JPS59102895A - Method for controlling diameter of single crystal - Google Patents
Method for controlling diameter of single crystalInfo
- Publication number
- JPS59102895A JPS59102895A JP21286282A JP21286282A JPS59102895A JP S59102895 A JPS59102895 A JP S59102895A JP 21286282 A JP21286282 A JP 21286282A JP 21286282 A JP21286282 A JP 21286282A JP S59102895 A JPS59102895 A JP S59102895A
- Authority
- JP
- Japan
- Prior art keywords
- single crystal
- diameter
- crystal
- circuit
- 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.)
- Pending
Links
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
- C30B15/20—Controlling or regulating
- C30B15/22—Stabilisation or shape controlling of the molten zone near the pulled crystal; Controlling the section of the crystal
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
Abstract
Description
【発明の詳細な説明】
（技術分野）
本発明は、チョクラルスキー法（以下、ＣＺ法と称す）
により半導体又は酸化物単結晶を引上げる際、単結晶の
直径を制御する方法に関するものである。[Detailed Description of the Invention] (Technical Field) The present invention relates to the Czochralski method (hereinafter referred to as CZ method).
This invention relates to a method for controlling the diameter of a single crystal when pulling a semiconductor or oxide single crystal.
（背景技術）
ＣＺ法は、第１図に例を示すように、ヒーター２により
加熱されたるつぼ１内に原料融液３を収容し、原料融液
３表面に種結晶４を浸漬し、なじませた後、種結晶４を
回転し々から引上げて単結晶５を引上げる方法である。(Background Art) As shown in FIG. 1, in the CZ method, a raw material melt 3 is placed in a crucible 1 heated by a heater 2, and a seed crystal 4 is immersed on the surface of the raw material melt 3. This is a method of pulling the single crystal 5 by rotating the seed crystal 4 and then pulling it up.
この単結晶５の直径の制御は、従来、図に示すような目
視法、又は重量法もしくは光学的方法を構造によっては
不可能な場合がある。す々わち、炉の構造上斜め上方か
ら見るため、のぞき窓を設けても原料蒸気により曇り、
観測が不＝Ｊ能になることが多く、又結晶径が細る方向
にある時は、結晶成長界面の観測ができなくなり、成長
界面の観測が非常に難かしい。重量法、光学的方法は設
備が複雑となるため、高価となる欠点がある。Conventionally, the diameter of the single crystal 5 cannot be controlled by a visual method as shown in the figure, a gravimetric method, or an optical method depending on the structure. Due to the structure of the furnace, it can be viewed from diagonally above, so even if a peephole is installed, it will become cloudy due to the raw material steam.
Observation often becomes impossible, and when the crystal diameter is in the direction of decreasing, it becomes impossible to observe the crystal growth interface, making observation of the growth interface very difficult. The gravimetric method and the optical method require complicated equipment and have the disadvantage of being expensive.
（発明の開示）
本発明は、上述の問題点を解決するため成されたもので
、高価な設備を必要とせず、成長界面を観測しなくても
単結晶の直径の変化を簡単に検知することができる単結
晶の１１径制御方法を提供批せんとするものである。(Disclosure of the Invention) The present invention was made to solve the above-mentioned problems, and it is possible to easily detect changes in the diameter of a single crystal without requiring expensive equipment and without observing the growth interface. The purpose of the present invention is to provide a method for controlling the diameter of a single crystal.
木発８１１は、チョクラルスキー法により単結晶を引上
げる方法において、種結晶と原料融液の間の電気抵抗を
連続的に測定し、該電気抵抗の変化により前記単結晶の
直径の変化を検知することを特徴とする即結晶の直径制
御方法である。Kihatsu 811 is a method of pulling a single crystal using the Czochralski method, in which the electrical resistance between the seed crystal and the raw material melt is continuously measured, and the change in the diameter of the single crystal is determined by the change in electrical resistance. This is a method for controlling the diameter of an instant crystal, which is characterized by detecting the diameter.
本発明により引上げられる単結晶は、酸化物（ｉｕｌ
、 Ｂｊ １２ Ｓ ｊ ０２０ ＋ Ｂｌ １２ Ｇ
ｅ ０２０等八又へ周期律表のｌ−Ｖ族化合物（例、Ｇ
ａＡｓ、 ＧａＰ、 ＩｎＳｂ。The single crystal pulled by the present invention is an oxide (iul)
, Bj 12 S j 020 + Bl 12 G
e 020, etc. to the l-V group compounds of the periodic table (e.g., G
aAs, GaP, InSb.
