JP3532245B2 - Method for producing mixed crystal single crystal - Google Patents
Method for producing mixed crystal single crystalInfo
- Publication number
- JP3532245B2 JP3532245B2 JP14834194A JP14834194A JP3532245B2 JP 3532245 B2 JP3532245 B2 JP 3532245B2 JP 14834194 A JP14834194 A JP 14834194A JP 14834194 A JP14834194 A JP 14834194A JP 3532245 B2 JP3532245 B2 JP 3532245B2
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- Prior art keywords
- crystal
- mixed crystal
- single crystal
- mixed
- raw material
- 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.)
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- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Description
【０００１】[0001]
【産業上の利用分野】この発明は混晶単結晶体の製造方
法に関するものである。さらに詳しくは、この発明は、
化合物半導体デバイス等に有用な混晶単結晶体製造方法
に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a mixed crystal single crystal body. More specifically, the present invention is
The present invention relates to a method for producing a mixed crystal single crystal body useful for a compound semiconductor device or the like.
【０００２】[0002]
【従来の技術とその課題】化合物半導体は、ＬＥＤ，Ｌ
Ｄ，その他の電子デバイス等に使用されており、その進
歩には著しいものがある。これらのデバイスに使用され
ている基板結晶は、ＧａＡｓ，ＧａＰ，ＩｎＰ等の２元
化合物であるが、基板上に多元の混晶半導体結晶をエピ
タキシャル成長させたデバイスが多い。この場合、基板
結晶とエピタキシャル層との間の格子定数の不整合や熱
膨張係数の差より生ずる歪みによってデバイスの性能が
低下するという問題がある。2. Description of the Related Art Compound semiconductors are LEDs, L
It is used in D, other electronic devices, etc., and its progress has been remarkable. The substrate crystal used for these devices is a binary compound such as GaAs, GaP, InP, etc., but many devices are obtained by epitaxially growing a multi-element mixed crystal semiconductor crystal on the substrate. In this case, there is a problem that the device performance is deteriorated due to the strain caused by the mismatch of the lattice constant between the substrate crystal and the epitaxial layer and the difference in the coefficient of thermal expansion.
【０００３】このように、従来は、基板結晶によって、
エピタキシャル層の混晶組成が制約されるという問題を
抱えていたことから、これら問題のない混晶基板の開発
が強く望まれていた。一方、結晶体の製造方法として
は、従来より、Ｃｚ法、ゾーンレベリング法、ＦＺ法等
が知られている。As described above, conventionally, according to the substrate crystal,
Since there is a problem that the mixed crystal composition of the epitaxial layer is restricted, development of a mixed crystal substrate without these problems has been strongly desired. On the other hand, the Cz method, the zone leveling method, the FZ method and the like have been conventionally known as a method for producing a crystal body.
【０００４】これらの従来法のうち、Ｃｚ法について
は、２元化合物単結晶の育成には適するが、混晶材料の
単結晶を育成する場合に、融液組成と結晶組成とが一致
しないこと、また結晶の成長方向に均一な組成になるよ
うに結晶成長させることが難しいことが知られている。
このため、最近になって、Ｃｚ法による混晶材料の単結
晶育成を可能とするために融液の添加方式の開発によっ
て、融液組成を一定に保つ方法が検討されている。しか
しながら、これらの方法を用いても、結晶体の製造装置
がさらに複雑となり、コストが高くなること、また、Ｃ
ｚ法による結晶組成の均一化が非常に難しい等の問題が
ある。Of these conventional methods, the Cz method is suitable for growing a binary compound single crystal, but when growing a single crystal of a mixed crystal material, the melt composition and the crystal composition do not match. Also, it is known that it is difficult to grow a crystal so as to have a uniform composition in the crystal growth direction.
Therefore, recently, in order to enable single crystal growth of a mixed crystal material by the Cz method, a method of maintaining a constant melt composition has been studied by developing a method of adding a melt. However, even if these methods are used, the apparatus for producing the crystal becomes more complicated and the cost becomes higher, and C
There is a problem that it is very difficult to make the crystal composition uniform by the z method.
