JP4122382B2 - Crystal growth method, bulk pre-crystal for bulk single crystal growth, and method for producing bulk pre-crystal for bulk single crystal growth - Google Patents
Crystal growth method, bulk pre-crystal for bulk single crystal growth, and method for producing bulk pre-crystal for bulk single crystal growth Download PDFInfo
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- 238000002109 crystal growth method Methods 0.000 title claims description 24
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- 229910001218 Gallium arsenide Inorganic materials 0.000 claims description 11
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 claims description 11
- 229910000577 Silicon-germanium Inorganic materials 0.000 claims description 7
- 239000004065 semiconductor Substances 0.000 claims description 5
- 229910000673 Indium arsenide Inorganic materials 0.000 claims description 4
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 2
- -1 GaAs compound Chemical class 0.000 claims 1
- 238000009826 distribution Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 3
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- 238000010438 heat treatment Methods 0.000 description 2
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- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- 229910008310 Si—Ge Inorganic materials 0.000 description 1
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- 230000003628 erosive effect Effects 0.000 description 1
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Description
本発明は、結晶成長方法、バルク単結晶成長用バルク予備結晶、及びバルク単結晶成長用バルク予備結晶の作製方法に関する。 The present invention relates to a crystal growth method, a bulk preliminary crystal for bulk single crystal growth, and a method for producing a bulk preliminary crystal for bulk single crystal growth.
従来、バルク単結晶の成長に用いる種結晶の結晶面は、デバイス・プロセス的な有用性という観点から選択されてきた。しかしながら、デバイス・プロセス的に有用な結晶面は必ずしも多結晶化の抑制という観点では、最適な成長面ではなく、多結晶化の問題はすべてのバルク単結晶の成長、生産にとって無視できない重要課題である。 Conventionally, the crystal plane of a seed crystal used for the growth of a bulk single crystal has been selected from the viewpoint of device process utility. However, crystal planes useful for devices and processes are not necessarily optimal growth planes in terms of suppression of polycrystallization, and the problem of polycrystallization is an important issue that cannot be ignored for the growth and production of all bulk single crystals. is there.
これまでバルク結晶の多結晶化を抑制する為に行われてきた対策は、ルツボ材の選択や、成長速度の制御などによる、マクロ的要因の制御による成長中の、結晶核発生の抑制にあった。そのため、一旦結晶核が発生すると、“その拡大”を抑制できなかった。 The countermeasures that have been taken so far to suppress polycrystallization of bulk crystals are to suppress the generation of crystal nuclei during growth by controlling macro factors, such as by selecting a crucible material and controlling the growth rate. It was. For this reason, once crystal nuclei are generated, the “expansion” cannot be suppressed.
融液や溶液などを用いて単結晶を成長する際に起こる多結晶化、即ち成長中にルソボ壁や融液あるいは溶液中から発生する結晶核から成長した結晶粒が、元の種結晶から成長した結晶を次第に侵食してしまう現象は、結晶成長において大きな問題であり、結晶成長学的観点から根本的な解決策が必要である。 Polycrystallization that occurs when a single crystal is grown using a melt or solution, that is, the crystal grains grown from the crystal walls generated from the wall of the Rusovo or from the melt or solution during growth grow from the original seed crystal. The phenomenon of gradually eroding the crystal is a major problem in crystal growth, and a fundamental solution is necessary from the viewpoint of crystal growth.
一方で、バルク単結晶は電気的あるいは光学的性質が一般に多結晶よりも優れており、太陽電池用結晶などの特殊な例をのぞいては、単結晶が産業上は利用されることが多い。そのため、常に高品質の単結晶の作製が要請されている。多結晶化の抑制については、これまでは、マクロ的な経験や試行錯誤に頼らざるを得ない状態で、抜本的な解決法はなかった。この様な解決策は、全率固溶型の状態図を有する多元系の半導体バルク結晶の基板としての新規応用などの実用的観点からも、新たな産業分野の開拓のために長く渇望されていた。 On the other hand, bulk single crystals generally have better electrical or optical properties than polycrystals, and single crystals are often used industrially except for special examples such as solar cell crystals. Therefore, it is always required to produce a high quality single crystal. Until now, there has been no drastic solution to the suppression of polycrystallization, with no choice but to rely on macro experience and trial and error. Such a solution has long been eagerly sought for the development of new industrial fields from a practical point of view, such as a new application as a substrate of a multi-element semiconductor bulk crystal having a solid solution type phase diagram. It was.