ｌｎＰ、 ＩｎＡｓ−等）、Ｓｉ、Ｇｅ等の半導体よ
り成るものである。It is made of semiconductors such as InP, InAs-, etc.), Si, and Ge.
以下、本発明を図面を用いて実施例により説、川、 す
る。第２図は本発明方法の実施例に用いられる単結晶育
成炉の例を示す縦μｓ１曲図である。図において第１図
と同一の符号にｔそれぞれ同一の部分を示す。Hereinafter, the present invention will be explained by way of examples using drawings. FIG. 2 is a vertical μs 1 curve diagram showing an example of a single crystal growth furnace used in an embodiment of the method of the present invention. In the figure, the same reference numerals as in FIG. 1 indicate the same parts.
図において、シード棒６の下端に収付けられだ種結晶４
に白金線７の一端が接続され、白金線７はシード棒６を
伝い、他端は白金箔製のスリスプリング８に接続されて
いる。スリップリング８に接続されたリード線９は抵抗
１０、回路電源１１を通り、他端は原料融液３を収容し
た白金製るつぼ１に接続されている。 １２は電圧レコ
ーダーである。回路電源１１としては電池又は回路内の
熱起電力が利用される。又測定器としては、電気抵抗又
はそれＫｔｌ：Ｉ当する他の電気的測定値を測定するも
ので、回路の構造、電源の種類により、電流計、電圧計
、抵抗測定器などが用いられる。In the figure, a seed crystal 4 is housed at the lower end of the seed rod 6.
One end of a platinum wire 7 is connected to the seed rod 6, and the other end is connected to a pick spring 8 made of platinum foil. A lead wire 9 connected to the slip ring 8 passes through a resistor 10 and a circuit power supply 11, and the other end is connected to a platinum crucible 1 containing a raw material melt 3. 12 is a voltage recorder. As the circuit power source 11, a battery or a thermal electromotive force within the circuit is used. The measuring device is one for measuring electrical resistance or other electrical measurement values corresponding to Ktl:I, and may be an ammeter, a voltmeter, a resistance measuring device, etc. depending on the circuit structure and the type of power source.
このような回路を形成し、種結晶４と原料融液３の間に
電圧を印加すると、種結晶４−単結晶５−原料融液３を
通って電流が流れ抵抗１０、電圧レコーダー１２により
電流が測定される。この場合、回路を流れる電流は、単
結晶５の長さと結晶成長界面１３の接触面積に依存する
。すなわち、引」−けを行なっている時は単結晶５の長
さが長くなるに従って抵抗が増Ｉ７、電流は単調に減少
する。若し引上げ途中に成長界面１３で単結晶５の直径
の変化があれば、その自在Ｋ Ａｒ〉Ｕて担″抗が斐化
し、電流か変化する。When such a circuit is formed and a voltage is applied between the seed crystal 4 and the raw material melt 3, a current flows through the seed crystal 4 - single crystal 5 - raw material melt 3 and is detected by the resistor 10 and the voltage recorder 12. is measured. In this case, the current flowing through the circuit depends on the length of the single crystal 5 and the contact area of the crystal growth interface 13. That is, when drawing is performed, as the length of the single crystal 5 becomes longer, the resistance increases I7 and the current decreases monotonically. If there is a change in the diameter of the single crystal 5 at the growth interface 13 during the pulling process, the free KAr>U carrier resistance changes and the current changes.
又回路電源１１．１！： して回路の熱起電力を利用し
た場合にＬＬ電圧レコーダー１２により電１１か測定さ
れ、同様に若し成長界面１３で単結晶５の直径の変化か
あれば、その内径に応じて電圧が変化する。Also circuit power supply 11.1! : When the thermal electromotive force of the circuit is used, the voltage 11 is measured by the LL voltage recorder 12, and similarly, if there is a change in the diameter of the single crystal 5 at the growth interface 13, the voltage will change according to the inner diameter. Change.
