JPH022840B2 - - Google Patents
Info
- Publication number
- JPH022840B2 JPH022840B2 JP55107219A JP10721980A JPH022840B2 JP H022840 B2 JPH022840 B2 JP H022840B2 JP 55107219 A JP55107219 A JP 55107219A JP 10721980 A JP10721980 A JP 10721980A JP H022840 B2 JPH022840 B2 JP H022840B2
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- compound semiconductor
- annealing
- semiconductor single
- present
- 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.)
- Expired - Lifetime
Links
Classifications
-
- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10P—GENERIC PROCESSES OR APPARATUS FOR THE MANUFACTURE OR TREATMENT OF DEVICES COVERED BY CLASS H10
- H10P95/00—Generic processes or apparatus for manufacture or treatments not covered by the other groups of this subclass
- H10P95/90—Thermal treatments, e.g. annealing or sintering
- H10P95/904—Thermal treatments, e.g. annealing or sintering of Group III-V semiconductors
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
Description
【発明の詳細な説明】
本発明は化合物半導体単結晶の焼鈍方法に係
り、特に揮発性物質例えば燐（Ｐ）、ヒ素（As）
等を含む化合物半導体単結晶の焼鈍方法に関する
ものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method of annealing a compound semiconductor single crystal, and particularly relates to an annealing method for annealing a compound semiconductor single crystal.
The present invention relates to an annealing method for compound semiconductor single crystals, including the following.
揮発性物質を含む化合物半導体単結晶の代表的
なGaP単結晶は可視発光ダイオード用基板として
重要な材料であり、通常高圧中で液体カプセル法
（LEC法）によつて作られている。 GaP single crystal, which is a typical compound semiconductor single crystal containing volatile substances, is an important material as a substrate for visible light emitting diodes, and is usually manufactured under high pressure by the liquid encapsulation method (LEC method).
しかしながらLEC法で作られた、GaP単結晶
はそのままの状態では必ず結晶生成時の歪みや生
成後の室温冷却時の熱歪みをもつている。このた
めその後の結晶切断、素子加工工程等においてク
ラツクが生じたり、素子の電気的特性にも悪影響
を及ぼしたりして、著しく加工歩留りを低下させ
る原因となつている。 However, GaP single crystals made by the LEC method always have distortions during crystal formation and thermal distortions during cooling to room temperature after formation. This causes cracks to occur during subsequent crystal cutting, device processing steps, etc., and also adversely affects the electrical characteristics of the device, resulting in a significant reduction in processing yield.
このような内部歪を除去する方法として、GaP
単結晶を焼鈍することが一般に行なわれている。
この方法では、不活性ガス中においてGaP単結晶
が均一に加熱されること、GaP単結晶表面からの
Ｐの揮散が抑えられるような措置を講じ、焼鈍に
よるクラツクの発生や単結晶表面の侵蝕を防ぐ必
要がある。そのために、高圧容器内焼鈍や二温度
法（Ｐの蒸気圧制御）焼鈍のような閉管法による
焼鈍が行なわれているが、装置が複雑で高価であ
ること、操作に熟練を要し、使用法を誤ると、爆
発等の恐れがあるなどの欠点がある。 As a method to remove such internal distortion, GaP
It is common practice to anneal a single crystal.
In this method, measures are taken to uniformly heat the GaP single crystal in an inert gas and to suppress the volatilization of P from the surface of the GaP single crystal, thereby preventing the occurrence of cracks due to annealing and corrosion of the single crystal surface. It is necessary to prevent it. For this purpose, closed-tube annealing methods such as high-pressure vessel annealing and two-temperature method (P vapor pressure control) annealing are carried out, but the equipment is complex and expensive, and the operation requires skill. There are drawbacks such as the risk of explosion if the law is incorrect.
