation raw material, a seed crystal is disposed substantially opposite to the sublimation raw material, and the sublimated sublimation raw material is recrystallized on the seed crystal to obtain silicon carbide single A method for manufacturing a silicon carbide single crystal for growing a crystal, the method for manufacturing a silicon carbide single crystal for growing a single crystal on a seed crystal fixed to a seed crystal arrangement portion by the seed crystal fixing method according to the above embodiment. Provided.
反応容器としては、図3に示すように、昇華用原料35を収容可能とする反応容器本体31と、反応容器本体31に着脱自在に取り付けられると共に種結晶9を配置可能とする種結晶配置部3と、を有する炭化ケイ素単結晶製造装置30が用いられる。反応容器の外周には炭化ケイ素の昇華雰囲気を形成するための第一誘導加熱コイル33a、第二誘導加熱コイル33bが設けられている。反応容器本体31としては、反応容器本体31内部に炭化ケイ素の昇華雰囲気を形成できるものであれば特に制限はない。反応容器本体31としては例えば坩堝を用いることができるが、その材質は黒鉛であることが好ましく、熱膨張係数が種結晶と略同一であるものがさらに好ましい。昇華用原料35を収納しやすくする観点から、反応容器本体31と、種結晶配置部3は着脱自在に一体に形成されていることが好ましい。接合手段としては、反応容器本体31内部の密閉性が保たれるのであればいずれの接合手段を用いても構わない。接合手段としては、螺合手段が挙げられる。 As shown in FIG. 3, the reaction vessel includes a reaction vessel main body 31 that can accommodate the sublimation raw material 35, and a seed crystal placement unit that is detachably attached to the reaction vessel main body 31 and can place the seed crystal 9. 3 is used. A first induction heating coil 33a and a second induction heating coil 33b for forming a silicon carbide sublimation atmosphere are provided on the outer periphery of the reaction vessel. The reaction vessel body 31 is not particularly limited as long as it can form a silicon carbide sublimation atmosphere inside the reaction vessel body 31. For example, a crucible can be used as the reaction vessel main body 31, and the material thereof is preferably graphite, and further preferably has a thermal expansion coefficient substantially the same as that of the seed crystal. From the viewpoint of easy storage of the sublimation raw material 35, it is preferable that the reaction vessel main body 31 and the seed crystal arrangement portion 3 are integrally formed detachably. As the joining means, any joining means may be used as long as the airtightness inside the reaction vessel main body 31 is maintained. Examples of the joining means include screwing means.
昇華用原料35としては従来公知の材料を用いることができる。昇華用原料35としては、例えば高純度のテトラエトキシシラン重合体をケイ素源とし、レゾール型フェノール樹脂を炭素源とし、これらを均一に混合して得た混合物をアルゴン雰囲気下で加熱焼成して得られた炭化ケイ素粉末を用いることができる。また炭化ケイ素単結晶の種結晶としては、従来公知の単結晶を用いることができる。 A conventionally known material can be used as the sublimation raw material 35. As the sublimation raw material 35, for example, a high purity tetraethoxysilane polymer is used as a silicon source, a resol type phenol resin is used as a carbon source, and a mixture obtained by uniformly mixing these is heated and fired in an argon atmosphere. The silicon carbide powder obtained can be used. A conventionally known single crystal can be used as the seed crystal of the silicon carbide single crystal.
昇華用原料35の加熱温度等の加熱条件は、特に制限されることなく周知の技術に基づいて当業者により適宜設定されうる。 The heating conditions such as the heating temperature of the sublimation raw material 35 are not particularly limited, and can be appropriately set by those skilled in the art based on known techniques.
(炭化ケイ素単結晶)
炭化ケイ素単結晶は、前述の炭化ケイ素単結晶の製造方法により製造される。炭化ケイ素単結晶は、溶融アルカリによりエッチングして評価した結晶欠陥(パイプ欠陥)は、50個/cm2以下が好ましく、10個/cm2以下がより好ましい。炭化ケイ素単結晶における金属不純物元素の総含有量としては10ppm以下が好ましい。本発明により得られる炭化ケイ素単結晶は、多結晶や多型の混入やマイクロパイプ等の結晶欠陥がなく、極めて高品質であるので、絶縁破壊特性、耐熱性、耐放射線性等に優れ、半導体ウエハ等の電子デバイス、発光ダイオード等の光学デバイスなどに特に好適に用いられる。
以上、本発明の炭化ケイ素単結晶製造方法によると、高品質な炭化ケイ素単結晶を効率よく、かつ割れ等の破損がない状態で容易に製造することができる。
(Silicon carbide single crystal)
The silicon carbide single crystal is manufactured by the above-described method for manufacturing a silicon carbide single crystal. The silicon carbide single crystal has a crystal defect (pipe defect) evaluated by etching with molten alkali of preferably 50 pieces / cm 2 or less, and more preferably 10 pieces / cm 2 or less. The total content of metal impurity elements in the silicon carbide single crystal is preferably 10 ppm or less. The silicon carbide single crystal obtained by the present invention is free from crystal defects such as polycrystals, polymorphs, and micropipes, and is extremely high quality. Therefore, the silicon carbide single crystal is excellent in dielectric breakdown characteristics, heat resistance, radiation resistance, etc. It is particularly suitably used for electronic devices such as wafers and optical devices such as light emitting diodes.