【０００５】また、ゾーンレベリング法については、溶
媒の組成とその量の決定や原料棒−種間への溶媒となる
材料の固定が難しいこと、スタート時における溶媒のみ
の溶融が困難であること、また、種結晶の人手が難しい
等の問題があり、現在のところ、混晶材料のバルク単結
晶育成は困難である。以上のような問題に対し、ＦＺ
（浮遊帯域）法は、混晶化合物半導体基板の製造に比較
的向いているものと考えられるが、実際には、従来のＦ
Ｚ法を単に適用するだけでは種付けが難しく、成長方向
に混晶比の均一な単結晶を製造することは極めて困難で
ある。Further, in the zone leveling method, it is difficult to determine the composition and amount of the solvent, to fix the material to be the solvent between the raw material rod and the species, and to melt only the solvent at the start, Further, there are problems such as difficulty in manipulating the seed crystal, and at present, it is difficult to grow a bulk single crystal of a mixed crystal material. For the above problems, FZ
The (floating zone) method is considered to be relatively suitable for manufacturing a mixed crystal compound semiconductor substrate.
By simply applying the Z method, seeding is difficult, and it is extremely difficult to produce a single crystal having a uniform mixed crystal ratio in the growth direction.
【０００６】そこでこの発明は、以上の通りの事情に鑑
みてなされたものであって、従来技術の問題点を解決
し、結晶の成長方向に混晶比の均一な高品質な混晶単結
晶の製造を可能とする新しい方法を提供することを目的
としている。Therefore, the present invention has been made in view of the above circumstances, solves the problems of the prior art, and provides a high-quality mixed crystal single crystal having a uniform mixed crystal ratio in the crystal growth direction. It is intended to provide a new method that enables the manufacture of
【０００７】[0007]
【課題を解決するための手段】この発明は、上記の課題
を解決するものとして、蒸気圧制御による浮遊帯域結晶
製造において、軸方向に一端部から勾配をもって混晶比
が増加する勾配部とそれに続く定混晶比部とを有する混
晶多結晶体原料棒により種組成近傍側より成長させるこ
とを特徴とする混晶単結晶体製造方法を提供する。In order to solve the above problems, the present invention provides a gradient part in which a mixed crystal ratio increases with a gradient from one end in the axial direction in the production of a floating zone crystal by vapor pressure control, and A method for producing a mixed crystal single crystal body, which comprises growing the mixed crystal polycrystalline body raw material rod having a constant mixed crystal ratio part from the side near the seed composition.
【０００８】そしてまた、この発明は、原料棒がＧａ−
Ａｌ−Ａｓ組成を有し、ＧａＡｓ種結晶を用い、Ａｓ圧
下においてＧａ−Ａｌ−Ａｓ混晶単結晶体を成長させる
ことや、混晶比の勾配を０．１〜０．２／ｃｍとするこ
と等をその態様としてもいる。Further, according to the present invention, the raw material bar is Ga-
A GaAs seed crystal having an Al-As composition is used to grow a Ga-Al-As mixed crystal single crystal under As pressure, and a mixed crystal ratio gradient is set to 0.1 to 0.2 / cm. This is also the case.
【０００９】[0009]
【作用】この発明は上記の通り、混晶比の勾配部と平坦
部とからなる原料棒を用いることに本質的な特徴があ
る。この原料棒を使用して蒸気圧制御ＦＺ法により混晶
単結晶体を製造することになる。As described above, the present invention is essentially characterized by using a raw material rod having a mixed crystal ratio gradient portion and a flat portion. This raw material rod is used to manufacture a mixed crystal single crystal body by the vapor pressure controlled FZ method.
