JPS59111994A - How to grow crystals - Google Patents

How to grow crystals

Info

Publication number
JPS59111994A
JPS59111994A JP22068082A JP22068082A JPS59111994A JP S59111994 A JPS59111994 A JP S59111994A JP 22068082 A JP22068082 A JP 22068082A JP 22068082 A JP22068082 A JP 22068082A JP S59111994 A JPS59111994 A JP S59111994A
Authority
JP
Japan
Prior art keywords
crucible
melt
crystal
holes
growing
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
Application number
JP22068082A
Other languages
Japanese (ja)
Inventor
Tetsuo Fukuda
哲生 福田
Iesada Hirai
平井 家定
Kazunari Amano
尼野 一成
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Fujitsu Ltd
Original Assignee
Fujitsu Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Fujitsu Ltd filed Critical Fujitsu Ltd
Priority to JP22068082A priority Critical patent/JPS59111994A/en
Publication of JPS59111994A publication Critical patent/JPS59111994A/en
Pending legal-status Critical Current

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
    • C30B15/30—Mechanisms for rotating or moving either the melt or the crystal
    • C30B15/305—Stirring of the melt

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

PURPOSE:To extrude the influence of heat convection and turbulent flow and to grow crystal with low oxygen concentration, by providing the inside of a crucible to put melt in it with the second crucible for growing crystal having a sh allow bottom and holes on the side face. CONSTITUTION:The inside of the crucible 1 to put the Si melt 12 in it is provided with the crucible 9 made of the same material having a shallow bottom and the plural through holes 10 on the side face in such a way that it is hung by the Mo wire 11 and fixed to the center of the crucible 1. The melt 12 is introduced through the holes 10 to the crucible 9, the tip of a seed crystal is brought into contact with the melt 12 in the crucible 9, and the grown crystal 4 is pulled up. A carbon heater to heat and to melt a semiconductor material for growth and to maintain a molten state is set at the outer periphery of the crucible 1. Consequently, a tubulent flow occuring from the bottom of the crucible 1 is cut off, heat convection reaches the liquid level, the Si melt which has released oxygen with high concentration in the form of SiO2 is introduced from the holes 10 to the crucible 9. Since the crucible 9 has the shallow bottom, and heat convection will not occur.

Description

【発明の詳細な説明】 (al  発明の技術分野 本発明は、融液中の乱流および熱対流の゛影響を遮断し
た結晶の成長方法に関する。
DETAILED DESCRIPTION OF THE INVENTION Technical Field of the Invention The present invention relates to a method for growing crystals in which the effects of turbulence and thermal convection in a melt are blocked.

(bl  技術の背景 IC,)ランジスタなどの半導体素子はシリコン(Si
)、カリウム砒素(QaAs)などの単結晶基板を用い
て形成されているが、これらの結晶はチョクラルスキー
法(略称CZ)か或にフローティングゾーン法(略称F
Z法)によって作られている0ここでC2法は大直径化
が可能な点でまたF’Z法は高純度のものが得られ易い
点に特徴があや。半導体デバイスの量産化の目的から多
くの場合C2法で得られた結晶が用いられている。
(bl Technology background IC,) Semiconductor elements such as transistors are silicon (Si)
), potassium arsenide (QaAs), etc., but these crystals are formed using the Czochralski method (abbreviated as CZ) or the floating zone method (abbreviated as F).
Here, the C2 method is characterized by the ability to make the diameter large, and the F'Z method is characterized by the fact that it is easy to obtain high-purity products. For the purpose of mass producing semiconductor devices, crystals obtained by the C2 method are often used.

(C)  従来技術と問題点 C2法は成長せんとする単結晶と同一材料からなる多結
晶体を坩堝に入れて不活性ガス中で加熱溶融し、該成長
融液と種結晶とを接触させ、平衡状態を維持し乍ら除々
に引上げることによ9種結晶を核として単結晶体の成長
を行うものである。
(C) Prior art and problems In the C2 method, a polycrystalline body made of the same material as the single crystal to be grown is placed in a crucible, heated and melted in an inert gas, and the growing melt is brought into contact with a seed crystal. By gradually pulling up the crystal while maintaining an equilibrium state, a single crystal is grown using the 9-seed crystal as a nucleus.

ここでIC,)ランジスタなど量産される半導体デバイ
スは特性の均等化およびコスト低減の見地から生産に使
用される結晶基板(ウェハ)の直径は益々犬型化に指向
している。
In mass-produced semiconductor devices such as ICs and transistors, the diameter of the crystal substrate (wafer) used for production is increasingly becoming dog-shaped from the viewpoint of equalizing characteristics and reducing costs.