As described above, according to the method for producing a silicon carbide single crystal of the present invention, a high-quality silicon carbide single crystal can be produced efficiently and easily without breakage such as cracks.
(実施例)
図1の種結晶固定装置を用いて、実施形態にかかる種結晶固定方法に準じて、種結晶9を種結晶配置部3に固定した。その際、接着剤5としてフェノール樹脂を7.5μl/cm2で塗布した。種結晶9として種結晶厚0.4mm、直径50mmの6Hのレーリー結晶を用いた。そして減圧下(30Torr)において、15分かけて90℃まで加熱しさらに90℃で2分間予備加熱を行った後、25分かけて160℃まで加熱した後160℃で10分間加熱することにより加熱硬化を行った。
その結果、図4(b)の種結晶の表面観察写真に示すように、実施例の種結晶9が接着ムラなく接着されたことが確認された。
(Example)
The seed crystal 9 was fixed to the seed crystal arrangement part 3 in accordance with the seed crystal fixing method according to the embodiment using the seed crystal fixing device of FIG. At that time, phenol resin was applied as an adhesive 5 at 7.5 μl / cm 2 . As the seed crystal 9, a 6H Rayleigh crystal having a seed crystal thickness of 0.4 mm and a diameter of 50 mm was used. Then, under reduced pressure (30 Torr), after heating to 90 ° C. over 15 minutes and further preheating at 90 ° C. for 2 minutes, heating to 160 ° C. over 25 minutes and then heating at 160 ° C. for 10 minutes. Curing was performed.
As a result, as shown in the surface observation photograph of the seed crystal of FIG. 4B, it was confirmed that the seed crystal 9 of the example was adhered without adhesion unevenness.
さらに、種結晶9が固定された種結晶配置部3を図3の炭化ケイ素単結晶製造装置30に装着して炭化ケイ素単結晶を成長させた。昇華用原料35は、高純度のテトラエトキシシラン重合体をケイ素源とし、レゾール型フェノール樹脂を炭素源とし、これらを均一に混合して得た混合物をアルゴン雰囲気下で加熱焼成して得られた炭化ケイ素粉末(6H(一部3Cを含む)、平均粒径が200μm)を用いた。炭化ケイ素単結晶製造装置30において、第一誘導加熱コイル33aに電流を通電させこれを加熱しその熱で昇華用原料35を加熱した。その際反応容器本体31の底部を2350℃にまで加熱した後、アルゴンガス雰囲気で圧力を50Torr(6645Pa)に維持した。昇華用原料35は、所定の温度(2540℃)にまで加熱されて昇華した。一方、種結晶配置部3側は、第二誘導加熱コイル33bにより加熱した。第二誘導加熱コイル33bによる種結晶配置部3の設定温度は2300℃であった。
得られた炭化ケイ素単結晶のウェハ断面を観察したところ(図4(b))、種結晶直上の全面のマクロ欠陥の数は10個以下であり、種結晶から10mm上のウェハ全面のマクロ欠陥の数は0個であった。また、欠陥の大きさは従来法により得られるものよりも小さかった。
Furthermore, the seed crystal arrangement part 3 to which the seed crystal 9 was fixed was mounted on the silicon carbide single crystal manufacturing apparatus 30 of FIG. 3 to grow a silicon carbide single crystal. The sublimation raw material 35 was obtained by heating and baking a mixture obtained by uniformly mixing a high purity tetraethoxysilane polymer as a silicon source and a resol type phenol resin as a carbon source in an argon atmosphere. Silicon carbide powder (6H (including part of 3C), average particle diameter of 200 μm) was used. In the silicon carbide single crystal manufacturing apparatus 30, a current was passed through the first induction heating coil 33a to heat it, and the sublimation raw material 35 was heated with the heat. At that time, after the bottom of the reaction vessel main body 31 was heated to 2350 ° C., the pressure was maintained at 50 Torr (6665 Pa) in an argon gas atmosphere. The sublimation raw material 35 was heated to a predetermined temperature (2540 ° C.) and sublimated. On the other hand, the seed crystal arrangement part 3 side was heated by the second induction heating coil 33b. The set temperature of the seed crystal arrangement part 3 by the second induction heating coil 33b was 2300 ° C.