従って−Ｅ述の電流又は電圧１１１′Ｉの変化を監視す
ることにより結晶径の大体の変化を知ることができ、そ
れによって単結晶の直径制御を定性的に行なうことがで
きる。この場合、電流又は電圧の大きさから成長界面１
３の面積（結晶径に相当）を定性的に検出することがで
きるので、それにｋｔ３して成長界面１３句近の〃ｉ（
度を調節すれば良い。Therefore, by monitoring the change in the current or voltage 111'I mentioned in -E, it is possible to know the approximate change in the crystal diameter, thereby making it possible to qualitatively control the diameter of the single crystal. In this case, due to the magnitude of the current or voltage, the growth interface 1
Since the area of 3 (corresponding to the crystal diameter) can be qualitatively detected, kt3 is added to it to calculate the area of 〃i(
Just adjust the degree.
（実施例）
第２図に示すような単結晶育成炉を使用し、ｌ内径３０
ｍ ｍのヒ゛スマスシリコンオキサイド（Ｂｉ１２Ｓ
ｌ ０２０ ）単結晶を引上げた。(Example) Using a single crystal growth furnace as shown in Fig. 2,
mm of bismuth silicon oxide (Bi12S
l 020 ) A single crystal was pulled.
回路の電源としては、電池の代りに回路内の熱起電力を
利用した。結晶原料約６００ｇを白金製るつぼ１に充埴
した後、約９００℃で加熱融解した。As the power source for the circuit, thermoelectromotive force within the circuit was used instead of batteries. Approximately 600 g of the crystal raw material was charged into platinum crucible 1, and then heated and melted at approximately 900°C.
引上げ中、回路の電圧をレコーダー１２により連続的に
記録した。第３図は得られた単結晶の断面形状とそれに
対応する電圧の変化のレコードを示す図である。During the pulling, the voltage of the circuit was continuously recorded by the recorder 12. FIG. 3 is a diagram showing a record of the cross-sectional shape of the obtained single crystal and the corresponding change in voltage.
第３図に示すように、種結晶が原料融液に接触しない状
態では回路に電流は流れず、レコーダーに信号は現われ
ないが、種結晶が原料融液に接触すると約０．４ｍＶの
電圧が観測され、引上げと共に中結晶５の直径が増大す
るにつれ、電圧の上昇が観測された。直径が変化しない
単結晶５の直胴部では、単結晶の長さが長くなるに従っ
て抵抗が増加し電圧はゆるやかに低下する（範囲Ａ）が
、この状態での単結晶の直径の変化は数１０μ■の変化
で、電圧変化の異常は充分観測ｉｆ能であり、それによ
り成長界面の温度を調節し、直径を制御することは６ノ
能であった。ｂｖ長界曲の目視ｄ、はとんど行なわなか
った。As shown in Figure 3, when the seed crystal is not in contact with the raw material melt, no current flows in the circuit and no signal appears on the recorder, but when the seed crystal is in contact with the raw material melt, a voltage of approximately 0.4 mV is generated. An increase in voltage was observed as the diameter of the middle crystal 5 increased with pulling. In the straight body of the single crystal 5, where the diameter does not change, as the length of the single crystal increases, the resistance increases and the voltage gradually decreases (range A), but in this state, the change in the diameter of the single crystal is only a few seconds. With a change of 10 μι, the abnormality of the voltage change was sufficiently observable, and thereby it was possible to adjust the temperature of the growth interface and control the diameter. Visual inspection of the bv long world song was rarely performed.
単結晶であった。It was a single crystal.
（発明の効果）
上述のように構成された本発明の単結晶の直径制御方法
は次のような効果かある。(Effects of the Invention) The single crystal diameter control method of the present invention configured as described above has the following effects.
（イ）種結晶上原料融液の間の電気抵抗を連続的に測定
し、該電気抵抗の変化によりｖｒＩ記単結晶の直径の変
化を検知するから、結晶成長界面での接触抵抗の面積依
存性を利用しているため、回路内Ω電気的接触を保証す
る金属線を新だに設置するだけで、高価な設備を必要と
せず、他の直径制御装置のない単結晶育成炉でも簡単に
単結晶の直径の変化を検知でき、それに応じて単結晶の
直径の制御を定性的に行なうことができる。(b) Since the electrical resistance between the seed crystal and the raw material melt is continuously measured, and the change in the diameter of the vrI single crystal is detected from the change in electrical resistance, the contact resistance at the crystal growth interface depends on the area. Because it takes advantage of the characteristics, it does not require expensive equipment by simply installing a new metal wire to ensure ohm electrical contact in the circuit, and can easily be used in single crystal growth furnaces without other diameter control devices. Changes in the diameter of the single crystal can be detected, and the diameter of the single crystal can be qualitatively controlled accordingly.