本発明は、上述した結晶成長学的観点及び実用的観点に基づき、種結晶以外からの結晶核の発生及び拡大を抑制し、高品質のバルク単結晶を作製することを目的とする。 An object of the present invention is to produce a high-quality bulk single crystal by suppressing the generation and expansion of crystal nuclei from other than the seed crystal based on the above-mentioned crystal growth viewpoint and practical viewpoint.
上記目的を達成すべく、本発明は、
多数の結晶片を第１の種結晶として結晶成長を行い、異なる面方位の複数の結晶面を有するバルク予備結晶を成長させる工程と、
前記バルク予備結晶において、最も面積増加率の高い結晶面を優先面として決定し選択する工程と、
前記優先面を成長面に有する単結晶を準備する工程と、
前記単結晶を第２の種結晶として結晶成長を行い、バルク単結晶を得る工程と、
を具えることを特徴とする、結晶成長方法に関する。
In order to achieve the above object, the present invention provides:
Performing a crystal growth using a large number of crystal pieces as a first seed crystal and growing a bulk preliminary crystal having a plurality of crystal planes of different plane orientations;
In the bulk preliminary crystal, a step of determining and selecting a crystal plane having the highest area increase rate as a priority plane;
Preparing a single crystal having the preferred surface as a growth surface;
Performing a crystal growth using the single crystal as a second seed crystal to obtain a bulk single crystal;
It is related with the crystal growth method characterized by comprising.
本発明では、目的とするバルク単結晶を作製するに当り、結晶成長を２段階で行う。最初の結晶成長工程では、板状または球状などの多数の結晶片を第１の種結晶として用い、これを結晶核として、例えば一方向成長により結晶成長を行う。前記第１の種結晶は種々の面方位を有するため、前記結晶成長を通じて、異なる面方位の複数の結晶面を有するバルク予備結晶が得られるようになる。 In the present invention, crystal growth is carried out in two stages for producing the target bulk single crystal. In the first crystal growth step, a large number of crystal pieces such as a plate shape or a spherical shape are used as the first seed crystal, and this is used as a crystal nucleus to perform crystal growth, for example, by unidirectional growth. Since the first seed crystal has various plane orientations, a bulk preliminary crystal having a plurality of crystal planes with different plane orientations can be obtained through the crystal growth.
このとき、面方位の異なる各結晶粒の成長速度は微妙な差を有するため、結晶成長に伴い成長速度の速い結晶面の面積は増加し、成長速度の遅い結晶面の面積は減少するという現象、即ち面方位の競合関係が起きる。この様子は、成長した結晶を成長方向と垂直にスライスし、電子後方分散パターン法（Electron Back Scattering pattern法:ＥＢＳＰ法）のような方位顕微鏡などを用いて各結晶における面積の割合の連続的な変化を追うことにより観察できる。そして、最も面積増加率の高い結晶面を、優先方位の面方位（優先面）として決定する。 At this time, because the growth rate of each crystal grain with different plane orientations has a subtle difference, the area of the crystal plane with a high growth rate increases and the area of the crystal plane with a low growth rate decreases with crystal growth. That is, a competing relationship between plane orientations occurs. This is done by slicing the grown crystal perpendicularly to the growth direction, and using an orientation microscope such as the electron back scattering pattern method (EBSP method) to continuously measure the area ratio of each crystal. It can be observed by following changes. Then, the crystal plane with the highest area increase rate is determined as the plane orientation (priority plane) of the preferred orientation.
