JPH01282194A - Production of single crystal - Google Patents
Production of single crystalInfo
- Publication number
- JPH01282194A JPH01282194A JP13514788A JP13514788A JPH01282194A JP H01282194 A JPH01282194 A JP H01282194A JP 13514788 A JP13514788 A JP 13514788A JP 13514788 A JP13514788 A JP 13514788A JP H01282194 A JPH01282194 A JP H01282194A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- granular
- crucible
- single crystal
- amount
- 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 63
- 238000004519 manufacturing process Methods 0.000 title claims description 27
- 239000002994 raw material Substances 0.000 claims abstract description 123
- 238000000034 method Methods 0.000 claims abstract description 41
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000005052 trichlorosilane Substances 0.000 claims abstract description 14
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000077 silane Inorganic materials 0.000 claims abstract description 13
- 238000002844 melting Methods 0.000 claims abstract description 12
- 230000008018 melting Effects 0.000 claims abstract description 12
- 238000005192 partition Methods 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000000155 melt Substances 0.000 claims description 16
- 239000002245 particle Substances 0.000 claims 1
- 230000009172 bursting Effects 0.000 abstract description 4
- 230000001681 protective effect Effects 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 13
- 239000001257 hydrogen Substances 0.000 description 12
- 230000005855 radiation Effects 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 8
- 239000008187 granular material Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 5
- 239000000460 chlorine Substances 0.000 description 5
- 229910052801 chlorine Inorganic materials 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910005921 H—Si—H Inorganic materials 0.000 description 1
- 101100353042 Mycobacterium bovis (strain BCG / Pasteur 1173P2) lnt gene Proteins 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000000516 activation analysis Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000008710 crystal-8 Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 101150028022 ppm1 gene Proteins 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明はＳｉ単結晶を製造する単結晶製造方法に関し、
更に詳述すれば顆粒状Ｓｉ原料を用いてＳｉ単結晶を製
造する単結晶製造方法に関するものである。[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a single crystal manufacturing method for manufacturing a Si single crystal,
More specifically, the present invention relates to a single crystal manufacturing method for manufacturing a Si single crystal using a granular Si raw material.
Ｓｉ単結晶を成長させる方法としては、石英製の坩堝内
にＳｉ原料を収納して融解させ、このＳｉ融液にＳｉの
種結晶を浸し、これを回転させつつ上方に引上げて種結
晶下端にＳｉ単結晶を成長せしめる、所謂チョクラルス
キー（ＣＺ）法が知られている。To grow a Si single crystal, a Si raw material is stored in a quartz crucible and melted, a Si seed crystal is immersed in this Si melt, and the Si seed crystal is pulled upward while rotating to reach the lower end of the seed crystal. The so-called Czochralski (CZ) method for growing Si single crystals is known.
最初に坩堝内に収納するＳｉ原料としては、多結晶を粉
砕して塊状とした原料がよく用いられ、融解に伴う容量
の減少を鑑みて、最初に坩堝内には山盛り状態にして塊
状原料を収納しておく。従って、融解するに伴って塊状
原料がブリッジ状態となり、このブリッジがくずれて融
液が飛散したり、石英が変形するという難点がある。As the Si raw material initially stored in the crucible, a raw material made into a lump by pulverizing a polycrystal is often used.In consideration of the decrease in capacity due to melting, the raw material is piled up in a heap in the crucible. Store it away. Therefore, as it melts, the bulk raw material becomes in a bridge state, and this bridge collapses, causing the melt to scatter and the quartz to deform.
このよう難点を解消するために、最初に坩堝内に収納す
るＳｉ原料（初期チャージ用Ｓｉ原料という）として、
顆粒状のＳｉ原料を使用することがある。In order to solve these difficulties, as the Si raw material (referred to as initial charging Si raw material) to be initially stored in the crucible,
A granular Si raw material may be used.
顆粒状のＳｉ原料を初期チャージ用Ｓｉ原料として使用
する場合には上述のような難点を解消し、しかも塊状原
料に比して充填率を大きくできるのでチップあたりのコ
ストの低減化を図ることができ、また塊状原料に比して
嵩が小さいので取扱いが容易となる。When using granular Si raw material as the Si raw material for initial charging, the above-mentioned difficulties can be overcome, and the filling rate can be increased compared to bulk raw material, so the cost per chip can be reduced. Moreover, it is easier to handle because it has a smaller bulk than bulk raw materials.
坩堝内に収納したＳｉ原料を融解させるとその容量が減
少するので、坩堝容量を十分に活かすように、追加のＳ
ｉ原料（チャージアップ用Ｓｉ原料という）を更に坩堝
内に収納してそれを融解させる。When the Si raw material stored in the crucible is melted, its capacity decreases, so in order to make full use of the crucible capacity, additional S is added.
The i raw material (referred to as the Si raw material for charge-up) is further placed in the crucible and melted.
そして、このチャージアップ用Ｓｉ原料の収納方法とし
ては、棒状Ｓｉ原料を収納して融解させる方法（実公昭
５０−１１７８８号公報）、または特殊な治具にて塊状
Ｓｉ原料を収納して融解させる方法（特開昭５０−１．
１７８８号公報）等が知られている。As a method for storing this Si raw material for charge-up, there is a method of storing and melting a rod-shaped Si raw material (Japanese Utility Model Publication No. 11788/1988), or a method of storing and melting a lumpy Si raw material using a special jig. Method (Unexamined Japanese Patent Publication No. 50-1.
1788) etc. are known.
ところが、棒状Ｓｉ原料を利用する場合にあっては、原
料を収納し過ぎると坩堝が破損したり、液漏れしたりす
る難点があり、また原料と融液とを離散した状態にて放
置するときには融液が沸騰するという難点がある。また
塊状Ｓｉ原料を利用する場合にあっては、原料を融液内
に収納する際に融液が飛散するので、融液表面を一旦固
化させた後原料を収納することとするが、この固化時に
坩堝が割れて液漏れが住じるという難点がある。However, when using a rod-shaped Si raw material, there are disadvantages such as damage to the crucible or liquid leakage if the raw material is stored too much, and when the raw material and melt are left in a discrete state. The problem is that the melt boils. In addition, when using a bulk Si raw material, the melt will scatter when the raw material is stored in the melt, so the raw material is stored after the surface of the melt is solidified. The problem is that sometimes the crucible cracks and liquid leaks.