【００１０】つまり、この発明の混晶単結晶体の製造方
法は蒸気圧制御ＦＺ法において、原料棒の軸方向に混晶
比の勾配部を設けることによって種結晶の組成に近い側
より結晶成長を開始させることを特徴とする。この原料
棒を用いることによって溶媒と原料棒との一体化が可能
となり、また混晶を構成するひとつの２元化合物単結晶
を種として用いることができる等種付けが容易となる。
また種付け後溶融帯域を混晶比の勾配部を経て一定混晶
比部へと移動し所望の混晶比の単結晶を成長させるもの
であるが、この場合成長方向に沿って原料棒の融点、熱
膨張系数等はゆるやかに変化しているので溶融電力の調
整が容易で溶融帯を安定に保持でき、安定した条件下で
格子歪みの少ない単結晶を成長させることができる。That is, in the method for producing a mixed crystal single crystal of the present invention, in the vapor pressure controlled FZ method, a gradient portion of the mixed crystal ratio is provided in the axial direction of the raw material rod to grow crystals from the side closer to the composition of the seed crystal. It is characterized by starting. By using this raw material rod, the solvent and the raw material rod can be integrated, and one binary compound single crystal forming a mixed crystal can be used as a seed, which facilitates seeding.
Further, after seeding, the melting zone is moved to a constant mixed crystal ratio portion through a mixed crystal ratio gradient portion to grow a single crystal having a desired mixed crystal ratio.In this case, the melting point of the raw material rod is set along the growth direction. Since the coefficient of thermal expansion and the like are gradually changed, the melting power can be easily adjusted, the melting zone can be stably maintained, and a single crystal with less lattice strain can be grown under stable conditions.
【００１１】この時、原料棒の結晶成長開始端の組成
は、単結晶の組成に応じて決めることができる。また混
晶比の勾配は平坦部の混晶比、混晶を構成する元素の分
配系数、溶融帯幅、成長速度等によって適宜変えること
ができる。一般的には、低勾配にすると単結晶成長は容
易になるが、一定混晶比の単結晶の歩留まりが低下する
ことになる。At this time, the composition of the crystal growth start end of the raw material rod can be determined according to the composition of the single crystal. The gradient of the mixed crystal ratio can be appropriately changed depending on the mixed crystal ratio in the flat portion, the number of distribution systems of elements forming the mixed crystal, the melting zone width, the growth rate, and the like. Generally, a low gradient facilitates single crystal growth, but reduces the yield of single crystals with a constant mixed crystal ratio.
【００１２】一方で、高勾配になる程、また成長開始組
成が高混晶比になる程、種付け直後の単結晶成長が困難
となるため、この場合には分配係数に応じた低勾配の原
料棒あるいはまた低混晶比の種結晶を使用した方がよ
い。この発明の方法を用いる場合における望ましい混晶
比勾配は、０．１〜０．２／ｃｍである。On the other hand, the higher the gradient and the higher the mixed crystal ratio of the growth start composition, the more difficult it becomes to grow a single crystal immediately after seeding. In this case, therefore, the raw material having a low gradient corresponding to the distribution coefficient is obtained. It is better to use rods or also seed crystals with a low mixed crystal ratio. A desirable mixed crystal ratio gradient when the method of the present invention is used is 0.1 to 0.2 / cm.
【００１３】以下実施例を示し、さらに詳しくこの発明
を説明する。The present invention will be described in more detail with reference to the following examples.
【００１４】[0014]
【実施例】実施例１
この発明の混晶単結晶体の製造方法を用いて、混晶単結
晶体製造装置を作製した。図１は、混晶単結晶体製造装
置の断面図である。たとえばこの図１に例示したよう
に、混晶単結晶体製造装置には、耐圧容器（１）中に多
結晶体（６）と多結晶体を支持する支持棒（８）を取り
囲む石英管（２）が配設されており、その石英管（２）
の上下端にシール材（１３）を配設し、石英管（２）が
密封されている。 Example 1 An apparatus for producing a mixed crystal single crystal body was produced using the method for producing a mixed crystal single crystal body of the present invention. FIG. 1 is a sectional view of an apparatus for producing a mixed crystal single crystal body. For example, as illustrated in FIG. 1, in the mixed crystal single crystal body manufacturing apparatus, a quartz tube (6) surrounding a polycrystalline body (6) and a supporting rod (8) supporting the polycrystalline body in a pressure vessel (1) ( 2) is provided and its quartz tube (2)
Sealing materials (13) are arranged at the upper and lower ends of the quartz tube (2) to be sealed.
