JPH0310598B2 - - Google Patents
Info
- Publication number
- JPH0310598B2 JPH0310598B2 JP57144073A JP14407382A JPH0310598B2 JP H0310598 B2 JPH0310598 B2 JP H0310598B2 JP 57144073 A JP57144073 A JP 57144073A JP 14407382 A JP14407382 A JP 14407382A JP H0310598 B2 JPH0310598 B2 JP H0310598B2
- Authority
- JP
- Japan
- Prior art keywords
- silicon
- crucible
- single crystal
- molten
- molten silicon
- 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
-
- 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
- C30B15/02—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt
- C30B15/04—Single-crystal growth by pulling from a melt, e.g. Czochralski method adding crystallising materials or reactants forming it in situ to the melt adding doping materials, e.g. for n-p-junction
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)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
Description
【発明の詳細な説明】
本発明は制御された酸素濃度を有するシリコン
単結晶を製造する方法およびその装置に関するも
のである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method and apparatus for producing a silicon single crystal with a controlled oxygen concentration.
一般にシリコン単結晶はCZ法においては石英
ガラス製ルツボが使用され、この石英ガラスルツ
ボ中でシリコンを溶融し、種結晶を使用して引き
上げられる。この際、石英ガラスは一部溶融シリ
コンに溶解し、酸素がシリコン単結晶中に混入す
る。このシリコン単結晶の酸素濃度は融液シリコ
ンと石英ガラスルツボの接触面積、温度、対流の
大きさ等によつて決まり、品質管理上改善が求め
られていたが、これをコントロールすることは困
難であつた。 Generally, silicon single crystals are produced using a quartz glass crucible in the CZ method, and silicon is melted in the quartz glass crucible and pulled using a seed crystal. At this time, a portion of the quartz glass is dissolved in the molten silicon, and oxygen is mixed into the silicon single crystal. The oxygen concentration of this silicon single crystal is determined by the contact area between the molten silicon and the silica glass crucible, the temperature, the size of convection, etc., and there has been a need to improve it for quality control purposes, but it is difficult to control this. It was hot.
最近、窒化珪素あるいは炭化珪素を利用したル
ツボを使用してシリコン単結晶を引き上げる技術
が開発されたが、これらの場合はルツボからの酸
素混入がないため、シリコンウエーハの酸化処理
あるいは拡散処理等の熱処理に際し無酸素構造に
伴なうウエーハのひずみ（スリツプ）が発生しや
すくなり、LSIや超LSI等の精密な材質であるこ
とを要求される用途においては問題となつてい
た。 Recently, a technique for pulling silicon single crystals using a crucible made of silicon nitride or silicon carbide has been developed, but in these cases, there is no oxygen contamination from the crucible, so it is difficult to perform oxidation or diffusion treatments on silicon wafers. During heat treatment, wafer distortion (slip) due to the oxygen-free structure tends to occur, which has become a problem in applications that require precision materials such as LSI and super LSI.
本発明は、シリコン単結晶を所定の酸素濃度と
すべく、少なくとも内表面の全面がSi3N4または
SiCからなるルツボを用い、このルツボ内の溶融
シリコンに、重量物を内封した酸化珪素を沈積し
たり、あるいは酸化珪素塊を融解シリコン表面か
ら浸漬することにより、溶融シリコンに対し必要
量の酸素を融解させるようにしたものである。 In the present invention, at least the entire inner surface is made of Si 3 N 4 or
By using a crucible made of SiC and depositing silicon oxide containing a heavy object into the molten silicon in the crucible, or by immersing a silicon oxide lump from the surface of the molten silicon, the necessary amount of oxygen can be supplied to the molten silicon. It is designed to melt.
以下に本発明の実施例を図を参照して説明す
る。 Embodiments of the present invention will be described below with reference to the drawings.
第１図において、１はカーボンを基材２としそ
の内表面にコーテイングした窒化珪素膜である。
３は溶融シリコン、４は引き上げつつあるシリコ
ン単結晶である。５が本発明にかゝる装填物で第
２図に示す如く、溶融シリコンより比重を大きく
するために石英ガラス外管６内にタングステン棒
７を封入した構造を有しており、シリコン融液中
に沈積されている。 In FIG. 1, reference numeral 1 denotes a silicon nitride film having a carbon base material 2 coated on its inner surface.