このような難点を解消するために、チャージアップ用Ｓ
ｉ原料として顆粒状のＳｉ原料を使用することがある。In order to solve this problem, we have developed a charge-up S
A granular Si raw material may be used as the i raw material.
顆粒状のＳｉ原料をこのような目的に使用する場合には
、前述したような難点を解消することができる。When a granular Si raw material is used for such purposes, the above-mentioned difficulties can be overcome.
また、種結晶を引上げなからＳｉ単結晶を連続して成長
させていく際には、坩堝容量には限りがあるから単結晶
の成長容量に応じてＳｉ原料を坩堝内に供給する必要が
あるが、このＳｉ原料（追加チャージ用Ｓｉ原料）の供
給は成長条件を変化させないように行わなければならな
い。In addition, when growing Si single crystals continuously without pulling the seed crystal, the capacity of the crucible is limited, so it is necessary to supply Si raw material into the crucible according to the growth capacity of the single crystal. However, this Si raw material (Si raw material for additional charging) must be supplied without changing the growth conditions.
このため従来にあっては坩堝の内側に、融液の通流口を
開口した他の坩堝、または円筒体を配置して融液面を単
結晶を引上げる内側領域と、Ｓｉ原料を供給する外側領
域とに区分し、原料供給に伴う融液面の波動、粉塵、温
度変化等が結晶成長域である内側領域に及ぼす影響を可
逆的に低減することが行われている（特開昭５７−１８
３３９２号公報。For this reason, conventionally, inside the crucible, another crucible with an opening for the flow of the melt or a cylindrical body is arranged so that the melt surface is used as an inner region for pulling the single crystal and for supplying the Si raw material. The method is used to reversibly reduce the effects of waves, dust, temperature changes, etc. on the melt surface due to supply of raw materials on the inner region, which is the crystal growth region. -18
Publication No. 3392.
特開昭４７−１０３５５号公報）。そしてこの追加チャ
ージ用Ｓｉ原料としては、シリコン多結晶を粉砕した塊
粒状のＳｉ原料が広く使用されている。JP-A-47-10355). As the Si raw material for this additional charge, bulk Si raw material obtained by pulverizing polycrystalline silicon is widely used.
ところが上述した塊粒状のＳｉ原料は形状が不定形性で
あるので、原料供給部内においてブリッジ状態となって
詰まりが生じ易いという難点がある。However, since the above-mentioned lumpy and granular Si raw material has an amorphous shape, there is a problem in that it tends to form a bridging state and cause clogging in the raw material supply section.
そこで、この難点を解消すべく、顆粒状のＳｉ原料を追
加チャージ用Ｓｉ原料として使用することがある。Therefore, in order to solve this difficulty, granular Si raw material is sometimes used as the Si raw material for additional charging.
ところが、初期チャージ用、チャージアップ用として顆
粒状のＳｉ原料を使用する場合には、Ｓｉ原料が融解温
度直前まで加熱されたときに生じる破裂現象のために、
飛散物が坩堝表面に集積し、集積した飛散物が融液面に
脱落して結晶成長条件が乱れて欠陥結晶が生じるという
問題点がある。However, when using granular Si raw material for initial charging and charge-up, due to the rupture phenomenon that occurs when the Si raw material is heated to just before its melting temperature,
There is a problem in that flying debris accumulates on the crucible surface, and the accumulated flying debris falls onto the melt surface, disrupting crystal growth conditions and producing defective crystals.
また追加チャージ用として顆粒状のＳｉ原料を使用する
場合には、同様の破裂現象のために、飛散物が単結晶成
長域である内側領域、または結晶成長界面に飛び込み、
結晶成長条件を乱して結晶欠陥を誘発するという問題点
がある。Furthermore, when using granular Si raw material for additional charging, a similar rupture phenomenon causes scattered objects to fly into the inner region of the single crystal growth region or into the crystal growth interface.
There is a problem in that crystal growth conditions are disturbed and crystal defects are induced.
第５図（イ）、（ロ）、（ハ）は本発明者が実験、研究
の結果知見したシラン法（トリクロルシラン法の場合も
実質的に同じ）により得た顆粒状Ｓｉ原料の破裂現象の
説明図であり、第５図（イ）に示す如く、顆粒はその表
面のＳｉに周囲のガス中のＳｉが結合して順次成長して
ゆくが、この成長過程ではＳｉにＳｉ或いはＨも結合し
て顆粒内にＨが取り込まれ、また顆粒の表面にはＳ ｉ
−Ｈ又はＨ−Ｓｉ−Ｈ等の形態で未分解水素が吸着さ
れる。Figures 5 (a), (b), and (c) show the rupture phenomenon of granular Si raw materials obtained by the silane method (substantially the same in the case of the trichlorosilane method) as found by the present inventor as a result of experiments and research. As shown in FIG. 5(a), the granules grow as Si in the surrounding gas combines with the Si on the surface, but during this growth process, Si or H is also added to the Si. H is bound into the granules, and Si
Undecomposed hydrogen is adsorbed in the form of -H or H-Si-H.
ところでこのような顆粒の成長過程では顆粒同士も結合
するが、第５図（ロ）に示す如く結合した顆粒Ａ、Ｂ、
Ｃ相互の隙間内では粒界表面に吸着された未分解水素が
閉じ込められた状態となる。By the way, during the growth process of such granules, the granules also combine with each other, and as shown in Figure 5 (b), the combined granules A, B,
In the gaps between C, undecomposed hydrogen adsorbed on the grain boundary surfaces becomes trapped.
このような原料が加熱されると第５図（ハ）に示す如く
粒界表面、或いは内部に閉じ込められた未分解水素が分
離して水素ガスとなり、融解直前に達して顆粒相互の結
合力が低下したとき水素ガスの急速膨張によって破裂し
、顆粒細片が飛散物として坩堝の内側領域、或いは単結
晶成長界面に侵入することとなると考えられる。When such a raw material is heated, as shown in Figure 5 (c), undecomposed hydrogen trapped on the grain boundary surface or inside separates and becomes hydrogen gas, reaching the point of melting, and the bonding force between the grains is reduced. It is thought that when the temperature decreases, the hydrogen gas ruptures due to rapid expansion, and the granule fragments enter the inner region of the crucible or the single crystal growth interface as flying objects.