【００１５】石英管（２）内においては、多結晶（６）
を回転させる支持棒（８）が、多結晶と支持棒の接続部
（７）によって、多結晶（６）に接続されており、それ
らの多結晶（６）は、高周波誘導加熱コイル（１８）か
ら発する高周波によって、融液部（５）において単結晶
化され、単結晶（４）となる。その下部には、単結晶を
誘導するための種結晶（３）が接続されており、さらに
下部では、接続部（９）を経て、再び支持棒（１０）に
接続する。石英管（２）には、管内に蒸気を送るため
に、化合物半導体の成分元素のうち蒸発し易い方の元素
が収容された容器（１４）が設置されており、内部に蒸
発し易い元素である蒸発元素（１６）が収容される。In the quartz tube (2), the polycrystalline (6)
A support rod (8) for rotating the is connected to the polycrystal (6) by a connecting portion (7) between the polycrystal and the support rod, and the polycrystal (6) is a high frequency induction heating coil (18). Due to the high frequency emitted from the single crystal (4), it is single crystallized in the melt portion (5). A seed crystal (3) for inducing a single crystal is connected to the lower portion thereof, and further connected to the support rod (10) via the connecting portion (9) at the lower portion. The quartz tube (2) is provided with a container (14) accommodating an element that is more likely to evaporate among the constituent elements of the compound semiconductor in order to send vapor into the tube. A vaporizing element (16) is contained.
【００１６】蒸発元素収容器（１４）内の蒸発元素（１
６）は、蒸発容器加熱ヒータ（１７）で加熱されること
によって蒸発し、石英管接続パイプ（１５）を通って、
石英管（２）に注入される。また、石英管（２）は、上
部加熱ヒータ（１９）、下部加熱ヒータ（２０）、上部
シール部加熱ヒータ（２１）、下部シール部加熱ヒータ
（２２）によって加熱されている。The evaporation element (1) in the evaporation element container (14)
6) is evaporated by being heated by the evaporation container heater (17), passes through the quartz tube connection pipe (15),
It is poured into a quartz tube (2). The quartz tube (2) is heated by an upper heater (19), a lower heater (20), an upper seal heater (21) and a lower seal heater (22).
【００１７】耐圧容器（１）内は、加圧用ガス導入口
（２５）より加圧用ガス（２７）を導入し、圧力調整器
（２６）によって、内圧を監視し調整している。また多
結晶（６）の温度等の状態変化は、耐圧容器（１）に取
り付けられた、内部観察用窓（２３）を通して、温度計
（２４）によって、測定されている。そこで、この混晶
単結晶体製造装置を用いて、実際に、混晶単結晶の製造
を行う。蒸発元素には、砒素を用いる。A pressurizing gas (27) is introduced from the pressurizing gas inlet (25) into the pressure resistant container (1), and an internal pressure is monitored and adjusted by a pressure adjuster (26). The change in state of the polycrystal (6) such as temperature is measured by a thermometer (24) through an internal observation window (23) attached to the pressure vessel (1). Therefore, the mixed crystal single crystal is actually manufactured using this mixed crystal single crystal manufacturing apparatus. Arsenic is used as the evaporation element.
【００１８】単結晶製造の条件は、種結晶に直径１３ｍ
ｍのＧａＡｓを用い、原料棒には、直径１４ｍｍのＧａ
(1-x) Ａｌx Ａs を用いた。この例で用いた原料多結晶
の混晶比は、最大０．１５であり、原料棒軸線方向の起
点における混晶比を０とし、軸線方向の原料棒の長さ
は、１．５ｃｍとしたので、混晶比勾配は、０．１／ｃ
ｍとなる。また、単結晶の成長条件は、砒素圧を約１気
圧とし、溶融帯幅を約４．０ｍｍ、成長速度は結晶開始
時には、１．５ｍｍ／ｍｉｎとし、勾配部は徐々に速度
を遅くするようにした。さらに定混晶比部での速度は、
０．５ｍｍ／ｍｉｎとした。The condition for producing a single crystal is that the seed crystal has a diameter of 13 m.
m of GaAs is used, and the raw material rod is made of Ga having a diameter of 14 mm.