例えばSiについて言えば径4〔インチ〕長さ1〔W〕
のものは普通であり、径5〔インチ〕のものも作られる
ようになってきている。このように成長結晶の径が大き
く且つ長くなるに従って使用する坩堝もこれに比例して
大型化している。例えは径4〜5〔インチ〕のSi結晶
に使用される石英(Si02)製の坩堝の寸法は直径約
300 〔mm〕、高さ約200 Cmm〕に及び、こ
れに約2o(ky:]の高純度多結晶Siを入れ該坩堝
の周囲に配設されたカーボンヒーター(図示せず)によ
り加熱溶融して融液としている。このように坩堝が大型
化するに従って融液の対流が顕著となシ、この影響が引
上げ結晶に現われてくる。以下現在最も大型の結晶引上
げが行われているSiを例として説明する。
For example, for Si, the diameter is 4 [inches] and the length is 1 [W].
These are common, and those with a diameter of 5 inches are also being made. In this way, as the diameter of the grown crystal becomes larger and longer, the crucible used also becomes larger in proportion. For example, the dimensions of a quartz (Si02) crucible used for Si crystals with a diameter of 4 to 5 [inches] are approximately 300 [mm] in diameter and 200 cm in height, and approximately 2o (ky:). High-purity polycrystalline Si is placed in the crucible and heated and melted into a melt using a carbon heater (not shown) placed around the crucible.As the crucible becomes larger, the convection of the melt becomes more pronounced. However, this effect appears in pulled crystals.Hereinafter, Si, which is currently the largest crystal pulled, will be explained as an example.

第1図はCZ法によりSi単結晶の引上げを行っている
状態での坩堝と成長結晶の要部断面図であって多結晶S
i体を入れた坩堝1はアルゴン(Ar)雰囲気中でこれ
を取り囲んで設けられているカーボンヒーター(図示せ
ず)に通電することにより加熱され多結晶Si体は溶融
して融液2とされている。ここで81の融点は1410
〔℃〕であるため融液の状態を維持するにはこの温度以
上に加熱する必要がある。
Figure 1 is a cross-sectional view of the essential parts of the crucible and the growing crystal when Si single crystal is being pulled by the CZ method.
The crucible 1 containing the i-body is heated in an argon (Ar) atmosphere by energizing a carbon heater (not shown) provided surrounding it, and the polycrystalline Si body is melted into a melt 2. ing. Here, the melting point of 81 is 1410
[°C], so it is necessary to heat it above this temperature to maintain the melt state.

次に結晶成長を行うには引上軸3の先端に固定しである
種結晶の先端を融液2に浸漬し平衡状態を保ち乍ら種結
晶を徐々に引上げることにより直胴形の成長結晶4の成
長が行われる。然し乍ら坩堝1の直径が約3o o C
try〕で深さが約200〔rn声〕あり、この中の融
液の温度が14.00 [:’C:]を越えている条件
下では坩堝底部の融液2の温度は表面部と較べて数10
 [’C:]高く、こね、による熱対流5が生じている
。
Next, for crystal growth, the tip of the seed crystal is fixed to the tip of the pulling shaft 3 and immersed in the melt 2, and while maintaining an equilibrium state, the seed crystal is gradually pulled up to grow a straight body. Growth of crystal 4 takes place. However, the diameter of crucible 1 is approximately 3 o C
Under the conditions that the depth is about 200 [rn voice] and the temperature of the melt in this exceeds 14.00 [:'C:], the temperature of the melt 2 at the bottom of the crucible is equal to that at the surface. Comparative number 10
['C:] High heat convection 5 is occurring due to kneading.