また本発明者は顆粒状Ｓｉ原料に生じる原料自身の融解
直前の破裂現象はシラン法によって得た顆粒状Ｓｉ原料
にあっては残留〔Ｈ〕量と、またトリクロルシラン法に
よって得た顆粒状Ｓｉ原料にあっては残留〔Ｃ１〕量と
夫々密接な関係にあり１．この残留〔Ｈ〕量、〔Ｃ１〕
量が所定値以下になると破裂が著しく低減されることを
知見した。The present inventor also found that the rupture phenomenon that occurs in granular Si raw materials immediately before melting of the raw material itself is due to the amount of residual [H] in the granular Si raw materials obtained by the silane method, and the amount of residual [H] in the granular Si raw materials obtained by the trichlorosilane method. Regarding raw materials, there is a close relationship with the amount of residual [C1].1. This residual [H] amount, [C1]
It has been found that bursting is significantly reduced when the amount is below a predetermined value.
本発明はかかる知見に基づきなされたものであって、残
留（ＨＥ量、残留（Ｃｊり量を所定値以下に低減した顆
粒状Ｓｉ原料を用いることにより、破裂現象が生じず、
しかも棒状または塊状のＳｉ原料を使用する際に発生す
る難点を解消することができる単結晶製造方法を提供す
ることを目的とする。The present invention has been made based on this knowledge, and by using a granular Si raw material in which the residual (HE amount) and residual (Cj amount) are reduced to below a predetermined value, the rupture phenomenon does not occur.
Moreover, it is an object of the present invention to provide a method for producing a single crystal that can overcome the difficulties that occur when using rod-shaped or lump-shaped Si raw materials.
本発明に係る単結晶製造方法は、シラン法により得た残
留〔Ｈ〕ｉｔが７．５ｗｔｐｐｍ以下、又はトリクロル
シラン法により得た残留（Ｃ／り ｆｆｉが１５ｗｔｐ
ｐａ＋以下とした顆粒状Ｓｉ原料を用いることを特徴と
する。In the single crystal manufacturing method according to the present invention, the residual [H] it obtained by the silane method is 7.5 wtppm or less, or the residual [H]it obtained by the trichlorosilane method is 15 wtppm or less.
It is characterized by using a granular Si raw material having a temperature of not more than pa+.
本発明方法の単結晶製造方法にあっては、上述したよう
な顆粒状Ｓｉ原料を用いてＳｉ単結晶を製造する。そう
すると融解直前における破裂現象が生じない。In the single crystal manufacturing method of the present invention, a Si single crystal is manufactured using the granular Si raw material as described above. This prevents the phenomenon of bursting immediately before melting.
シラン法による顆粒状Ｓｉ原料はペルジャー内に導入し
た粉状のＳｉ種の表面にシランガス５ｉｆ１４を温度６
００〜８００°Ｃで熱解離させて顆粒状に成長させて製
造される。The granular Si raw material produced by the silane method is prepared by applying 5if14 silane gas to the surface of the powdered Si species introduced into the Pelger at a temperature of 6.
It is produced by thermally dissociating it at 00 to 800°C and growing it into granules.
ところでこの製造された顆粒状Ｓｉ原料は微細単結晶粒
が集合した構造となっているが、この結晶粒界には通常
未分解水素〔Ｈ〕が ２０〜４０ｗｔｐｐｍ程度取り込
まれているからこの残留〔Ｈ〕量を７．５ｗｔｐｐｍ以
下に低減せしめる処理を施す。この残留〔Ｈ〕量の低減
法には、例えば顆粒状Ｓｉ原料を真空熱処理する方法、
或いは製造過程での反応を遅延させる方法、或いは製造
後原料を保温徐冷する方法等があり、必要に応じて選定
して適用すればよい。By the way, the produced granular Si raw material has a structure in which fine single crystal grains are aggregated, and since approximately 20 to 40 wtppm of undecomposed hydrogen [H] is normally incorporated into the grain boundaries, this residual [H] A process is performed to reduce the amount of H] to 7.5 wtppm or less. Methods for reducing the amount of residual [H] include, for example, a method of vacuum heat treating a granular Si raw material;
Alternatively, there are methods of delaying the reaction during the manufacturing process, or methods of keeping the raw material warm and slowly cooling after manufacturing, and these methods may be selected and applied as necessary.
適正な水素濃度、処理温度、処理時間を得るため本発明
者等が行った実験について以下に説明する。実験は直径
２１以下の顆粒状Ｓｉ原料を石英製の坩堝内に１０ｋｇ
収納し、抵抗加熱によって処理温度、処理時間を変えて
加熱処理し、得られた顆粒状Ｓｉ原料の水素濃度を求め
ると共に、水素濃度と熱処理時間との関係、処理温度と
処理時間との関係を求めた。なお雰囲気圧力は０．０５
〜０． ＩＴｏｒｒ及びＡｒガスにより１０〜２０Ｔｏ
ｒｒに調整した圧力の２水準で行い、終了後は室温迄冷
却した。なおこの間真空排気はそのまま継続した。Experiments conducted by the present inventors to obtain appropriate hydrogen concentration, treatment temperature, and treatment time will be described below. In the experiment, 10 kg of granular Si raw material with a diameter of 21 mm or less was placed in a quartz crucible.
The hydrogen concentration of the obtained granular Si raw material was determined by storing and heat-treating by resistance heating while changing the treatment temperature and treatment time, and the relationship between the hydrogen concentration and heat treatment time, and the relationship between treatment temperature and treatment time I asked for it. Note that the atmospheric pressure is 0.05
~0. 10-20To with ITorr and Ar gas
The test was carried out at two levels of pressure adjusted to rr, and after completion of the test, the test was cooled to room temperature. During this time, vacuum evacuation continued.
