JPS6090896A - Manufacture of gallium-arsenic single crystal - Google Patents
Manufacture of gallium-arsenic single crystalInfo
- Publication number
- JPS6090896A JPS6090896A JP58196054A JP19605483A JPS6090896A JP S6090896 A JPS6090896 A JP S6090896A JP 58196054 A JP58196054 A JP 58196054A JP 19605483 A JP19605483 A JP 19605483A JP S6090896 A JPS6090896 A JP S6090896A
- Authority
- JP
- Japan
- Prior art keywords
- crystal
- melt
- temp
- temperature
- speed
- 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.)
- Granted
Links
- 239000013078 crystal Substances 0.000 title claims abstract description 103
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 8
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 title claims description 9
- 230000001965 increasing effect Effects 0.000 claims abstract description 18
- 239000000155 melt Substances 0.000 claims abstract description 11
- 229910001218 Gallium arsenide Inorganic materials 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 abstract description 6
- 230000003028 elevating effect Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 description 10
- 238000009826 distribution Methods 0.000 description 7
- 239000000565 sealant Substances 0.000 description 6
- 230000008646 thermal stress Effects 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
- C30B15/00—Single-crystal growth by pulling from a melt, e.g. Czochralski method
-
- 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
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/42—Gallium arsenide
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
この発明は高品質々ガリウム砒素単結晶の製造方法に関
するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing high quality gallium arsenide single crystals.
副祈ｍ−ｖ族化合物半導体は高品質な単結晶が得られる
ようにな９、高速集積回路、光−電子集積回路、電子素
子用材料などに広く用いられるようになってきた。■＝
■族化合物半導体の中でもガリウム砒素（ＧａＡａ）は
シリコンに較べて電子移動度がはるかに早く、比抵抗が
１０″Ω、ｃＴｎ以上の高抵抗の大型ウェハーの製造が
容易であることなどにより注目を浴びている。このよう
なＧａＡ、単結晶は現在上として液体封止引き上げ法に
より製造されているが、この方法ではルツボ内の結晶原
料融液と封止剤との界面、結晶原料融液と引き上げ中の
結晶との界面及び結晶内の温度勾配が大きいため、形成
した結晶内に熱応力が生じ、これが結晶欠陥の一種であ
る転位の発生の原因となり、特に結晶の胴体部に較べて
テイル部において転位密度が通常著しく大きく々ってい
る。この原因は成長した結晶を結晶原料融液から切り離
す工程において、結晶の引き上げ速度を結晶の胴体部形
成時の１０〜１００倍の速度としていたことにあシ、こ
れにより結晶の下半部に与える温度変化が大きく、過大
な熱応力が発生して結晶のテイル部の転位密度を増大さ
せる結果と力っていた。従ってこのように結晶をウェー
Ｉ・にすると製品としての歩留りは低下し、特に結晶の
下半部よりテイル部までは製品化できず、無駄々ものと
なる。As high-quality single crystals of the MV group compound semiconductors have become available9, they have come to be widely used in high-speed integrated circuits, opto-electronic integrated circuits, materials for electronic devices, and the like. ■=
Among group compound semiconductors, gallium arsenide (GaAa) has attracted attention because it has much faster electron mobility than silicon, has a specific resistance of 10''Ω, and is easy to manufacture large wafers with high resistance of cTn or higher. Currently, such GaA single crystals are manufactured by the liquid-sealed pulling method, as described above, but in this method, the interface between the crystal raw material melt and the sealant in the crucible, the crystal raw material melt and the Due to the large temperature gradient at the interface with the crystal and within the crystal during pulling, thermal stress is generated within the formed crystal, which causes the generation of dislocations, which are a type of crystal defect. The dislocation density is usually extremely large in the crystal body.The reason for this is that in the process of separating the grown crystal from the crystal raw material melt, the pulling speed of the crystal was 10 to 100 times faster than when forming the body of the crystal. However, this causes a large temperature change in the lower half of the crystal, generating excessive thermal stress and increasing the dislocation density in the tail of the crystal. When I. is used, the yield as a product decreases, and in particular, the lower half of the crystal to the tail cannot be manufactured into a product, resulting in waste.
この発明の目的は結晶の下半部よシテイル部に亘っての
転位密度の増大を抑制し、結晶の頭部よりテイル部に到
るまで転位密度分布が実質的に均一の結晶を作成するＧ
ａＡ３単結晶を製造する方法を提供することにあ石。The purpose of this invention is to suppress the increase in dislocation density from the lower half of the crystal to the tail, and to create a crystal in which the dislocation density distribution is substantially uniform from the head of the crystal to the tail.