別の方法として開管法による焼鈍は、複雑な装
置を必要とせず、操作も簡単で危険を伴うことは
ないが、不活性雰囲気ガスの流れが単結晶に直接
触れるため、熱の均一性やＰの揮散の点で、問題
がある。そこで小孔を有する半密閉型容器内に単
結晶を収容することにより、上記欠点を改善する
ことが行なわれている。しかし前記の方法にくら
べてその効果は十分とは言えない。 An alternative method, open-tube annealing, does not require complicated equipment, is easy to operate, and is not dangerous; There is a problem with the volatilization of P. Therefore, attempts have been made to improve the above-mentioned drawbacks by housing the single crystal in a semi-closed container having small holes. However, the effect cannot be said to be sufficient compared to the above-mentioned methods.
近年単結晶の大型化が進み、さらに、オレン
ジ、イエロー発光ダイオード用の基板が要求され
ている。そのため、十分歪の少い、良質な基板が
低コストで得られることが必要となつている。 In recent years, single crystals have become larger, and substrates for orange and yellow light emitting diodes are also required. Therefore, it is necessary to obtain a high-quality substrate with sufficiently low distortion at a low cost.
本発明は上記点に鑑みなされたもので、LEC
法により製造した化合物半導体単結晶を、単結晶
と同種の単結晶粉末及び保温シートで２層に被覆
し、しかるのち円筒容器に収納した状態で焼鈍す
ることにより、雰囲気ガス流との遮断、均熱化を
図り、単結晶からのＰの揮散を防止し、クラツク
の発生を招くことなく、歪を効果的に解消しうる
簡便な焼鈍方法を提供することにある。 The present invention has been made in view of the above points, and is
A compound semiconductor single crystal produced by this method is coated with two layers of single crystal powder of the same type as the single crystal and a heat insulating sheet, and then annealed while stored in a cylindrical container. The object of the present invention is to provide a simple annealing method that can heat the single crystal, prevent P from volatilizing from the single crystal, and effectively eliminate strain without causing cracks.
即ち本発明は、従来のいずれの方法においても
Ｐの揮散は少なからず生じること、及びＰの揮散
は単結晶表面から生じることに鑑み、単結晶の周
囲を同種の単結晶粉末及び保温シートで２層に被
覆し、開管法により不活性雰囲気中で、焼鈍する
ことを特徴とするものである。 That is, in the present invention, in view of the fact that a considerable amount of P volatilization occurs in any of the conventional methods, and that the P volatilization occurs from the surface of the single crystal, the single crystal is surrounded by two layers of the same type of single crystal powder and a heat insulating sheet. It is characterized in that it is coated in a layer and annealed in an inert atmosphere by an open tube method.
本発明に用いる化合物半導体単結晶としては、
GaPの他にGaAs，InP等の揮発性物質を含むも
のを挙げることが出きる。 The compound semiconductor single crystal used in the present invention includes:
In addition to GaP, materials containing volatile substances such as GaAs and InP can be mentioned.
以下、図面を参照して本発明方法の一実施例を
説明する。まずLEC法によつて（100）軸引上げ
で製造し、45mmφ×70mmｌのGaP単結晶１を第１
図に示すように、粒径10μ〜30μの同種の単結晶
粉末２及びカーボンフエルト３で被覆したのち、
円筒形石英容器４に収納して、カーボンのフタ５
をした。この容器４を第２図に示すごとく炉芯管
６，発熱体７を有する横型電気炉８の内に装填し
フタ９をかぶせた。次にN2ガスを1.5l／minの流
量で炉芯管６内に供給し、内部をN2ガスに置換
した後、200℃／Hrの昇温速度で1100℃まで昇温
し、そこで８時間、加熱保持した。焼鈍終了後、
100℃／Hrの降温速度で室温まで徐冷した。第３
図はこのようにして得られたGaP単結晶からウエ
ハを切り出した後、クロスニコル像により観察し
た歪の状態の一例を示している。図中ａは本発明
の方法により得られたGaPウエハの歪分布図であ
り、ｂは従来の小孔を有する半密閉型容器内に設
置して焼鈍したGaPウエハの歪分布図である。さ
らに第４図は焼鈍によるGaP単結晶インゴツトの
重量損失割合を示したものである。図中ｃは本発
明の方法によるものであり、ｄは小孔を有する半
密閉型容器内に設置して焼鈍した場合、ｅは直接
炉芯管内に置いて焼鈍した場合である。このよう
に本発明の方法によれば、従来の方法に較べて、
歪の量を半分以下に低減することができ、さらに
Ｐの揮散による重量損失も0.2％と非常に少く、
Ｐの揮散を抑えることにおいても絶大な効果を有
するものである。 An embodiment of the method of the present invention will be described below with reference to the drawings. First, a GaP single crystal 1 of 45 mmφ x 70 mml was manufactured by (100) axis pulling using the LEC method.