第１図は顆粒状Ｓｉ原料の熱処理時間と水素濃度とが飛
散に与える影響についての実験結果を示すグラフであり
、横軸に熱処理時間（時間）を、また縦軸に水素濃度（
ｗｔｐｐｍ ）をとって示しである。FIG. 1 is a graph showing the experimental results on the effects of heat treatment time and hydrogen concentration on scattering of granular Si raw materials. The horizontal axis shows the heat treatment time (hours), and the vertical axis shows the hydrogen concentration (
wtppm).
グラフ中白丸は飛散なし、黒丸は飛散ありの場合を示し
ている。このグラフから明らかなようにハツチングを付
して示す線で囲われた領域内に納まる水素濃度７．５ｈ
ｔｐｐｍ以下に設定すれば飛散のない顆粒状Ｓｉ原料と
することが可能であることが解る。なおグラフ中の温度
表示は処理温度を示している。White circles in the graph indicate no scattering, and black circles indicate cases with scattering. As is clear from this graph, the hydrogen concentration of 7.5 hours falls within the area enclosed by the hatched line.
It can be seen that if it is set to tppm or less, it is possible to obtain a granular Si raw material without scattering. Note that the temperature display in the graph indicates the processing temperature.
第２図は顆粒状Ｓｉ原料に対する熱処理温度と処理時間
とが飛散に与える影響についての実験結果を示すグラフ
であり、横軸に熱処理温度（’ｃ）、また縦軸に処理時
間（時間）をとって示しである。Figure 2 is a graph showing the experimental results on the effects of heat treatment temperature and treatment time on scattering on granular Si raw materials, with the heat treatment temperature ('c) on the horizontal axis and the treatment time (hours) on the vertical axis. This is a great indication.
グラフ中白丸は飛散なし、黒丸は飛散ありの場合を示し
ている。White circles in the graph indicate no scattering, and black circles indicate cases with scattering.
このグラフから明らかな如くハツチングを付して示す限
界曲線で囲われた領域内に納まる範囲で処理を行えば、
飛散のない顆粒状Ｓｉ原料とすることができることが解
る。As is clear from this graph, if processing is performed within the area enclosed by the hatched limit curve,
It can be seen that a granular Si raw material without scattering can be obtained.
トリクロルシラン法による顆粒状Ｓｉ原料の製造は、ペ
ルジャー内に導入した粉状のＳｉ種の表面にトリクロル
シランガスと水素の混合ガスを導入し、温度１０００〜
１２００℃で還元により顆粒状に成長させるものである
。In the production of granular Si raw material by the trichlorosilane method, a mixed gas of trichlorosilane gas and hydrogen is introduced onto the surface of powdered Si seeds introduced into a Pelger, and the temperature is 1000~1000.
It is grown into granules by reduction at 1200°C.
このトリクロルシラン法により製造された顆粒状Ｓｉ原
料にも通常未分解塩素（ＣＸ）が５０〜２００ｗｔｐｐ
ｍ程度取り込まれており、前記したシラン法により得た
顆粒状Ｓｉ原料の場合と同様の方法により残留（Ｃｊ２
）量を１５ｗｔｐｐｍ以下に低減せしめて用いる。The granular Si raw material produced by this trichlorosilane method also usually contains 50 to 200 wtpp of undecomposed chlorine (CX).
Cj2 is taken in, and remaining (Cj2
) is used by reducing the amount to 15wtppm or less.
第３図はトリクロルシラン法により製造した顆粒状Ｓｉ
原料における残留（Ｃｊ２）量と飛散との関係を示すグ
ラフである。グラフは横軸に残留塩素濃度（ｗｔｐｐｍ
：放射化分析法に依る）を、また縦軸に飛散の有無
をとって示しである。グラフ中白丸は飛散なし、また黒
丸は飛散有りの場合を示している。Figure 3 shows granular Si produced by the trichlorosilane method.
It is a graph showing the relationship between the amount of residual (Cj2) in the raw material and scattering. The graph shows the residual chlorine concentration (wtppm) on the horizontal axis.
: Depends on the activation analysis method) and the presence or absence of scattering is plotted on the vertical axis. White circles in the graph indicate no scattering, and black circles indicate cases with scattering.
このグラフから明らかなように残留塩素濃度は１５ｗｔ
ｐｐｍ以下で飛散が無くなることが解る。As is clear from this graph, the residual chlorine concentration is 15wt.
It can be seen that scattering disappears below ppm.
次に前述した如き顆粒状Ｓｉ原料を用いて単結晶成長を
行う場合の具体的装置の例を示す。Next, an example of a specific apparatus for growing a single crystal using the granular Si raw material as described above will be shown.
第４図は本発明に係る単結晶製造方法を用いる単結晶製
造装置の模式的断面図であり、図中１はチャンバ、２は
保温壁、３は坩堝、４はヒータを示している。チャンバ
１内にはその側周に保温壁２が内張すされ、この保温壁
２で囲われた中央部に坩堝３が配設され、この坩堝３と
保温壁２との間にヒータ４がこれらとの間に排気用の通
気路を構成する間隙を隔てて配設されている。FIG. 4 is a schematic cross-sectional view of a single crystal manufacturing apparatus using the single crystal manufacturing method according to the present invention, in which 1 indicates a chamber, 2 a heat retaining wall, 3 a crucible, and 4 a heater. A heat insulating wall 2 is lined around the side of the chamber 1, a crucible 3 is disposed in the center surrounded by the heat insulating wall 2, and a heater 4 is placed between the crucible 3 and the heat insulating wall 2. A gap forming an exhaust air passage is provided between them.
坩堝３はグラファイト製の容器の内側に石英製の容器を
嵌め合わせた二重構造に構成されており、底部中央には
チャンバｌの底壁を貫通させた軸３ａの上端が連結され
、該軸３ａにて回転させつつ昇降せしめられるようにな
っている。The crucible 3 has a double structure in which a quartz container is fitted inside a graphite container, and the upper end of a shaft 3a passing through the bottom wall of the chamber 1 is connected to the center of the bottom. It can be raised and lowered while rotating at 3a.