3 is molten silicon, and 4 is a silicon single crystal that is being pulled. 5 is a charge according to the present invention, and as shown in FIG. 2, it has a structure in which a tungsten rod 7 is enclosed in a quartz glass outer tube 6 in order to make the specific gravity larger than that of molten silicon. deposited inside.
本発明のものはこのように構成されており、溶
融シリコンはルツボからの酸素の混入がない代り
にシリコン融液中に沈積されている石英ガラスが
その表面から溶融し、シリコン融液の酸素濃度
を、ひいてはシリコン単結晶中の酸素濃度を特定
することになる。酸素濃度を制御するには溶融シ
リコンと接触している石英ガラスの表面積量、温
度等に比例するから、これによつて必要な条件を
決定することができる。 The device of the present invention is constructed as described above, and instead of the molten silicon being mixed with oxygen from the crucible, the quartz glass deposited in the silicon melt melts from its surface, and the oxygen concentration of the silicon melt increases. This will ultimately determine the oxygen concentration in the silicon single crystal. Since the oxygen concentration is proportional to the amount of surface area of the quartz glass in contact with the molten silicon, the temperature, etc., the necessary conditions can be determined based on this.
第３図は石英ガラスの接触方法を第１図の場合
の如く沈積するのではなく、石英ガラス製棒状体
８を上方で支持することによつて浸漬する方法を
示している。溶融シリコンと接触する石英ガラス
の面積を調節するには矢印で示すように石英ガラ
ス製棒状体を上下させ、あるいは必要に応じて複
数本を同時使用すればよい。このような棒状体を
使用した場合は溶融シリコンの撹拌が容易に行な
えるという利点もある。 FIG. 3 shows a method of contacting the quartz glass, not by depositing it as in FIG. 1, but by immersing it by supporting the quartz glass rod 8 above. To adjust the area of the quartz glass that comes into contact with the molten silicon, the quartz glass rod can be moved up and down as shown by the arrows, or if necessary, multiple rods can be used at the same time. When such a rod-shaped body is used, there is an advantage that the molten silicon can be easily stirred.
第１図および第３図の方法によつて溶融シリコ
ン４Kgから４インチシリコン単結晶を引き上げた
が、石英ガラスの接触表面積を50cm2の状態に保つ
たまゝ、シリコン単結晶を引き上げた場合におけ
るシリコン単結晶の長さ方向の酸素濃度の変化す
る状態を第４図に示す。参考迄に石英ガラスルツ
ボを使用した場合(A)およびSi3N4製ルツボを使用
した場合(B)について併記したが、図に示すように
石英ガラスルツボを使用した場合は長さ方向に大
きく変動するのに対し、本発明の場合はほとんど
変化していない。一方、窒化珪素ルツボを使用し
た場合は酸素濃度が極端に低く、かつこれを増減
させることはできない。 A 4-inch silicon single crystal was pulled from 4 kg of molten silicon by the method shown in Figures 1 and 3 . FIG. 4 shows how the oxygen concentration changes along the length of the single crystal. For reference, we have also listed the case where a quartz glass crucible is used (A) and the case where a Si 3 N 4 crucible is used (B), but as shown in the figure, when a quartz glass crucible is used, the length is larger However, in the case of the present invention, there is almost no change. On the other hand, when a silicon nitride crucible is used, the oxygen concentration is extremely low and cannot be increased or decreased.
本発明のものにおいては、溶融シリコン４Kgに
対し石英ガラスの表面積を50cm2とした場合、(C)、
(D)の酸素濃度が７〜９×1017atoms〔cm-3〕とほゞ
一定であり、また石英ガラスの表面積を変えるこ
とによつてシリコン単結晶の長さ方向にはほゞ一
定のまゝ酸素濃度を容易に変化させることができ
る。 In the case of the present invention, when the surface area of quartz glass is 50 cm 2 for 4 kg of molten silicon, (C),
The oxygen concentration in (D) is approximately constant at 7 to 9×10 17 atoms [cm -3 ], and by changing the surface area of the silica glass, it is approximately constant in the length direction of the silicon single crystal. Well, the oxygen concentration can be easily changed.