すなわち熱対流5け坩堝1の底部より内壁に沿って生じ
ており成長する単結晶を中心として循還している。ここ
で熱対流5け石英から成る坩堝1の内壁を削るため、坩
堝の構成成分である5ho2が融液2の中に溶は出し、
融液2の中の酸素0)濃度を増加させる。従って成長す
る成長結晶4の中の酸素濃度を増加させる。そこで、従
来熱対流5の結晶品質への影響を緩和する目的で成長結
晶4自身および坩堝1をそれぞれ反対方向に回転させて
いる。ととろが、坩堝1の回転により水平方向に起る強
制諸6に、熱対流5と干渉して禅雑な融液2の揺ぎを起
こしこれが原因して成長結晶4に不純物濃度分布の異る
成長縞を生じ易い。また成長結晶4に回転を与えること
は均一な組成をもつ直胴状の結晶を得るために必要であ
るがこの回転が融液2の表面の中心を掻き回わす結果高
酸素濃度の融液を坩堝1の底部より龍巻き状の乱流7を
生じ、成長結晶4の成長面に近づく。このような熱対流
5を減少させる方法としては底の浅い坩堝を用いて、成
長融液を外部から自動供給する方法も考案されてはいる
が、天川化されるには到っていない。
That is, thermal convection occurs from the bottom of the five-piece crucible 1 along the inner wall and circulates around the growing single crystal. Here, in order to scrape the inner wall of the crucible 1 made of five-quartz quartz, 5ho2, which is a component of the crucible, is dissolved into the melt 2.
Increase the oxygen concentration in the melt 2. Therefore, the oxygen concentration in the growing crystal 4 is increased. Therefore, conventionally, the growing crystal 4 itself and the crucible 1 are rotated in opposite directions for the purpose of alleviating the influence of thermal convection 5 on crystal quality. The melt 2 interferes with the thermal convection 5 in the horizontal forces 6 caused by the rotation of the crucible 1, causing rough fluctuations in the melt 2, which causes a different impurity concentration distribution in the growing crystal 4. Prone to growth streaks. In addition, it is necessary to give rotation to the growing crystal 4 in order to obtain a cylindrical crystal with a uniform composition, but this rotation stirs the center of the surface of the melt 2, resulting in a high oxygen concentration melt. A tornado-shaped turbulent flow 7 is generated from the bottom of the crucible 1 and approaches the growth surface of the growing crystal 4. As a method for reducing such heat convection 5, a method has been devised in which a crucible with a shallow bottom is used and a growing melt is automatically supplied from the outside, but this method has not yet been adopted.

(dl  発明の目的 本発明は熱対流および乱流の影響を遮断し低酸素濃度の
結晶を成長させる方法を提供することを目的とする。
(dl) Object of the Invention The object of the present invention is to provide a method for growing crystals with low oxygen concentration while blocking the influence of thermal convection and turbulence.

(el  発明の構成 本発明の目的は、融液を収容する第1の坩堝の内側に、
底が浅く月つ側面穴を有する第2の坩堝を備え、該第2
の坩堝中の融液に種結晶を接触して結晶成長を行うこと
により達成することができる。
(el Structure of the Invention The object of the present invention is to
a second crucible with a shallow bottom and a moon-shaped side hole;
This can be achieved by bringing a seed crystal into contact with the melt in a crucible to cause crystal growth.

(f)  発明の実施例 本発明V!第1図において、坩堝1を構成する5i02
が熱対流5により削られて融液2に溶は込むことが引上
げ成長結晶4の酸素0)#度を大きくする原因となって
いるが、仔細に観、察した結果、これは坩堝の内壁に沿
って上昇し循還する熱対流5よりもむしろ中心部に起っ
ている乱流7の影去によることを見出した。その理由σ
熱対流5により坩堝1よす融液2の中に溶出して生じた
高酸素礫度のSi融液は液面8に達すると一酸化硅累(
Sin)の形でかなりの量が蒸発するので、液面8に達
した後の坩堝1の中心部に向う熱対流5の中の酸素濃度
は低いことが予想される。一方坩堝1の底から中心部を
上昇する乱流7は箭酸累濃度のSi融液がそのまま引上
は中の成長結晶4に接する可能性が太きい。このため、
低酸素濃度の成長結晶4を得るには底面からの乱済7を
遮断し液面8に泊って流れる熱対流5をオリ用すればよ
いことになる。
(f) Embodiments of the invention Invention V! In FIG. 1, 5i02 constituting crucible 1
is scraped off by thermal convection 5 and melted into the melt 2, which causes the increase in the oxygen concentration in the pulled-grown crystal 4.As a result of careful observation and observation, we found that this is due to the inner wall of the crucible. It was found that this is due to the shadowing of the turbulent flow 7 occurring in the center rather than the heat convection 5 that rises and circulates along the center. The reason σ
When the Si melt with high oxygen agglomeration, which is eluted into the melt 2 from the crucible 1 by thermal convection 5, reaches the liquid level 8, it becomes silica monoxide (
Since a considerable amount is evaporated in the form of Sin), it is expected that the oxygen concentration in the thermal convection 5 toward the center of the crucible 1 after reaching the liquid level 8 is low. On the other hand, in the turbulent flow 7 rising from the bottom to the center of the crucible 1, there is a high possibility that the Si melt having a cumulative concentration of saline acid will directly come into contact with the growing crystal 4 inside. For this reason,
In order to obtain a grown crystal 4 with a low oxygen concentration, it is sufficient to block the disturbance 7 from the bottom and use the thermal convection 5 flowing on the liquid surface 8.