It is our aim to provide a method for producing aA3 single crystals.
液体封止引き上げ法によるＧａｋｓ単結晶の製造方法は
、通常不活性ガスによる１０〜７０気圧下において、上
面を一液体封止剤で被覆され、封止剤との界面が１２５
８℃に加熱されたルツボ中の結晶原料融液に種結晶を接
触させ、ルツボ及び種結晶を回転させながら、結晶直径
が約５０ｍの場合種結晶を１時間８〜１２−程度の速度
で引き上げて結晶の成長を行う。成長した結晶が目的と
する長さに達すると、種結晶の引き上げ速度を急激に１
００〜１０００町句と増加し、結晶をＧａＡｓ融液から
切り離していた。その結果、結晶のティル部は平面また
は半球面となるが、結晶の下半部からティル部は急速に
温度の高低の差の激しい液体封止剤内を通過し、不活性
ガス中に置かれるため、この太き々温度変化によって熱
応力が発生し、結晶の下半部からティル部に亘って転位
密度が増大する結果となる。The method for manufacturing Gaks single crystals using the liquid seal pulling method is to coat the upper surface with a single liquid sealant under an inert gas atmosphere of 10 to 70 atmospheres, and the interface with the sealant is 125
A seed crystal is brought into contact with the crystal raw material melt in a crucible heated to 8°C, and while rotating the crucible and seed crystal, if the crystal diameter is about 50 m, the seed crystal is pulled up at a speed of about 8 to 12 mm for 1 hour. crystal growth. When the grown crystal reaches the desired length, the pulling speed of the seed crystal is suddenly increased to 1.
The number of crystals increased from 00 to 1000, and the crystal was separated from the GaAs melt. As a result, the till part of the crystal becomes flat or hemispherical, but from the bottom half of the crystal the till part rapidly passes through a liquid sealant with a large temperature difference and is placed in an inert gas. Therefore, thermal stress is generated due to this drastic temperature change, resulting in an increase in dislocation density from the lower half of the crystal to the till portion.
そこでこの発明においては、成長したＧａＡｓ結晶が目
的の長さに達し、結晶を融液よシ切シ離す工程に入った
ら結晶の引き上げ速度を徐々に増速すると共に、ルツボ
内の結晶原料融液の表面温度も徐々に昇温する。Therefore, in this invention, when the grown GaAs crystal reaches the desired length and the crystal is separated from the melt, the pulling speed of the crystal is gradually increased, and the crystal raw material melt in the crucible is The surface temperature also gradually increases.
上述の結晶引き上げ速度の増速割合は結晶の胴体部を作
成した時の引き上げ速度の５倍以下とし、具体的には５
０鋼径の結晶を引き上げる場合１時間２０〜６０闘程度
に増速する。即ち、結晶の引き上げ速度が１０鱈／時の
場合は３０■／時程度が限度であって急激に引き上げ速
度を増速すると温度変化が大きくなり、結晶に転位が増
加する傾向を示すので、所定速度に達するまで４゜分か
ら１時間程度の時間を掛は徐々に増速する。The rate of increase in the crystal pulling speed mentioned above should be 5 times or less than the pulling speed at which the body of the crystal was created, specifically 5 times or less.
When pulling a crystal with a steel diameter of 0, the speed is increased to about 20 to 60 fights per hour. That is, when the crystal pulling rate is 10/hour, the limit is about 30/hour, and if the pulling rate is rapidly increased, the temperature change will increase and the number of dislocations in the crystal will tend to increase. It takes about 4° minutes to 1 hour to reach the speed, and the speed is gradually increased.
一方、結晶原料融液の結晶と接している表面の温度の上
昇範囲は結晶の胴体部を成長完了時の温度より１５℃ま
でであって、増速して引き上けた結晶の状態を考慮して
温度の上昇割合を調整する。即ち、所定の上昇割合で融
液の表面温度を徐々に昇温しても結晶のテイル部の外径
が減少しはじめないようであれば、温度の上昇割合を更
に大きくする。その結果、結晶のテイル部では結晶径が
次第に細くなシ、下方に凸の円錐状となシ、最後にルツ
ボの結晶原料融液と細い糸のような状態より切り離され
ることになる。On the other hand, the temperature increase range of the surface of the crystal raw material melt that is in contact with the crystal is up to 15 degrees Celsius from the temperature at which the growth of the body of the crystal is completed, taking into account the state of the crystal that is pulled up at increased speed. to adjust the temperature increase rate. That is, if the outer diameter of the tail portion of the crystal does not begin to decrease even if the surface temperature of the melt is gradually increased at a predetermined rate of increase, the rate of increase in temperature is further increased. As a result, at the tail portion of the crystal, the crystal diameter gradually becomes thinner, becomes conical with a convex shape downward, and finally separates from the crystal raw material melt in the crucible in a thin thread-like state.