SiO2の溶出量と結晶中の酸素濃度との関係を
第５図に示す。 FIG. 5 shows the relationship between the amount of SiO 2 eluted and the oxygen concentration in the crystal.
なお実施例においては、カーボン基材の内表面
に窒化珪素をコーテイングしたルツボを使用した
が、炭化珪素をコーテイングしたものでも同等の
効果が得られ、また窒化珪素あるいは炭化珪素単
味のもの、若しくはその複合体からなるルツボを
使用したものであつてもよい。また酸化珪素は石
英ガラスが高純度として容易に入手しやすいもの
であるが、一酸化珪素あるいは水晶のようなもで
もよい。更に石英ガラスを溶融シリコンに接触さ
せるには石英ガラスの比重溶融シリコンより小さ
いため、工夫が必要であるが、実施例の場合に限
られたものではない。 In the examples, a crucible in which the inner surface of a carbon base material is coated with silicon nitride is used, but the same effect can be obtained with a crucible coated with silicon carbide. A crucible made of the composite may be used. As for silicon oxide, quartz glass is easily available as it has a high purity, but silicon monoxide or crystal may also be used. Further, in order to bring quartz glass into contact with molten silicon, some measures are required since the specific gravity of quartz glass is smaller than that of molten silicon, but this is not limited to the case of the embodiment.
以上のように本発明によれば、少なくとも内表
面の全面がSi3N4またはSiCからならルツボを用
い、このルツボ内の溶融シリコンに、重量物を内
封した酸化珪素を沈積したり、あるいは酸化珪素
塊を溶融シリコン表面から浸漬するようにしたの
で、上記酸化珪素の沈積量を増減したり、あるい
は酸化珪素塊の浸漬量を増減することにより、シ
リコン単結晶中の酸素濃度を簡易に調節すること
ができ、又、単結晶育成中における酸素濃度も自
由かつ微細に変更することができると共に、ルツ
ボが溶融シリコンに侵食されることがなく、重量
物を内封した酸化珪素等を新しいものに交換する
ことによつてルツボの長期間使用が可能となる。 As described above, according to the present invention, if at least the entire inner surface is made of Si 3 N 4 or SiC, a crucible is used, and silicon oxide containing a heavy object is deposited on the molten silicon in the crucible, or Since the silicon oxide lump is immersed from the surface of the molten silicon, the oxygen concentration in the silicon single crystal can be easily adjusted by increasing or decreasing the amount of silicon oxide deposited or by increasing or decreasing the immersion amount of the silicon oxide lump. In addition, the oxygen concentration during single crystal growth can be freely and minutely changed, and the crucible is not eroded by molten silicon, making it possible to produce new products such as silicon oxide containing heavy objects. The crucible can be used for a long period of time by replacing the crucible with a new one.
図は本発明の実施例を示し、第１図、第３図は
本発明方法を実施する装置の概略縦断正面図、第
２図は装填物を示す概略縦断正面図、第４図はシ
リコン単結晶の長さ方向の酸素濃度の変化する状
態を示す図、第５図はSiO2の溶出量と結晶中の
酸素濃度との関係を示す図である。
１……窒化珪素膜、２……カーボン基材、３…
…溶融シリコン、４……シリコン単結晶、５……
装填物、６……石英ガラス外管、７……タングス
テン棒、８……石英ガラス製棒状体。
The figures show embodiments of the present invention; FIGS. 1 and 3 are schematic longitudinal sectional front views of an apparatus for carrying out the method of the invention; FIG. 2 is a schematic longitudinal sectional front view showing a charge; and FIG. FIG. 5 is a diagram showing how the oxygen concentration changes in the length direction of the crystal, and FIG. 5 is a diagram showing the relationship between the amount of SiO 2 eluted and the oxygen concentration in the crystal. 1...Silicon nitride film, 2...Carbon base material, 3...
...molten silicon, 4...silicon single crystal, 5...
Loading materials, 6... quartz glass outer tube, 7... tungsten rod, 8... quartz glass rod-shaped body.