次いで、２段目の結晶成長工程では、前記優先面を成長面とする単結晶を準備し、これを第２の種結晶としてさらに結晶成長を行う。この結果、結晶成長中に発生した結晶核は、前記優先面から成長した優先方位を持つ結晶粒内に取り込まれるようになるため、前記結晶核は結晶粒として拡大しない。従って、多結晶化を抑制でき、高品質の単結晶を常に得ることができる。なお、前述した取り込み効果は、前記優先面の優先度合い、すなわち面積増大率が大きいほど顕著になる。 Next, in the second-stage crystal growth step, a single crystal having the priority surface as a growth surface is prepared, and this is further used as a second seed crystal for further crystal growth. As a result, crystal nuclei generated during crystal growth are taken into crystal grains having a preferred orientation grown from the preferred plane, so that the crystal nuclei do not expand as crystal grains. Therefore, polycrystallization can be suppressed and a high-quality single crystal can always be obtained. The above-described capturing effect becomes more prominent as the priority level of the priority surface, that is, the area increase rate is larger.
前記優先面は結晶系、成長速度、多元系の組成などに依存して決定される。 The priority plane is determined depending on the crystal system, growth rate, multi-component composition, and the like.
前記２段目の結晶成長工程における前記単結晶は、上述した１段目の結晶成長とは別個の工程で得たものを用いることもできるし、前記バルク予備結晶から前記優先面を成長面に有する単結晶部分を切り出して用いることもできる。 The single crystal in the second-stage crystal growth step can be a single crystal obtained in a step separate from the first-stage crystal growth described above, or the preferential surface can be used as a growth surface from the bulk preliminary crystal. It is also possible to cut out and use the single crystal portion it has.
なお、本発明の目的をより効果的に実現するためには、前記バルク予備結晶を作製するために使用する前記第１の種結晶は、前記バルク予備結晶を構成する元素の少なくとも一つを含むことが好ましい。同様に、前記バルク予備結晶を切り出して得た前記第２の種結晶は、前記バルク単結晶を構成する元素の少なくとも一つを含むことが好ましい。さらに、前記バルク予備結晶と前記バルク単結晶の成長条件は同一とすることが好ましい。 In order to more effectively realize the object of the present invention, the first seed crystal used for producing the bulk preliminary crystal includes at least one element constituting the bulk preliminary crystal. It is preferable. Similarly, the second seed crystal obtained by cutting out the bulk preliminary crystal preferably contains at least one element constituting the bulk single crystal. Furthermore, it is preferable that the growth conditions of the bulk preliminary crystal and the bulk single crystal are the same.
以上説明したように、本発明によれば、種結晶以外からの結晶核の発生を抑制し、高品質のバルク単結晶を作製することが可能となる。 As described above, according to the present invention, generation of crystal nuclei from other than the seed crystal can be suppressed, and a high-quality bulk single crystal can be produced.
以下、本発明の詳細、並びにその他の特徴及び利点について詳述する。
上述したように、本発明では２段階の結晶成長を経て目的とするバルク単結晶を得る。最初の工程では、多数の結晶片を第１の種結晶として結晶成長を行い、得られたバルク予備結晶から本結晶成長過程における優先面を決定する。前記第１の種結晶は、板状又は球状などいずれの形態の結晶片からも構成することができる。
Details of the present invention, as well as other features and advantages, are described in detail below.
As described above, in the present invention, a target bulk single crystal is obtained through two stages of crystal growth. In the first step, crystal growth is performed using a large number of crystal pieces as a first seed crystal, and a priority plane in the crystal growth process is determined from the obtained bulk preliminary crystal. The first seed crystal can be composed of any form of crystal pieces such as a plate shape or a spherical shape.
また、前記第１の種結晶の大きさは特に限定されるものではないが、好ましくは５０ｍｍ以下とする。さらに、前記第１の種結晶は前記バルク予備結晶を構成する元素の少なくとも一つを含むことが好ましい。これらの要件を満足する場合は、前記第１の種結晶からの前記バルク予備結晶の成長を容易ならしめ、目的とするバルク単結晶を簡易に得ることができる。 The size of the first seed crystal is not particularly limited, but is preferably 50 mm or less. Furthermore, it is preferable that the first seed crystal contains at least one element constituting the bulk preliminary crystal. When these requirements are satisfied, the growth of the bulk preliminary crystal from the first seed crystal can be facilitated, and the intended bulk single crystal can be easily obtained.