チャンバ１の上部壁中央にはチャンバ１内の雰囲気ガス
の供給口を兼ねる単結晶の引上口１ａが開口され、また
その周囲の１個所には、原料供給口１ｂが開口せしめら
れており、前記引上口１ａには保護筒５が立設され、ま
た原料供給口１ｂを通じて原料供給装置６の原料供給管
６ａがチャンバ１内に差し込まれている。A single-crystal pulling port 1a that also serves as a supply port for atmospheric gas in the chamber 1 is opened at the center of the upper wall of the chamber 1, and a raw material supply port 1b is opened at one location around the single-crystal pulling port 1a. A protection tube 5 is provided upright at the pulling port 1a, and a raw material supply pipe 6a of a raw material supply device 6 is inserted into the chamber 1 through the raw material supply port 1b.
保護筒５の上端からは引上軸５ａを用いて種結晶５ｃを
掴持するチャック５ｂが吊り下げられ、また引上軸５ａ
の上端は図示しない回転、昇降機構に連繋されており、
種結晶５ｃを坩堝３内の融液になじませた後、回転させ
つつ上昇させることによって、種結晶５ｃ下端にシリコ
ン単結晶７を成長せしめるようになっている。A chuck 5b that grips the seed crystal 5c using a pulling shaft 5a is suspended from the upper end of the protective tube 5.
The upper end of the is connected to a rotating and lifting mechanism (not shown).
After the seed crystal 5c is adapted to the melt in the crucible 3, it is rotated and raised to grow a silicon single crystal 7 at the lower end of the seed crystal 5c.
チャンバ１内の上方には前記単結晶７の引上げ域の周囲
に位置させて輻射スクリーン８が配設され、またこの輻
射スクリーン８には筒状隔壁９、原料導入治具１０が取
り付けられている。A radiation screen 8 is disposed above the chamber 1 around the pulling area of the single crystal 7, and a cylindrical partition wall 9 and a raw material introduction jig 10 are attached to the radiation screen 8. .
輻射スクリーン８は金属製あるいはカーボン製の環状リ
ム８ａの外周縁部に輻射スクリーン８を保温壁２の上面
に支持する円筒形の支持部８ｂを、また内周縁部にはこ
こから下方に向かうに従って縮径され、中空の逆円錐台
形をなすよう傾斜させたテーパ部８ｃを夫々設けて構成
されている。The radiation screen 8 has a cylindrical support part 8b that supports the radiation screen 8 on the upper surface of the heat retaining wall 2 at the outer peripheral edge of an annular rim 8a made of metal or carbon, and a cylindrical support part 8b that supports the radiation screen 8 on the upper surface of the heat insulation wall 2, and a cylindrical support part 8b that supports the radiation screen 8 on the upper surface of the heat insulation wall 2, and a cylindrical support part 8b that supports the radiation screen 8 on the inner peripheral edge as it goes downward from here. The tapered portions 8c each have a reduced diameter and are inclined to form a hollow inverted truncated cone shape.
筒状隔壁９は石英製であって、円筒形の隔壁本体部９ａ
の上端部に周方向の複数個所から立設した図示しない支
持片を輻射スクリーン８のテーパ部８ｃに取り付けられ
、その下端が坩堝３の内底から所要高さの位置であって
、且つ融液中の適正な深さ位置まで漬かり、坩堝３内を
同心状に内側領域とその外側の環状領域とに区分するよ
うになっている。The cylindrical partition wall 9 is made of quartz, and has a cylindrical partition main body 9a.
Support pieces (not shown), which are erected from multiple positions in the circumferential direction at the upper end, are attached to the tapered part 8c of the radiation screen 8, and the lower end thereof is located at a required height from the inner bottom of the crucible 3, and the melt is The crucible 3 is immersed in the crucible 3 to an appropriate depth, and the inside of the crucible 3 is concentrically divided into an inner region and an annular region outside the crucible 3.
一方原料導入治具１０はロート部１０ａ及びこれに連な
る管部を備えており、輻射スクリーン８の環状リム８ａ
に穿った孔に管部を通して取り付けられ、ロート部１０
ａは原料供給口１ｂから差し込まれた原料供給管６ａの
下端に臨み、また管部の下端は坩堝３内であって、筒状
隔壁９で仕切られる外側、即ち外側の環状領域に臨ませ
である。On the other hand, the raw material introduction jig 10 includes a funnel part 10a and a pipe part connected to the funnel part 10a, and an annular rim 8a of the radiation screen 8.
The funnel part 10 is attached by passing the tube part through a hole drilled in the
a faces the lower end of the raw material supply pipe 6a inserted from the raw material supply port 1b, and the lower end of the pipe portion faces the outside, that is, the outer annular area partitioned by the cylindrical partition 9, inside the crucible 3. be.
原料供給管６ａの上端はチャンバ１の外に配した原料供
給装置６におけるケーシング６ｂ内に配した秤量計付の
電磁フィーダ６Ｃの排出端下に臨ませである。電磁フィ
ーダ６Ｃの受給端にはサブホッパ６ｄが配設され、該サ
ブホッパ６ｄ上にはケーシング６ｂに固定したメインホ
ッパ６ｅを臨ませである。The upper end of the raw material supply pipe 6a faces below the discharge end of an electromagnetic feeder 6C equipped with a weighing scale, which is disposed inside the casing 6b of the raw material supply device 6 disposed outside the chamber 1. A sub-hopper 6d is provided at the receiving end of the electromagnetic feeder 6C, and a main hopper 6e fixed to the casing 6b faces above the sub-hopper 6d.
次にこのような構成の装置を用いるＳｉ単結晶の製造方
法の具体的手順について説明する。Next, a detailed procedure of a method for manufacturing a Si single crystal using an apparatus having such a configuration will be described.
まず、本発明に係る顆粒状Ｓｉ原料を初期チャージ用Ｓ
ｉ原料として坩堝３内に収納した後、ヒータ４にて坩堝
３を加熱し、坩堝３に収納した顆粒状Ｓｉ原料を加熱溶
融する。なおこの際融解の進行に伴って容量が減少する
ので、本発明に係る顆粒状Ｓｉ原料を、チャージアップ
用Ｓｉ原料として適量だけ坩堝３内に追加収納して融解
させる。First, the granular Si raw material according to the present invention is used as S for initial charging.