As shown in the figure, after being coated with the same kind of single crystal powder 2 with a particle size of 10μ to 30μ and carbon felt 3,
It is stored in a cylindrical quartz container 4 and covered with a carbon lid 5.
Did. This container 4 was loaded into a horizontal electric furnace 8 having a furnace core tube 6 and a heating element 7, as shown in FIG. 2, and a lid 9 was placed thereon. Next, N 2 gas was supplied into the furnace core tube 6 at a flow rate of 1.5 l/min to replace the inside with N 2 gas, and then the temperature was raised to 1100 °C at a rate of 200 °C/Hr. The mixture was heated and maintained for a period of time. After annealing,
It was slowly cooled to room temperature at a cooling rate of 100°C/Hr. Third
The figure shows an example of the state of strain observed using a crossed Nicol image after cutting a wafer from the GaP single crystal thus obtained. In the figure, a is a strain distribution diagram of a GaP wafer obtained by the method of the present invention, and b is a strain distribution diagram of a GaP wafer placed in a conventional semi-closed container with small holes and annealed. Furthermore, FIG. 4 shows the weight loss rate of the GaP single crystal ingot due to annealing. In the figure, c shows the method of the present invention, d shows the case where the material was annealed by being placed in a semi-closed container with small holes, and e shows the case where the material was annealed by being placed directly in the furnace core tube. As described above, according to the method of the present invention, compared to the conventional method,
The amount of distortion can be reduced to less than half, and the weight loss due to P volatilization is extremely small at 0.2%.
It also has a tremendous effect in suppressing the volatilization of P.
このように本発明の方法では、同種の単結晶粉
末及び保温シートで覆うことによりGaP単結晶と
保温シートとの密着性、外部雰囲気との気密性を
高め熱の均一性を向上させるものである。さらに
Ｐの揮散をまず単結晶粉末から生じさせることで
ストツパーとなり、GaP単結晶からのＰの揮散を
効果的に抑圧するものである。円筒形容器は保温
シートの形を保つものでこの容器の有無は、本発
明の効果に何ら影響を及すものではない。 As described above, in the method of the present invention, by covering the GaP single crystal with the same type of single crystal powder and a heat insulating sheet, the adhesiveness between the GaP single crystal and the heat insulating sheet and the airtightness with the external atmosphere are improved, and the uniformity of heat is improved. . Furthermore, by first causing the volatilization of P from the single crystal powder, it acts as a stopper and effectively suppresses the volatilization of P from the GaP single crystal. The cylindrical container maintains the shape of the heat insulating sheet, and the presence or absence of this container does not affect the effects of the present invention in any way.
以上詳述したごとく、本発明の方法によれば
(1) 結晶を均一に加熱でき、クラツク発生を招く
ことなく歪を低減できる。 As detailed above, according to the method of the present invention, (1) crystals can be heated uniformly, and distortion can be reduced without causing cracks.
(2) Ｐの揮散が防止でき、結晶重量損失が少い。(2) P volatilization can be prevented and crystal weight loss is small.
(3) 単結晶及び素子加工の歩留り、素子特性が改
善できる。(3) Yield of single crystal and device processing and device characteristics can be improved.
(4) 複雑な装置を必要とせず、操作が簡単であ
る。(4) It does not require complicated equipment and is easy to operate.