前記バルク予備結晶の作製は、例えば前記第１の種結晶を所定の容器の底部に配置し、前記第１の種結晶の上方に原材料を充填し、加熱溶融させることによって、前記第１の種結晶と接触するように融液を形成し、次いで、前記融液中に所定の温度勾配を形成し、前記融液の過飽和を駆動力とすることにより前記第１の種結晶を結晶核として結晶成長を行うことによって実施する。 The bulk preliminary crystal is manufactured by, for example, placing the first seed crystal at the bottom of a predetermined container, filling the raw material above the first seed crystal, and heating and melting the first seed crystal. A melt is formed so as to come into contact with the crystal, then a predetermined temperature gradient is formed in the melt, and the first seed crystal is used as a crystal nucleus by using supersaturation of the melt as a driving force. Implement by growing.
上述のようにして前記バルク予備結晶を作製した後、前記バルク予備結晶を成長方向と垂直な面でスライスし、ＥＢＳＰ法などによってその結晶面の分布を観察し、各結晶面の面積の割合を測定する。これによって、前記バルク予備結晶の、面積増加率の最も高い結晶面を優先面として決定する。なお、ＥＢＳＰ法は公知の結晶観察方法であって、例えば日本金属学会誌、２００１年７月号、Vol．4D, pp611-654などに記載されている。 After the bulk preliminary crystal is manufactured as described above, the bulk preliminary crystal is sliced in a plane perpendicular to the growth direction, the distribution of the crystal plane is observed by an EBSP method or the like, and the ratio of the area of each crystal plane is determined. taking measurement. Thus, the crystal plane having the highest area increase rate of the bulk preliminary crystal is determined as the priority plane. The EBSP method is a known crystal observation method. For example, the Journal of the Japan Institute of Metals, July 2001, Vol. 4D, pp611-654, etc.
次いで、前記優先面を成長面に有する単結晶を準備し、これを第２の種結晶としてさらに結晶成長を行う。前記単結晶は上述した第１の結晶成長とは別個の工程で得たものを用いることもできるし、前記バルク予備結晶の前記優先面を含む単結晶部分を選択して切り出して用いることもできる。 Next, a single crystal having the priority surface as a growth surface is prepared, and this is further used as a second seed crystal for further crystal growth. As the single crystal, one obtained in a step separate from the first crystal growth described above can be used, or a single crystal portion including the priority surface of the bulk preliminary crystal can be selected and cut out. .
なお、前記第２の種結晶の大きさは特に限定されるものではないが、好ましくは３００ｍｍ以下とする。さらに、前記第２の種結晶は前記バルク単結晶を構成する元素の少なくとも一つを含むことが好ましい。これらの要件を満足する場合は、前記第２の種結晶からの前記バルク単結晶の成長を容易ならしめ、目的とするバルク単結晶を簡易に得ることができる。 The size of the second seed crystal is not particularly limited, but is preferably 300 mm or less. Furthermore, it is preferable that the second seed crystal contains at least one element constituting the bulk single crystal. When these requirements are satisfied, the bulk single crystal can be easily grown from the second seed crystal, and the intended bulk single crystal can be easily obtained.
前記バルク予備結晶の作製は、例えば前記第２の種結晶を所定の容器の底部に配置し、前記第２の種結晶の上方に原材料を充填し、加熱溶融させることによって、前記第２の種結晶と接触するように融液を形成し、次いで、前記融液中に所定の温度勾配を形成し、前記融液の過飽和を駆動力とすることにより前記第２の種結晶を結晶核として結晶成長を行うことによって実施する。 The bulk preliminary crystal is produced, for example, by placing the second seed crystal at the bottom of a predetermined container, filling the raw material above the second seed crystal, and heating and melting the second seed crystal. A melt is formed so as to come into contact with the crystal, then a predetermined temperature gradient is formed in the melt, and the second seed crystal is used as a crystal nucleus by using supersaturation of the melt as a driving force. Implement by growing.