Claims (1)
を引き上げるに際し、少なくとも内表面の全面が
Si3N4またはSiCからなるルツボを用い、このル
ツボ内の溶融シリコンに重量物を内封した酸化珪
素を沈積することを特徴とするシリコン単結晶の
製造方法。 ２ ルツボ内の溶融シリコンからシリコン単結晶
を引き上げるに際し、少なくとも内表面の全面が
Si3N4またはSiCからなるルツボを用い、このル
ツボ内の溶融シリコンに酸化珪素塊を溶融シリコ
ン表面から浸漬することを特徴とするシリコン単
結晶の製造方法。 ３ 酸化珪素が一酸化珪素または二酸化珪素であ
ることを特徴とする特許請求の範囲第１項又は第
２項記載のシリコン単結晶の製造方法。 ４ ルツボ内の溶融シリコンからシリコン単結晶
を引き上げる装置であつて、少なくとも内表面の
全面がSi3N4またはSiCからなるルツボと、この
ルツボ内の溶融シリコンに沈積される重量物を内
封した酸化珪素とを備えたことを特徴とするシリ
コン単結晶の製造装置。 ５ ルツボ内の溶融シリコンからシリコン単結晶
を引き上げる装置であつて、少なくとも内表面の
全面がSi3N4またはSiCからなるルツボと、この
ルツボ内の溶融シリコンに浸漬される酸化珪素塊
と、この酸化珪素塊をルツボ上方において支持す
る支持具とを備えたことを特徴とするシリコン単
結晶の製造装置。[Claims] 1. When pulling a silicon single crystal from molten silicon in a crucible, at least the entire inner surface is
1. A method for producing a silicon single crystal, which comprises using a crucible made of Si 3 N 4 or SiC, and depositing silicon oxide containing a heavy substance in molten silicon in the crucible. 2 When pulling a silicon single crystal from molten silicon in the crucible, at least the entire inner surface is
1. A method for producing a silicon single crystal, comprising using a crucible made of Si 3 N 4 or SiC, and immersing a silicon oxide lump into molten silicon from the surface of the molten silicon in the crucible. 3. The method for producing a silicon single crystal according to claim 1 or 2, wherein the silicon oxide is silicon monoxide or silicon dioxide. 4 A device for pulling silicon single crystals from molten silicon in a crucible, which includes a crucible whose entire inner surface is made of Si 3 N 4 or SiC, and a heavy object to be deposited on the molten silicon in this crucible. A silicon single crystal manufacturing device characterized by comprising silicon oxide. 5 A device for pulling silicon single crystals from molten silicon in a crucible, which comprises a crucible whose entire inner surface is made of Si 3 N 4 or SiC, a silicon oxide lump immersed in the molten silicon in the crucible, and 1. An apparatus for manufacturing a silicon single crystal, comprising: a support for supporting a silicon oxide lump above a crucible.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14407382A JPS5935094A (en) | 1982-08-20 | 1982-08-20 | Method and apparatus for preparation of silicon single crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14407382A JPS5935094A (en) | 1982-08-20 | 1982-08-20 | Method and apparatus for preparation of silicon single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5935094A JPS5935094A (en) | 1984-02-25 |
| JPH0310598B2 true JPH0310598B2 (en) | 1991-02-14 |
Family
ID=15353648
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14407382A Granted JPS5935094A (en) | 1982-08-20 | 1982-08-20 | Method and apparatus for preparation of silicon single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5935094A (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20030052467A (en) * | 2001-12-21 | 2003-06-27 | 주식회사 실트론 | Graphite Crucible |
| US7635414B2 (en) | 2003-11-03 | 2009-12-22 | Solaicx, Inc. | System for continuous growing of monocrystalline silicon |
| KR100693917B1 (en) | 2004-12-31 | 2007-03-12 | 주식회사 실트론 | Silicon single crystal |
| JP4499698B2 (en) * | 2006-10-04 | 2010-07-07 | 昭和電工株式会社 | Method for producing silicon carbide single crystal |
| KR101063250B1 (en) * | 2008-10-16 | 2011-09-07 | 한국에너지기술연구원 | Graphite Crucible for Silicon Electromagnetic Induction Melting |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5678496A (en) * | 1979-11-30 | 1981-06-27 | Toshiba Ceramics Co Ltd | Quartz glass crucible for pulling silicon single crystal |
| JPS5771894A (en) * | 1980-10-16 | 1982-05-04 | Toshiba Corp | Preparation of single crystal of semiconductor |
-
1982
- 1982-08-20 JP JP14407382A patent/JPS5935094A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5935094A (en) | 1984-02-25 |
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