等の効果を得ることが出きる。You can obtain effects such as
第１図は本発明の方法により焼鈍する化合物単
結晶の状態を示す図、第２図は本発明の実施例で
用いる横型電気炉の構成を示す図、第３図、第４
図は本発明の効果を説明する図である。
１：GaP単結晶、２：単結晶粉末、３：保温シ
ート、４：円筒容器、５：カーボンフタ、６：炉
芯管、７：発熱体、８：横型電気炉、９：フタ。
FIG. 1 is a diagram showing the state of a compound single crystal annealed by the method of the present invention, FIG. 2 is a diagram showing the configuration of a horizontal electric furnace used in an embodiment of the present invention, FIGS.
The figure is a diagram explaining the effects of the present invention. 1: GaP single crystal, 2: single crystal powder, 3: heat insulation sheet, 4: cylindrical container, 5: carbon lid, 6: furnace core tube, 7: heating element, 8: horizontal electric furnace, 9: lid.
Claims (1)
体単結晶を不活性ガス雰囲気で焼鈍する際に、前
記化合物半導体単結晶と同種の単結晶の粉末及び
カーボンフエルトからなる被覆シートで被覆し、
しかるのち石英製容器に収納した状態で焼鈍する
ことを特徴とする化合物半導体単結晶の焼鈍方
法。 ２ 前記化合物半導体単結晶は、液体カプセル法
によつて製造されたインゴツトであることを特徴
とする特許請求の範囲第１項記載の化合物半導体
単結晶の焼鈍方法。 ３ 前記焼鈍は、開管法により不活性雰囲気中で
行なうことを特徴とする特許請求の範囲第１項記
載の化合物半導体単結晶の焼鈍方法。[Scope of Claims] 1. When a compound semiconductor single crystal produced by a liquid capsule method is annealed in an inert gas atmosphere, the compound semiconductor single crystal is coated with a coating sheet made of a single crystal powder of the same type as the compound semiconductor single crystal and carbon felt. death,
A method for annealing a compound semiconductor single crystal, which is then annealed while being stored in a quartz container. 2. The method of annealing a compound semiconductor single crystal according to claim 1, wherein the compound semiconductor single crystal is an ingot manufactured by a liquid capsule method. 3. The method of annealing a compound semiconductor single crystal according to claim 1, wherein the annealing is performed in an inert atmosphere by an open tube method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10721980A JPS5732643A (en) | 1980-08-06 | 1980-08-06 | Annealing method of compound semiconductor single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10721980A JPS5732643A (en) | 1980-08-06 | 1980-08-06 | Annealing method of compound semiconductor single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5732643A JPS5732643A (en) | 1982-02-22 |
| JPH022840B2 true JPH022840B2 (en) | 1990-01-19 |
Family
ID=14453503
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10721980A Granted JPS5732643A (en) | 1980-08-06 | 1980-08-06 | Annealing method of compound semiconductor single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5732643A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60171300A (en) * | 1984-02-14 | 1985-09-04 | Sumitomo Electric Ind Ltd | Homogenizing method of compound semiconductor crystal |
| JPS61222999A (en) * | 1985-03-27 | 1986-10-03 | Dowa Mining Co Ltd | Method of improving electric characteristics of single crystal of compound semiconductor of group iii-v |
| JPH0831461B2 (en) * | 1986-03-06 | 1996-03-27 | 三菱化学株式会社 | Method for manufacturing epitaxial wafer for light emitting diode |
| US5093284A (en) * | 1988-05-27 | 1992-03-03 | Hitachi Chemical Company, Ltd. | Process for homogenizing compound semiconductor single crystal in properties |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5346070B2 (en) * | 1972-04-04 | 1978-12-11 | ||
| JPS526143B2 (en) * | 1972-07-26 | 1977-02-19 | ||
| JPS5361269A (en) * | 1976-11-15 | 1978-06-01 | Hitachi Ltd | Heat treatment of compound semiconductor |
-
1980
- 1980-08-06 JP JP10721980A patent/JPS5732643A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5732643A (en) | 1982-02-22 |
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