このときの結晶の下半部は結晶の胴体部の引き上げ速度
よシも２〜３倍の早い速度で液体封止剤中を通過するこ
とと々るが、これまでの方法と比較した場合、結晶に急
激々温度変化を与えることはなく、従って過大力温度勾
配が結晶内に生じることもなく、その結果、転位の増大
は抑制される。また上述の結晶原料融液の表面温度の上
昇範囲が１５℃を越えたり、急激に所定の温度に昇温し
たりすると、既に固化して結晶となった部分が溶融する
こともあり好ましくない。At this time, the lower half of the crystal passes through the liquid sealant at a speed 2 to 3 times faster than the pulling speed of the body of the crystal, but when compared with previous methods, A sudden temperature change is not applied to the crystal, so no excessive force temperature gradient is generated within the crystal, and as a result, the increase in dislocations is suppressed. Furthermore, if the range of increase in the surface temperature of the above-mentioned crystal raw material melt exceeds 15° C. or if the temperature is rapidly raised to a predetermined temperature, the portions that have already solidified into crystals may melt, which is not preferable.
上記の説明で明らかなように、この発明の方法により結
晶の胴体部の成長が完了し、結晶を融液よシ切り離す工
程において、結晶の引き上げ速度及び融液の表面の温度
を上述の如く徐々に増速、昇温することにより、形成す
る結晶の下半部の転位の増大を抑制し、転位密度分布が
結晶全体に亘ってほぼ均一な結晶を得ることができるよ
うになったため、Ｇ（ｚＡＢ結晶の製品化の歩留りが著
しく向上し、安価に高品質のウェーハを提供することと
なる。As is clear from the above description, the growth of the body of the crystal is completed by the method of the present invention, and in the step of separating the crystal from the melt, the pulling speed of the crystal and the temperature of the surface of the melt are gradually adjusted as described above. By accelerating the speed and increasing the temperature to The yield of commercializing zAB crystals is significantly improved, and high-quality wafers can be provided at low cost.
次にこの発明を実施例により説明する。Next, the present invention will be explained with reference to examples.
内径９５ｍ、深さ１００ｍのパイロリテツク窒化ボロン
製ルツボにＧａ５００ｐ、Ａ８５４０ ｆ ｓ 液体封
止剤として酸化ボロン（Ｂ＊Ｏｓ） ５ｏｎｙを入れ、
とのルツボを高圧容器内に設置して、アルゴンガスで５
０気圧に加圧し、ルツボを１３００℃で加熱してＧａＡ
ｓ融液を合成した。Ga500p, A8540fs, and boron oxide (B*Os) 5ony as a liquid sealant were placed in a pyrolithic boron nitride crucible with an inner diameter of 95m and a depth of 100m.
Place the crucible in a high-pressure container and heat it with argon gas for 5 minutes.
Pressurize to 0 atmospheres and heat the crucible at 1300℃
s melt was synthesized.
次にＧａＡｓ融液と馬０．との界面の温度が１２３８℃
となるように調整した後、種結晶をＧａｐｓ融液に接触
させ、ルツボは１分間１５回の速度で時計方向に回転さ
せ、種結晶は１分間１０回の速度で反時計方向に回転さ
せながら、種結晶を１時間１０閣の速度で引き上げた。Next, GaAs melt and horse 0. The temperature at the interface with
After adjusting the seed crystal so that , the seed crystal was pulled up at a speed of 10 centimeters for one hour.
７時間の引き上は操作の結果、直径約５０ｍｍ、長さ約
８０冑の円柱状の結晶が形成したので、結晶の引き上げ
速度を１時間掛けて２０晴／時の速度に増速し、結晶融
液表面温度も１２４０℃に昇温した。２０ｍ／時に増速
してから更に１時間３０分間結晶の引き上げを行った結
果、結晶のテイル部の末尾は結晶原料融液と切離された
。As a result of the 7-hour pulling operation, cylindrical crystals with a diameter of about 50 mm and a length of about 80 mm were formed, so the crystal pulling speed was increased to 20 crystals/hour by multiplying the crystal by 1 hour. The surface temperature of the melt was also increased to 1240°C. As a result of increasing the speed to 20 m/hr and pulling the crystal for another 1 hour and 30 minutes, the tail of the crystal was separated from the crystal raw material melt.