第2図(5)は本実施例に係る坩堝及び成長結晶の断面
図、同図中JFiこの平面図であり、第、1図で駅、明
した部分と同部分は同記号で指示しである。すなわち内
側に設けた内側坩堝9は坩堝lと同弥材料で6る石英(
SiO2)よυすり、直径tri 200Cynrs〕
深さは80 [my:]と浅く側面に複数11i!il
(本実施例では4個)の直径20〔mπ〕の貫通穴10
を備えると共に例えばモリブデンCMO片線11を用い
て上部より吊り下げて坩堝1の中央部に固定し、該内側
坩堝9中の融液12に浄結晶の先端を接触して成長結体
材料を加熱溶融し溶液状態を維持する為のカーボンヒー
タが配設されている。このようにすれば第1図で示した
坩堝lの底部から生じる乱流7は遮蔽され、熱対R,5
が液面8に達して高濃度の酸素をSiOの形で放出した
Si融液が穴10をf8じて内側坩堝9内に入り、該内
側坩堝9内には酸素イ 龜贋の低い融液12が導入される。Iして該内側坩堝1
2の底は浅いため熱対流が生じない状態で成長結晶4の
引上げ成長が可能となる。
Figure 2 (5) is a cross-sectional view of the crucible and growing crystal according to this example, and a plan view of JFi in the same figure. be. In other words, the inner crucible 9 provided inside is made of quartz (6) made of the same material as the crucible I.
SiO2) cross-section, diameter tri 200Cynrs]
The depth is 80 [my:] and there are multiple 11i on the sides! il
(4 in this example) through holes 10 with a diameter of 20 [mπ]
For example, using a piece of molybdenum CMO wire 11, it is suspended from the upper part and fixed in the center of the crucible 1, and the tip of the purified crystal is brought into contact with the melt 12 in the inner crucible 9 to heat the growing solid material. A carbon heater is provided to maintain the melted solution state. In this way, the turbulent flow 7 generated from the bottom of the crucible l shown in FIG.
reaches the liquid level 8 and releases high concentration oxygen in the form of SiO.The Si melt enters the inner crucible 9 through the hole 10 through f8, and the inner crucible 9 contains the melt with low oxygen content. 12 is introduced. I and the inner crucible 1
Since the bottom of the crystal 2 is shallow, the growing crystal 4 can be pulled up and grown without thermal convection.

本実施例によれは、酸素濃度が1O18〔cm−3〕以
下で成長縞のコントラストが弱い成長結晶が得られる。
According to this example, a grown crystal with an oxygen concentration of 1O18 [cm-3] or less and a weak contrast of growth stripes can be obtained.

(g)  発明の効果 本発明によれは、熱対流及び電流の影俟を遮断し、酸素
濃度の低い結晶をM長させることを可能とする。
(g) Effects of the Invention According to the present invention, it is possible to block the influence of thermal convection and electric current, and to increase the M length of a crystal with a low oxygen concentration.

【図面の簡単な説明】[Brief explanation of the drawing]

図において、1は坩堝、2と12は融液、4は成長結晶
、5は熱対流、6は強制済、7は乱流、9は内側州堝、
10は穴、 第 第2図 11−ヨ;≧2−−≦3ノ (βジ □ρ
In the figure, 1 is the crucible, 2 and 12 are the melt, 4 is the growing crystal, 5 is the thermal convection, 6 is the forced flow, 7 is the turbulent flow, 9 is the inner melt,
10 is a hole, Fig. 2 11-Y; ≧2--≦3ノ

Claims (1)

【特許請求の範囲】[Claims] 融液を収容する第1の坩堝の内側に底が浅く且つ側面に
穴を有するg(H2の坩堝を備え、該第2の坩堝中の融
液に種結晶を接触して結晶成長を行うことを特徴とする
結晶の成長方法。
A first crucible that accommodates the melt has a shallow bottom and a hole on the side. A crucible of H2 is provided, and crystal growth is performed by contacting a seed crystal with the melt in the second crucible. A crystal growth method characterized by:
JP22068082A 1982-12-16 1982-12-16 How to grow crystals Pending JPS59111994A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP22068082A JPS59111994A (en) 1982-12-16 1982-12-16 How to grow crystals

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP22068082A JPS59111994A (en) 1982-12-16 1982-12-16 How to grow crystals

Publications (1)

Publication Number Publication Date
JPS59111994A true JPS59111994A (en) 1984-06-28

Family

ID=16754779

Family Applications (1)

Application Number Title Priority Date Filing Date
JP22068082A Pending JPS59111994A (en) 1982-12-16 1982-12-16 How to grow crystals

Country Status (1)

Country Link
JP (1) JPS59111994A (en)

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