Using (1-x) Al x A s. The mixed crystal ratio of the raw material polycrystal used in this example was 0.15 at maximum, the mixed crystal ratio at the starting point in the raw material rod axial direction was 0, and the length of the raw material rod in the axial direction was 1.5 cm. Therefore, the mixed crystal ratio gradient is 0.1 / c
m. The growth conditions for the single crystal were as follows: the arsenic pressure was about 1 atm, the melting zone width was about 4.0 mm, the growth rate was 1.5 mm / min at the start of crystallization, and the gradient portion was gradually slowed down. I chose Furthermore, the speed in the constant mixed crystal ratio part is
It was 0.5 mm / min.
【００１９】これらの条件下で、単結晶の製造を行なっ
たところ、結晶面内でＡｌ濃度の均一な混晶比０．１５
±０．０１の単結晶の成長が確認された。実施例２
実施例１で用いた混晶単結晶体製造装置により、混晶単
結晶の製造を行なった。蒸発元素には、砒素を用いた。When a single crystal was manufactured under these conditions, a mixed crystal ratio of 0.15 with a uniform Al concentration in the crystal plane was obtained.
A single crystal growth of ± 0.01 was confirmed. Example 2 A mixed crystal single crystal was manufactured using the mixed crystal single crystal manufacturing apparatus used in Example 1. Arsenic was used as the evaporation element.
【００２０】単結晶製造の条件は、種結晶に直径１３ｍ
ｍのＧａＡｓを用い、原料棒には、直径１４ｍｍのＧａ
(1-x) Ａｌx Ａｓを用いた。この実施例で用いた原料多
結晶の混晶比は、最大０．３０であり、原料棒軸線方向
の起点における混晶比を０とし、軸線方向の原料棒の長
さは、１．５ｃｍであるので、混晶比勾配は、０．２／
ｃｍとなる。また、単結晶の成長条件は、砒素圧を約１
気圧とし、溶融帯幅を約３．０ｍｍ、成長速度は結晶開
始時には１．５ｍｍ／ｍｉｎとし、勾配部は徐々に速度
を遅くするようにした。さらに定混晶比部での速度は、
０．３ｍｍ／ｍｉｎとした。The condition for producing a single crystal is that the seed crystal has a diameter of 13 m.
m of GaAs is used, and the raw material rod is made of Ga having a diameter of 14 mm.
(1-x) Al x As was used. The mixed crystal ratio of the raw material polycrystal used in this example was 0.30 at maximum, the mixed crystal ratio at the starting point in the axial direction of the raw material rod was 0, and the length of the raw material rod in the axial direction was 1.5 cm. Therefore, the mixed crystal ratio gradient is 0.2 /
cm. In addition, the single crystal growth condition is that the arsenic pressure is about 1
The pressure was set to atmospheric pressure, the melting zone width was set to about 3.0 mm, the growth rate was set to 1.5 mm / min at the start of crystallization, and the speed of the gradient portion was gradually decreased. Furthermore, the speed in the constant mixed crystal ratio part is
It was set to 0.3 mm / min.
【００２１】これらの条件下で、単結晶の製造を行なっ
たところ、結晶面内でＡｌ濃度の均一な混晶比０．３０
±０．０２の単結晶の成長が確認された。When a single crystal was produced under these conditions, a mixed crystal ratio of 0.30 with a uniform Al concentration in the crystal plane was obtained.
A single crystal growth of ± 0.02 was confirmed.
【００２２】[0022]
【発明の効果】以上詳しく説明した通り、この発明によ
って、種付けが容易であり、二元化合物をも種として使
用することが可能となる。また、高混晶比の単結晶も容
易に成長させることができ、混晶比が均一でかつ化学量
論組成の単結晶を得ることが可能となる。As described in detail above, according to the present invention, seeding is easy and a binary compound can be used as a seed. Further, a single crystal having a high mixed crystal ratio can be easily grown, and a single crystal having a uniform mixed crystal ratio and a stoichiometric composition can be obtained.
【図１】この発明の混晶単結晶体製造装置を例示した構
成図である。FIG. 1 is a block diagram illustrating a mixed crystal single crystal body manufacturing apparatus of the present invention.