When the wafer cross section of the obtained silicon carbide single crystal was observed (FIG. 4B), the number of macro defects on the entire surface immediately above the seed crystal was 10 or less, and the macro defects on the entire surface of the wafer 10 mm above the seed crystal. The number of was zero. Further, the size of the defect was smaller than that obtained by the conventional method.
(比較例)
図6に示すように、載置台101に種結晶配置部103を配置し、その上に接着剤(フェノール樹脂)105を介して種結晶109を配置した。そして、重石107を種結晶109の上に配置して、重石107により種結晶109に荷重を加えながら、大気圧下300℃で0.5時間フェノール樹脂の加熱硬化を行った。その結果、図4(a)の種結晶の表面観察写真に示すように、比較例の種結晶109の表面に接着ムラが確認された。
得られた種結晶109を用いて実施例と同様にして炭化ケイ素単結晶を成長させた。
得られた炭化ケイ素単結晶の側面断面図を観察したところ(図4(a))、種結晶直上の全面のマクロ欠陥の数は100個以下であり、種結晶から10mm上のウェハ全面のマクロ欠陥の数は10〜20個であった。マクロ欠陥の大きさは実施例よりも大きかった。
(Comparative example)
As shown in FIG. 6, a seed crystal placement unit 103 was placed on the mounting table 101, and a seed crystal 109 was placed thereon via an adhesive (phenolic resin) 105. Then, the weight stone 107 was placed on the seed crystal 109, and the phenol resin was heat-cured at 300 ° C. for 0.5 hours under atmospheric pressure while applying a load to the seed crystal 109 with the weight stone 107. As a result, as shown in the surface observation photograph of the seed crystal in FIG. 4A, adhesion unevenness was confirmed on the surface of the seed crystal 109 of the comparative example.
Using the obtained seed crystal 109, a silicon carbide single crystal was grown in the same manner as in the example.
When the side sectional view of the obtained silicon carbide single crystal was observed (FIG. 4A), the number of macro defects on the entire surface immediately above the seed crystal was 100 or less, and the macro on the entire wafer surface 10 mm above the seed crystal. The number of defects was 10-20. The size of the macro defect was larger than that of the example.
1、101…種結晶固定装置
3、103…種結晶配置部
5、105…接着剤
9、109…種結晶
10…チャンバー
11…上チャンバー
13…下チャンバー
12…吸引排気口
15…Oリング
17…ガイド
19…吸引機
20…ヒータ(加熱体)
30…炭化ケイ素単結晶製造装置
31…反応容器本体
33a…第一誘導加熱コイル
33b…第二誘導加熱コイル
35…昇華用原料
107…重石
DESCRIPTION OF SYMBOLS 1,101 ... Seed crystal fixing device 3, 103 ... Seed crystal arrangement part 5, 105 ... Adhesive 9, 109 ... Seed crystal 10 ... Chamber 11 ... Upper chamber 13 ... Lower chamber 12 ... Suction exhaust port 15 ... O-ring 17 ... Guide 19 ... Suction machine 20 ... Heater (heating body)
30 ... Silicon carbide single crystal production apparatus 31 ... Reaction vessel body 33a ... First induction heating coil 33b ... Second induction heating coil 35 ... Sublimation raw material 107 ... Clay stone
Claims (8)
前記種結晶配置部を内部に配置可能とし密閉雰囲気を形成するチャンバーと、
前記チャンバーに接続され前記チャンバー内に減圧雰囲気を形成する吸引機と、
を備えることを特徴とする種結晶固定装置。 A seed crystal fixing device for fixing a seed crystal to the seed crystal arrangement part of the reaction vessel via an adhesive,
A chamber capable of arranging the seed crystal arrangement portion inside to form a sealed atmosphere;
A suction device connected to the chamber to form a reduced pressure atmosphere in the chamber;
A seed crystal fixing device comprising:
前記密閉雰囲気内に減圧雰囲気を形成する工程と、
を含むことを特徴とする種結晶固定方法。 Arranging the seed crystal placement portion provided with the seed crystal via an adhesive in a sealed atmosphere;
Forming a reduced pressure atmosphere in the sealed atmosphere;
A seed crystal fixing method comprising the steps of:
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