After being stored in a crucible 3 as an i raw material, the crucible 3 is heated by a heater 4 to heat and melt the granular Si raw material stored in the crucible 3. At this time, since the capacity decreases as the melting progresses, an appropriate amount of the granular Si raw material according to the present invention is additionally stored in the crucible 3 as a charge-up Si raw material and melted.
坩堝３をこれを支持する軸３ａにて矢符方向に回転させ
、また引上げ手段を構成する引上軸５ａを下降して種結
晶５ｃを筒状隔壁９にて囲われた内側の融液中に浸漬し
た後、引上軸５ａを回転させつつ所定の速度で引上げ（
平均１．５ｍｍ／分）、種結晶５ｃ下に単結晶７を成長
せしめる。The crucible 3 is rotated in the direction of the arrow by the shaft 3a that supports it, and the pulling shaft 5a constituting the pulling means is lowered to drop the seed crystal 5c into the melt inside the cylindrical partition wall 9. After being immersed in water, it is pulled up at a predetermined speed while rotating the pulling shaft 5a (
The single crystal 7 is grown under the seed crystal 5c at an average rate of 1.5 mm/min).
本発明に係る顆粒状Ｓｉ原料を追加チャージ用Ｓｉ原料
として、予めメインホッパ６ｅに貯留しておき、ここか
らサブホッパ６ｄを経て電磁フィーダ６ｃにより計量さ
れつつ原料供給管６ａ、原料導入治具１０を経て坩堝３
における筒状隔壁９の外側の環状領域に供給されること
とする。The granular Si raw material according to the present invention is stored in the main hopper 6e in advance as the Si raw material for additional charging, and from there the raw material supply pipe 6a and the raw material introduction jig 10 are metered by the electromagnetic feeder 6c via the sub-hopper 6d. After that, Crucible 3
It is assumed that the water is supplied to the outer annular region of the cylindrical partition wall 9 in .
なお最初に収納された顆粒状Ｓｉ原料の融解開始から、
単結晶の引上げ終了に到るまで保護筒５の上端に接続し
た供給管からＡｒ等の雰囲気ガスが保護筒５を通じて坩
堝３上にその上方から導入される。Note that from the start of melting of the initially stored granular Si raw material,
Atmospheric gas such as Ar is introduced from above onto the crucible 3 through the protection tube 5 from a supply pipe connected to the upper end of the protection tube 5 until the pulling of the single crystal is completed.
保護筒５の上方から坩堝３上に下降した雰囲気ガスは輻
射スクリーン８のテーバ部８Ｃに沿って坩堝３内の融液
表面に達し、ここから輻射スクリーン８の下面側を経て
筒状隔壁９間を経、次いで筒状隔壁９の外側の環状領域
を経、坩堝３とヒータ４、保温壁２との間に形成された
通気路を経てチャンバ１の下部側壁に開口した排気口Ｉ
Ｃから図示しない排気ポンプにより吸引排出される。The atmospheric gas that descends onto the crucible 3 from above the protective tube 5 reaches the surface of the melt in the crucible 3 along the tapered portion 8C of the radiation screen 8, and from there passes through the lower surface side of the radiation screen 8 between the cylindrical partition walls 9. , then through the annular region outside the cylindrical partition wall 9 , through the ventilation path formed between the crucible 3 , the heater 4 , and the heat retaining wall 2 , and then through the exhaust port I opened in the lower side wall of the chamber 1
It is suctioned and discharged from C by an exhaust pump (not shown).
なお本実施例では、本発明に係る顆粒状Ｓｉ原料を、初
期チャージ用Ｓｉ原料、チャージアップ用Ｓｉ原料及び
追加チャージ用Ｓｉ原料として、何れの場合においても
使用することとしたが、この３１の用途のうちの任意の
１種または任意の２種の用途において、本発明に係る顆
粒状Ｓｉ原料を使用してもよいことは勿論である。In this example, the granular Si raw material according to the present invention was used as the Si raw material for initial charging, the Si raw material for charge-up, and the Si raw material for additional charging. Of course, the granular Si raw material according to the present invention may be used in any one or two of the applications.
以上詳述した如く本発明の単結晶製造方法では、Ｓｉ原
料としてシラン法により製造した残留〔Ｈ〕量が７．５
ｗｔｐｐｍ以下、またはトリクロルシラン法により製
造した残留（ＣＸ）量が１５ｗｔｐｐｍ以下の顆粒状Ｓ
ｉ原料を用いてＳｉ単結晶を製造することとするので、
破裂現象を防止することができ、しかも顆粒状Ｓｉ原料
を使用する際における利点を活かすことができる。As detailed above, in the single crystal production method of the present invention, the amount of residual [H] produced by the silane method as a Si raw material is 7.5
Granular S with a residual (CX) amount of 15 wtppm or less, or produced by the trichlorosilane method
Since we will manufacture Si single crystal using i raw material,
It is possible to prevent the phenomenon of bursting, and also to take advantage of the advantages of using a granular Si raw material.
第１図は本発明に係る単結晶製造方法において用いる顆
粒状Ｓｉ原料の残留ＣＨ）量の低減のための熱処理時間
と水素濃度とが破裂に伴う飛散に与る影響を示すグラフ
、第２図は同じく熱処理温度と処理時間とが破裂に伴う
飛散に与える影響を示すグラフ、第３図は同じく残留塩
素濃度〔Ｃ１〕が破裂に伴う飛散に与える影響を示すグ
ラフ、第４図は本発明の単結晶製造方法実施するための
装置の縦断面図、第５図はシラン法によって製造した顆
粒状Ｓｉ原料の破裂現象の説明図である。
１・・・チャンバ、３・・・坩堝 ４・・・ヒータ ５
・・・保護筒 ６・・・原料供給装置 ６ｃ・・・電磁
フィーダ６ｄ・・・サブホッパ ６ｅ・・・メインホッ
パ ７・・・単結晶８・・・輻射スクリーン １０・・
・原料導入治具１０ａ・・・ロート部
特 許 出願人 大阪チタニウム製造株式会社外１名
代理人 弁理士 河 野 登 夫藁 ４ 図
熱処理時日（時間）
第１図
処１！温度（℃）
第２図
０ １０ ２０ ３０ ４０ ５［１６０塩素
濃度（ｗｔ ｐｐｍ１
第 ３ 図
第５図FIG. 1 is a graph showing the influence of heat treatment time and hydrogen concentration on scattering due to rupture for reducing the amount of residual CH in the granular Si raw material used in the single crystal production method according to the present invention, and FIG. 3 is a graph showing the influence of heat treatment temperature and treatment time on scattering due to rupture, FIG. 3 is a graph showing the effect of residual chlorine concentration [C1] on scattering due to rupture, and FIG. FIG. 5 is a longitudinal cross-sectional view of an apparatus for implementing the single crystal manufacturing method, and is an explanatory diagram of the rupture phenomenon of the granular Si raw material manufactured by the silane method. 1... Chamber, 3... Crucible 4... Heater 5
...Protection tube 6...Raw material supply device 6c...Electromagnetic feeder 6d...Sub hopper 6e...Main hopper 7...Single crystal 8...Radiation screen 10...