１ 耐圧容器 ２ 石英管 ３ 種結晶 ４ 単結晶 ５ 融液部 ６ 多結晶 ７ 支持棒接続部 ８ 多結晶の支持棒 ９ 種結晶の支持棒 １０ 支持棒接続部 １１ 上部シール部 １２ 下部シール部 １３ シール材 １４ 蒸発させる元素を収容する容器 １５ 接続パイプ １６ 蒸発させる元素 １７ 蒸発容器加熱ヒータ １８ 高周波誘導コイル １９ 上部加熱ヒータ ２０ 下部加熱ヒータ ２１ 上部シール部加熱ヒータ ２２ 下部シール部加熱ヒータ ２３ 内部観察用窓 ２４ 温度計 ２５ 加圧用ガス導入口 ２６ バルブまたは圧力調整器 ２７ 加圧用ガス 1 Pressure vessel 2 Quartz tube 3 seed crystals 4 single crystal 5 Melt part 6 Polycrystal 7 Support rod connection 8 Polycrystalline support rod 9 seed crystal support rod 10 Support rod connection 11 Upper seal part 12 Lower seal part 13 Seal material 14 Vessels containing elements to be evaporated 15 Connection pipe 16 Elements to be evaporated 17 Evaporator heating heater 18 High frequency induction coil 19 Upper heating heater 20 Lower heating heater 21 Upper seal heater 22 Lower seal heater 23 Internal observation window 24 thermometer 25 Pressurizing gas inlet 26 Valves or pressure regulators 27 Pressurizing gas
───────────────────────────────────────────────────── フロントページの続き (72)発明者 澤藤 裕 宮城県仙台市太白区向山三丁目７番７号 (56)参考文献 特開 昭59−39797（ＪＰ，Ａ) 特開 昭60−86098（ＪＰ，Ａ) 特開 昭63−85083（ＪＰ，Ａ) 特開 昭63−291890（ＪＰ，Ａ) 特開 平２−79422（ＪＰ，Ａ) 特開 平２−311387（ＪＰ，Ａ) 特開 平３−5391（ＪＰ，Ａ) 特開 平４−164897（ＪＰ，Ａ) 特開 平４−114991（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C30B 1/00 - 35/00 ＪＳＴＰｌｕｓ（ＪＯＩＳ)─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Hiroshi Sawato 3-7-7 Mukoyama, Taichiro-ku, Sendai City, Miyagi Prefecture (56) References JP 59-39797 (JP, A) JP 60-86098 ( JP, A 63-85083 (JP, A) JP 63-291890 (JP, A) JP 2-79422 (JP, A) JP 2-311387 (JP, A) JP Hei 3-5391 (JP, A) JP-A 4-164897 (JP, A) JP-A 4-114991 (JP, A) (58) Fields investigated (Int.Cl. 7 , DB name) C30B 1 / 00-35/00 JST Plus (JOIS)
Claims (2)
いて、軸方向に一端部から勾配をもって混晶比が増加す
る勾配部とそれに続く定混晶比部とを有する混晶多結晶
体原料棒により種組成近傍側より成長させることを特徴
とする混晶単結晶体の製造方法。1. In a floating zone crystal production by vapor pressure control, a mixed crystal polycrystal raw material bar having a gradient part where the mixed crystal ratio increases with a gradient from one end in the axial direction, and a constant mixed crystal ratio part following it. A method for producing a mixed crystal single crystal body, which is characterized in that it is grown from the side near the seed composition.
ＧａＡｓ種結晶を用い、Ａｓ圧下に成長させる請求項１
のＧａ−Ａｌ−Ａｓ混晶単結晶体の製造方法。2. The raw material rod has a Ga—Al—As composition,
A GaAs seed crystal is used and is grown under As pressure.
A method for producing a Ga-Al-As mixed crystal single crystal.
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| JP14834194A JP3532245B2 (en) | 1994-06-29 | 1994-06-29 | Method for producing mixed crystal single crystal |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14834194A JP3532245B2 (en) | 1994-06-29 | 1994-06-29 | Method for producing mixed crystal single crystal |
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| JP3532245B2 true JP3532245B2 (en) | 2004-05-31 |
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