なお、前記第２の種結晶からの前記バルク単結晶の成長と、前記第１の種結晶からの前記バルク予備結晶の成長とは同一の成長条件で行うことが好ましい。すなわち、上述したバルク予備結晶の作製方法及びバルク単結晶の作製方法において、使用する原材料の種類及び組成などを同一にして同一組成の融液を作製し、前記融液中に同一の温度勾配などを形成する。これによって、前記第２の種結晶を構成する、前記バルク単結晶から選択した前記優先面の作用効果が増大し、前記優先面を種結晶面とした結晶成長が促進され、高品質のバルク単結晶をより簡易に作製することができるようになる。 It is preferable that the growth of the bulk single crystal from the second seed crystal and the growth of the bulk preliminary crystal from the first seed crystal are performed under the same growth conditions. That is, in the above-described bulk preliminary crystal production method and bulk single crystal production method, melts having the same composition are produced by using the same kind and composition of raw materials to be used, and the same temperature gradient or the like in the melt. Form. This increases the effect of the priority plane selected from the bulk single crystal constituting the second seed crystal, promotes crystal growth using the priority plane as a seed crystal plane, and produces a high-quality bulk single crystal. Crystals can be produced more easily.
以下、本発明を具体例に基づいて詳細に説明する。 Hereinafter, the present invention will be described in detail based on specific examples.
（実施例１）
本実施例では、ＳｉＧｅバルク単結晶の作製を試みた。
最初に、直径１５ｍｍの石英管中に直径約２ｍｍ以下の多数のＧｅ結晶の破片を第１の種結晶として配置し、その上方に直径１５ｍｍ、長さ４０ｍｍのＧｅ多結晶を配置した。さらにその上に、元素補給用Ｓｉ単結晶を配置し、真空封入した。次いで、前記Ｓｉ単結晶側が高温、前記種結晶側が低温となり、約３０℃／ｃｍの温度勾配を有するように前記石英管中の前記Ｓｉ単結晶及びＧｅ多結晶を加熱し、溶解させた。これによって、前記石英管中には、Ｓｉ‐Ｇｅ二元系融液が形成された。
(Example 1)
In this example, an attempt was made to produce a SiGe bulk single crystal.
First, a large number of Ge crystal fragments having a diameter of about 2 mm or less were arranged as a first seed crystal in a quartz tube having a diameter of 15 mm, and a Ge polycrystal having a diameter of 15 mm and a length of 40 mm was arranged thereon. Further thereon, an element replenishment Si single crystal was placed and sealed in a vacuum. Next, the Si single crystal and the Ge polycrystal in the quartz tube were heated and dissolved so that the Si single crystal side had a high temperature and the seed crystal side had a low temperature and had a temperature gradient of about 30 ° C./cm. As a result, a Si—Ge binary melt was formed in the quartz tube.
このとき、前記第１の種結晶上には過飽和を駆動力としてＳｉＧｅバルク予備結晶が成長した。得られた前記ＳｉＧｅバルク予備結晶を、その成長方向に垂直な面内でスライスし、結晶面の分布をＥＢＳＰ法により測定した。その結果、最も面積増加率の高い結晶面（優先面）は、（１１０）面であり、最も面積増加率の低い面は（１１１）面であった。 At this time, a SiGe bulk preliminary crystal was grown on the first seed crystal using supersaturation as a driving force. The obtained SiGe bulk preliminary crystal was sliced in a plane perpendicular to the growth direction, and the distribution of the crystal plane was measured by the EBSP method. As a result, the crystal plane (priority plane) with the highest area increase rate was the (110) plane, and the plane with the lowest area increase rate was the (111) plane.
次いで、直径１５ｍｍ、長さ２０ｍｍの、（１１０）面及び（１１１）面を有するＧｅ単結晶を準備し、これらを第２の種結晶として、前記バルク予備結晶の作製と同一の成長条件で結晶成長を行った。 Next, a Ge single crystal having a (110) plane and a (111) plane having a diameter of 15 mm and a length of 20 mm is prepared, and these are used as a second seed crystal under the same growth conditions as in the production of the bulk preliminary crystal. Made growth.