得られたＧａｋｓ結晶には高さ約５０Ｗ＋の円錐状のテ
ィル部が形成し、この結晶を結晶長に沿って切断し、転
位密度分布を測定した結果、頭部よシ約８０圏までの結
晶の転位密度分布はｌＸ１０’〜５ Ｘ １Ｑ’ ｃｍ
−”であった。A conical till part with a height of approximately 50W+ was formed in the Gaks crystal obtained, and as a result of cutting this crystal along the crystal length and measuring the dislocation density distribution, it was found that the crystal extends from the head to approximately 80 circles The dislocation density distribution is lX10'~5X1Q' cm
-” was.
比較のため、同一条件で結晶の成長を行い、直径約５０
−１長さ約８０ｍの円柱状結晶が形成した時点で、結晶
の引き上げ速度を５００ｍ＋膚に増速しで結晶テイル部
と結晶原料融液の切離しを行った。For comparison, crystals were grown under the same conditions and had a diameter of approximately 50 mm.
-1 When a cylindrical crystal with a length of about 80 m was formed, the crystal pulling speed was increased to 500 m+ to separate the crystal tail from the crystal raw material melt.
得られた結晶のティル部の形状は半円状であって、この
結晶を結晶長に沿って切断し、転位密度分布を測定した
結果、頭部より５０ｍ＋までの結晶の転位密度分布はｌ
Ｘ１０’〜１Ｑ’ｃＩｎ−”であったが、それ以上はテ
イル部に近づくに従って増大し、頭部よ＃）８０ｍの位
置の結晶の転位密度分布は５ Ｘ １０’ｃｌｎ−”で
あツタ。The shape of the till part of the obtained crystal is semicircular, and as a result of cutting this crystal along the crystal length and measuring the dislocation density distribution, the dislocation density distribution of the crystal up to 50 m+ from the head is l
X10' to 1Q'cln-'', but the dislocation density distribution increases as it approaches the tail, and the dislocation density distribution of the crystal at a position of 80 m from the head is 5 x 10'cln-''.
特許出願人 工業技術院長 ２１０１終りPatent applicant: Director of the Agency of Industrial Science and Technology 2101 end
Claims (1)
リウム砒素融液に種結晶を接触させ、引き上げる液体封
止引き上げ法によるガリウム砒素単結晶の製造方法にお
ける結晶の胴体部の成長が完了し、結晶を融液゛より切
り離す工程において、結晶の引き上げ速度を該胴体部を
形成したときの引き上げ速度より徐々に増速し、それに
伴って融液表面の温度を、胴体部の成長完了時の温度よ
り１５℃までの範囲で徐々に昇温することを特徴とする
ガリウム砒素単結晶の製造方法。The growth of the body of the crystal in the method for producing a gallium arsenide single crystal by the liquid-sealed pulling method in which a seed crystal is brought into contact with a gallium arsenide melt whose temperature on the surface of the melt has been adjusted to the optimum crystal pulling temperature has been completed; In the process of separating the crystal from the melt, the pulling speed of the crystal is gradually increased from the pulling speed at which the body was formed, and the temperature of the melt surface is accordingly lowered to the temperature at which the growth of the body is completed. A method for producing a gallium arsenide single crystal, characterized in that the temperature is gradually raised within a range of 15°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58196054A JPS6090896A (en) | 1983-10-21 | 1983-10-21 | Manufacture of gallium-arsenic single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP58196054A JPS6090896A (en) | 1983-10-21 | 1983-10-21 | Manufacture of gallium-arsenic single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6090896A true JPS6090896A (en) | 1985-05-22 |
| JPH0348160B2 JPH0348160B2 (en) | 1991-07-23 |
Family
ID=16351426
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58196054A Granted JPS6090896A (en) | 1983-10-21 | 1983-10-21 | Manufacture of gallium-arsenic single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6090896A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01188500A (en) * | 1988-01-19 | 1989-07-27 | Nippon Mining Co Ltd | Production of compound semiconductor single crystal |
-
1983
- 1983-10-21 JP JP58196054A patent/JPS6090896A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01188500A (en) * | 1988-01-19 | 1989-07-27 | Nippon Mining Co Ltd | Production of compound semiconductor single crystal |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0348160B2 (en) | 1991-07-23 |
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