・Raw material introduction jig 10a...Funnel part patent Applicant: Osaka Titanium Manufacturing Co., Ltd. and one other agent Patent attorney Noboru Kono 4 Figure Heat treatment date (hours) Figure 1 Location 1! Temperature (°C) Fig. 2 0 10 20 30 40 5 [160 Chlorine concentration (wt ppm1) Fig. 3 Fig. 5
Claims (1)
において、 前記顆粒状Ｓｉ原料として、シラン法により得た残留〔
Ｈ〕量が７．５ｗｔｐｐｍ以下、又はトリクロルシラン
法により得た残留〔Ｃ１〕量が１５ｗｔｐｐｍ以下とし
た顆粒状Ｓｉ原料を用いることを特徴とする単結晶製造
方法。 ２、坩堝内に顆粒状Ｓｉ原料を収納して該顆粒状Ｓｉ原
料を融解した後、前記坩堝内の融液にＳｉ種結晶を浸し
てＳｉ単結晶を成長させつつ引きあげる単結晶製造方法
において、前記顆粒状Ｓｉ原料として、シラン法により
得た残留〔Ｈ〕量が７．５ｗｔｐｐｍ以下、又はトリク
ロルシラン法により得た残留〔Ｃ１〕量が１５ｗｔｐｐ
ｍ以下とした顆粒状Ｓｉ原料を用いることを特徴とする
単結晶製造方法。 ３、坩堝内にＳｉ原料を収納して該Ｓｉ原料を融解した
後、更に前記坩堝内に顆粒状Ｓｉ原料を追加収納して該
顆粒状Ｓｉ原料を融解し、その後坩堝内の融液にＳｉ種
結晶を浸してＳｉ単結晶を成長させつつ引きあげる単結
晶製造方法において、 前記顆粒状Ｓｉ原料として、シラン法により得た残留〔
Ｈ〕量が７．５ｗｔｐｐｍ以下、又はトリクロルシラン
法により得た残留〔Ｃ１〕量が１５ｗｔｐｐｍ以下とし
た顆粒状Ｓｉ原料を用いることを特徴とする単結晶製造
方法。 ４、坩堝内にその単結晶原料融液の液面を液面下で連通
した状態で内、外の領域に区分する隔壁を配置し、外側
領域に顆粒状Ｓｉ原料を供給し、内側領域からＳｉ単結
晶を成長させつつ引き上げる単結晶製造方法において、 前記顆粒状Ｓｉ原料として、シラン法により得た残留〔
Ｈ〕量が７．５ｗｔｐｐｍ以下、又はトリクロルシラン
法により得た残留〔Ｃ１〕量が１５ｗｔｐｐｍ以下とし
た顆粒状Ｓｉ原料を用いることを特徴とする単結晶製造
方法。[Claims] 1. A method for producing a Si single crystal using a granular Si raw material, wherein the granular Si raw material is a residue obtained by a silane method [
A single crystal production method characterized by using a granular Si raw material having an amount of H] of 7.5 wtppm or less, or a residual [C1] amount of 15 wtppm or less obtained by a trichlorosilane method. 2. In a single crystal manufacturing method in which a granular Si raw material is stored in a crucible and the granular Si raw material is melted, a Si seed crystal is immersed in the melt in the crucible and pulled out while growing a Si single crystal. , as the granular Si raw material, the amount of residual [H] obtained by the silane method is 7.5 wtppm or less, or the amount of residual [C1] obtained by the trichlorosilane method is 15 wtpp
A method for producing a single crystal, characterized in that a granular Si raw material having a particle size of less than m is used. 3. After storing a Si raw material in a crucible and melting the Si raw material, further storing a granular Si raw material in the crucible and melting the granular Si raw material, and then adding Si to the melt in the crucible. In a method for producing a single crystal in which a seed crystal is immersed and pulled up while growing a Si single crystal, the residue obtained by the silane method is used as the granular Si raw material.