その後、得られた結晶を結晶方向に垂直な面内でスライスし、ＥＢＳＰ法により結晶面の分布を測定した。その結果、（１１１）面を有する単結晶部分を種結晶として用いた場合は、成長開始後間もなくルツボ壁から結晶粒が発生し、次第に（１１１）結晶面を持つ結晶粒を侵食するようにして、ＳｉＧｅバルク多結晶が生成されたのに対して、（１１０）面を有する単結晶部分を種結晶として用いた場合は、新たな結晶核の生成はなく、前記種結晶を結晶核とした結晶成長が行われ、ＳｉＧｅバルク単結晶が生成された。 Thereafter, the obtained crystal was sliced in a plane perpendicular to the crystal direction, and the distribution of the crystal plane was measured by the EBSP method. As a result, when a single crystal portion having a (111) plane is used as a seed crystal, crystal grains are generated from the crucible wall shortly after the start of growth, and the crystal grains having the (111) plane are gradually eroded. When a single crystal portion having a (110) plane is used as a seed crystal while a SiGe bulk polycrystal is generated, there is no generation of a new crystal nucleus, and a crystal using the seed crystal as a crystal nucleus. Growth took place and a SiGe bulk single crystal was produced.
（実施例２）
本実施例ではＩｎＧａＡｓバルク単結晶の作製を試みた。
最初に、直径１５ｍｍの石英管中に直径約２ｍｍ以下の多数のＩｎＧａＡｓ結晶片を第１の種結晶として配置し、その上方に直径１５ｍｍ、長さ４０ｍｍのＩｎＡｓ単結晶を配置した。さらにその上に、元素補給用ＧａＡｓ単結晶を配置し、真空封入した。前記ＧａＡｓ単結晶側が高温、前記種結晶側が低温となり、約３０℃／ｃｍの温度勾配を有するように前記ＩｎＡｓ単結晶及び前記ＧａＡｓ単結晶を加熱し、溶解させた。これによって、前記石英管中には、ＩｎＡｓ‐ＧａＡｓ擬二元系融液が形成された。
(Example 2)
In this example, an attempt was made to produce an InGaAs bulk single crystal.
First, a large number of InGaAs crystal pieces having a diameter of about 2 mm or less were disposed as first seed crystals in a quartz tube having a diameter of 15 mm, and an InAs single crystal having a diameter of 15 mm and a length of 40 mm was disposed thereon. Furthermore, a GaAs single crystal for element supplementation was placed thereon and sealed in a vacuum. The InAs single crystal and the GaAs single crystal were heated and dissolved so that the GaAs single crystal side had a high temperature and the seed crystal side had a low temperature and had a temperature gradient of about 30 ° C./cm. As a result, an InAs-GaAs pseudo binary melt was formed in the quartz tube.
このとき、前記第１の種結晶上には過飽和を駆動力としてＩｎＧａＡｓバルク予備結晶が成長した。得られたＩｎＧａＡｓバルク予備結晶を、その成長方向に垂直な面内でスライスし、結晶面の分布をＥＢＳＰ法により測定した。その結果、最も面積増加率の高い結晶面（優先面）は、（１１０）面であることが判明した。 At this time, an InGaAs bulk preliminary crystal was grown on the first seed crystal using supersaturation as a driving force. The obtained InGaAs bulk preliminary crystal was sliced in a plane perpendicular to the growth direction, and the distribution of the crystal plane was measured by the EBSP method. As a result, it was found that the crystal plane (priority plane) having the highest area increase rate was the (110) plane.
次いで、直径１５ｍｍ、長さ２０ｍｍの（１１０）ＧａＡｓ単結晶を準備し、これを第２の種結晶として、前記ＩｎＧａＡｓバルク予備結晶の作製と同一の成長条件で結晶成長を行った。 Next, a (110) GaAs single crystal having a diameter of 15 mm and a length of 20 mm was prepared, and this was used as a second seed crystal, and crystal growth was performed under the same growth conditions as the production of the InGaAs bulk preliminary crystal.