（ロ）納品成長界面を見ることができないような構造の
中結晶育成炉においても、抵抗測定により単結晶の直径
の大体の変化を知ることができ、それにより弔結晶の直
径の制御を定性的に行なうことができる。(b) Even in medium-sized crystal growth furnaces with a structure that makes it impossible to see the growth interface, it is possible to know the approximate change in the diameter of a single crystal by measuring resistance, which allows qualitative control of the diameter of a single crystal. can be done.
第１図は従来の単結晶育成炉の例を示す縦断面図である
。
第２図は本発明方法の実施例に用いられる単結晶育成炉
の例を示す縦断面図である。
第３図は本発明方法の実施例により得られ単結晶の断面
形状とそれに対応する電圧の変化のレコードを示す図で
ある。
１− るつぼ、２− ヒーター、３−原料融液、４−
種結晶、５−単結晶、６−シード捧、７−白金線、８−
スリップリング、９− リード線、１０−抵抗、１１
− 回路電源、１２−電圧レコーダー、１３− 結晶成
長界面、Ａ−範囲。FIG. 1 is a longitudinal sectional view showing an example of a conventional single crystal growth furnace. FIG. 2 is a longitudinal sectional view showing an example of a single crystal growth furnace used in an embodiment of the method of the present invention. FIG. 3 is a diagram showing a record of the cross-sectional shape of a single crystal obtained by an embodiment of the method of the present invention and the corresponding change in voltage. 1- Crucible, 2- Heater, 3- Raw material melt, 4-
Seed crystal, 5-single crystal, 6-seed, 7-platinum wire, 8-
Slip ring, 9- Lead wire, 10- Resistor, 11
- circuit power supply, 12- voltage recorder, 13- crystal growth interface, A- range.
Claims (2)
において、種結晶と原料融液の間の電気抵抗を連続的に
測定し、該電気抵抗の変化により前記単結晶の直径の変
化を検知することを特徴とする単結晶の直径制御方法。(1) In a method of pulling a single crystal using the Czochralski method, the electrical resistance between the seed crystal and the raw material melt is continuously measured, and the change in the diameter of the single crystal is detected from the change in the electrical resistance. A method for controlling the diameter of a single crystal, characterized by:
路内の熱起電力を用いて行なわれる特許請求の範囲第１
項記載の単結晶の直径制御方法。(2) The measurement of electrical resistance is carried out using a battery or thermoelectromotive force within the circuit as a power source of the circuit. Claim 1
Method for controlling the diameter of a single crystal as described in Section 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21286282A JPS59102895A (en) | 1982-12-03 | 1982-12-03 | Method for controlling diameter of single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21286282A JPS59102895A (en) | 1982-12-03 | 1982-12-03 | Method for controlling diameter of single crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS59102895A true JPS59102895A (en) | 1984-06-14 |
Family
ID=16629526
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21286282A Pending JPS59102895A (en) | 1982-12-03 | 1982-12-03 | Method for controlling diameter of single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59102895A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61136989A (en) * | 1984-12-05 | 1986-06-24 | Toshiba Ceramics Co Ltd | Method for controlling shape of single crystal while growing in pulling method |
| US10512959B2 (en) * | 2014-04-03 | 2019-12-24 | Pusan National University Industrial-University Cooperation Foundation | Method for manufacturing single-crystalline metal ultrafine wire |
-
1982
- 1982-12-03 JP JP21286282A patent/JPS59102895A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61136989A (en) * | 1984-12-05 | 1986-06-24 | Toshiba Ceramics Co Ltd | Method for controlling shape of single crystal while growing in pulling method |
| US10512959B2 (en) * | 2014-04-03 | 2019-12-24 | Pusan National University Industrial-University Cooperation Foundation | Method for manufacturing single-crystalline metal ultrafine wire |
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