A single crystal production method characterized by using a granular Si raw material having an amount of H] of 7.5 wtppm or less, or a residual [C1] amount of 15 wtppm or less obtained by a trichlorosilane method. 4. A partition wall is placed in the crucible to separate the inner and outer regions with the liquid surface of the single-crystal raw material melt communicating below the liquid surface, and the granular Si raw material is supplied to the outer region, and the granular Si raw material is supplied from the inner region. In a single crystal production method in which a Si single crystal is pulled while growing, the granular Si raw material is a residue obtained by a silane method [
A single crystal production method characterized by using a granular Si raw material having an amount of H] of 7.5 wtppm or less, or a residual [C1] amount of 15 wtppm or less obtained by a trichlorosilane method.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP13514788A JPH01282194A (en) | 1988-01-19 | 1988-05-31 | Production of single crystal |
| US07/357,717 US5037503A (en) | 1988-05-31 | 1989-05-26 | Method for growing silicon single crystal |
| US07/953,630 USRE35242E (en) | 1988-05-31 | 1992-09-30 | Method for growing silicon single crystal |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1040788 | 1988-01-19 | ||
| JP63-10407 | 1988-01-19 | ||
| JP13514788A JPH01282194A (en) | 1988-01-19 | 1988-05-31 | Production of single crystal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01282194A true JPH01282194A (en) | 1989-11-14 |
| JPH0477712B2 JPH0477712B2 (en) | 1992-12-09 |
Family
ID=26345665
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13514788A Granted JPH01282194A (en) | 1988-01-19 | 1988-05-31 | Production of single crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01282194A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1991013192A1 (en) * | 1990-03-02 | 1991-09-05 | Nkk Corporation | Single crystal production apparatus |
| JPH059097A (en) * | 1991-06-28 | 1993-01-19 | Shin Etsu Handotai Co Ltd | Method for pulling up silicon single crystal |
| JPH05148073A (en) * | 1991-11-29 | 1993-06-15 | Nkk Corp | Production of silicon single crystal |
| JPH05208889A (en) * | 1992-01-30 | 1993-08-20 | Shin Etsu Handotai Co Ltd | Production of silicon single crystal |
| JP2008266017A (en) * | 2007-03-29 | 2008-11-06 | Sharp Corp | Solid material supply device, solid material processing device and solid material supply method |
| WO2023007830A1 (en) * | 2021-07-30 | 2023-02-02 | グローバルウェーハズ・ジャパン株式会社 | Method for producing silicon single crystal, and single crystal pulling apparatus |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS50155423A (en) * | 1974-05-13 | 1975-12-15 | ||
| JPS57183392A (en) * | 1981-05-01 | 1982-11-11 | Tohoku Metal Ind Ltd | Apparatus for preparation of single crystal |
| JPS5945917A (en) * | 1982-09-02 | 1984-03-15 | Denki Kagaku Kogyo Kk | Continuous preparation of polycrystalline silicon |
| JPS6117537A (en) * | 1984-04-27 | 1986-01-25 | インペリアル・ケミカル・インダストリ−ズ・ピ−エルシ− | Phenol derivative, manufacture and antiestrogenic medicine |
| JPS61242984A (en) * | 1985-04-19 | 1986-10-29 | Shinetsu Sekiei Kk | Crucible for pulling up silicon single crystal |
-
1988
- 1988-05-31 JP JP13514788A patent/JPH01282194A/en active Granted
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS50155423A (en) * | 1974-05-13 | 1975-12-15 | ||
| JPS57183392A (en) * | 1981-05-01 | 1982-11-11 | Tohoku Metal Ind Ltd | Apparatus for preparation of single crystal |
| JPS5945917A (en) * | 1982-09-02 | 1984-03-15 | Denki Kagaku Kogyo Kk | Continuous preparation of polycrystalline silicon |
| JPS6117537A (en) * | 1984-04-27 | 1986-01-25 | インペリアル・ケミカル・インダストリ−ズ・ピ−エルシ− | Phenol derivative, manufacture and antiestrogenic medicine |
| JPS61242984A (en) * | 1985-04-19 | 1986-10-29 | Shinetsu Sekiei Kk | Crucible for pulling up silicon single crystal |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1991013192A1 (en) * | 1990-03-02 | 1991-09-05 | Nkk Corporation | Single crystal production apparatus |
| JPH059097A (en) * | 1991-06-28 | 1993-01-19 | Shin Etsu Handotai Co Ltd | Method for pulling up silicon single crystal |
| JPH05148073A (en) * | 1991-11-29 | 1993-06-15 | Nkk Corp | Production of silicon single crystal |
| JPH0822795B2 (en) * | 1991-11-29 | 1996-03-06 | 東芝セラミックス株式会社 | Method for producing silicon single crystal |
| JPH05208889A (en) * | 1992-01-30 | 1993-08-20 | Shin Etsu Handotai Co Ltd | Production of silicon single crystal |
| JP2008266017A (en) * | 2007-03-29 | 2008-11-06 | Sharp Corp | Solid material supply device, solid material processing device and solid material supply method |
| WO2023007830A1 (en) * | 2021-07-30 | 2023-02-02 | グローバルウェーハズ・ジャパン株式会社 | Method for producing silicon single crystal, and single crystal pulling apparatus |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0477712B2 (en) | 1992-12-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US5242531A (en) | Continuous liquid silicon recharging process in czochralski crucible pulling | |
| JP4225688B2 (en) | Method for producing a silicon melt from a polysilicon charge | |
| USRE35242E (en) | Method for growing silicon single crystal | |
| JP4103593B2 (en) | Recharge tube for solid polycrystalline raw material and method for producing single crystal using the same | |
| JP5777336B2 (en) | Recharging method of polycrystalline silicon raw material | |
| US9359691B2 (en) | Method of loading a charge of polysilicon into a crucible | |
| JPH09328391A (en) | Production of molten silicon melt from polycrystalline silicon charging material | |
| US5306473A (en) | Quartz glass crucible for pulling a single crystal | |
| JPH01282194A (en) | Production of single crystal | |
| US5306388A (en) | Quartz glass crucible for pulling a semiconductor single crystal | |
| JP4804348B2 (en) | Cooled lump of molten silicon and method for producing the same | |
| JP6708173B2 (en) | Recharge tube and method for manufacturing single crystal | |
| JPH06100394A (en) | Method for feeding raw material for producing single crystal and apparatus therefor | |
| JP2531415B2 (en) | Crystal growth method | |
| JP3085567B2 (en) | Polycrystalline recharge apparatus and recharge method | |
| JPH0550478B2 (en) | ||
| JPH0523580Y2 (en) | ||
| JPH0280392A (en) | Single crystal production device | |
| JP2010173880A (en) | Method for producing semiconductor single crystal, and raw material supply container | |
| US20230142420A1 (en) | Determination of mass/time ratios for buffer members used during growth of single crystal silicon ingots | |
| TW202248470A (en) | Use of quartz plates during growth of single crystal silicon ingots | |
| JPH05148073A (en) | Production of silicon single crystal | |
| JPH0558769A (en) | Production of silicon single crystal | |
| JPH02233582A (en) | Pulling device of single crystal | |
| JPH04357190A (en) | Single crystal production apparatus |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| S533 | Written request for registration of change of name |
Free format text: JAPANESE INTERMEDIATE CODE: R313533 |
|
| R350 | Written notification of registration of transfer |
Free format text: JAPANESE INTERMEDIATE CODE: R350 |
|
| LAPS | Cancellation because of no payment of annual fees |