その後、得られた結晶を結晶方向に垂直な面内でスライスし、ＥＢＳＰ法により結晶面の分布を測定した。その結果、新たな結晶核の生成はなく、前記種結晶を結晶核とした結晶成長が行われ、高品質なＩｎＧａＡｓバルク単結晶が生成された。 Thereafter, the obtained crystal was sliced in a plane perpendicular to the crystal direction, and the distribution of the crystal plane was measured by the EBSP method. As a result, no new crystal nucleus was generated, and crystal growth was performed using the seed crystal as a crystal nucleus, and a high-quality InGaAs bulk single crystal was generated.
なお、ＩｎＧａＡｓバルク単結晶は、光通信用の高効率、高温度特性を有する半導体レーザー用基板結晶として極めて有望である。 Note that the InGaAs bulk single crystal is extremely promising as a semiconductor laser substrate crystal having high efficiency and high temperature characteristics for optical communication.
以上、具体例を挙げながら発明の実施の形態に基づいて本発明を詳細に説明してきたが、本発明は上記内容に限定されるものではなく、本発明の範疇を逸脱しない限りにおいてあらゆる変形や変更が可能である。 As described above, the present invention has been described in detail based on the embodiments of the present invention with specific examples. However, the present invention is not limited to the above contents, and all modifications and changes are made without departing from the scope of the present invention. It can be changed.
例えば、実施例１では、Ｇｅ結晶片を第１の種結晶として用いているが、Ｓｉ結晶片を用いることもできる。また、実施例２ではＩｎＧａＡｓ結晶片を第１の種結晶として用いているが、ＧａＡｓ結晶片を用いることもできる。さらに、ＧａＡｓ単結晶の代わりに、ＩｎＡｓ単結晶を第２の種結晶として用いることもできる。 For example, in Example 1, a Ge crystal piece is used as the first seed crystal, but a Si crystal piece can also be used. In Embodiment 2, an InGaAs crystal piece is used as the first seed crystal, but a GaAs crystal piece can also be used. Further, an InAs single crystal can be used as the second seed crystal instead of the GaAs single crystal.
本発明によれば、従来単結晶化が困難であった全率固溶型の状態図を有する多元系のバルク単結晶を簡易に作製することができる。したがって、このようなバルク単結晶を利用する種々の工業分野に適用することができる。特にＩｎＧａＡｓなどのＧａＡｓ系半導体バルク単結晶を簡易に作製することができ、光通信用の高効率及び高温度特性を有する基板材料の提供が可能となる。また、Ｓｉ系バルク単結晶を簡易に作製することができ、高性能化された新規な電子デバイスの提供が可能となる。 According to the present invention, it is possible to easily produce a multi-element bulk single crystal having a complete solid solution type phase diagram that has been difficult to convert into a single crystal. Therefore, it can be applied to various industrial fields using such bulk single crystals. In particular, a GaAs-based semiconductor bulk single crystal such as InGaAs can be easily produced, and a substrate material having high efficiency and high temperature characteristics for optical communication can be provided. In addition, a Si-based bulk single crystal can be easily manufactured, and a new electronic device with high performance can be provided.
Claims (25)
前記バルク予備結晶において、最も面積増加率の高い結晶面を優先面として決定し選択する工程と、
前記優先面を成長面に有する単結晶を準備する工程と、
前記単結晶を第２の種結晶として結晶成長を行い、バルク単結晶を得る工程と、
を具えることを特徴とする、結晶成長方法。 Performing a crystal growth using a large number of crystal pieces as a first seed crystal and growing a bulk preliminary crystal having a plurality of crystal planes of different plane orientations;
In the bulk preliminary crystal, a step of determining and selecting a crystal plane having the highest area increase rate as a priority plane;
Preparing a single crystal having the preferred surface as a growth surface;
Performing a crystal growth using the single crystal as a second seed crystal to obtain a bulk single crystal;
A crystal growth method comprising the steps of:
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