JPH07118089A - Recharging device and recharging method for polycrystal - Google Patents
Recharging device and recharging method for polycrystalInfo
- Publication number
- JPH07118089A JPH07118089A JP28762293A JP28762293A JPH07118089A JP H07118089 A JPH07118089 A JP H07118089A JP 28762293 A JP28762293 A JP 28762293A JP 28762293 A JP28762293 A JP 28762293A JP H07118089 A JPH07118089 A JP H07118089A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- supply pipe
- gas
- polycrystal
- melt
- 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
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002994 raw material Substances 0.000 claims abstract description 66
- 239000000155 melt Substances 0.000 claims abstract description 51
- 239000007789 gas Substances 0.000 claims abstract description 46
- 239000013078 crystal Substances 0.000 claims abstract description 42
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000011261 inert gas Substances 0.000 claims abstract description 15
- 238000007667 floating Methods 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 239000004065 semiconductor Substances 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052710 silicon Inorganic materials 0.000 abstract description 11
- 239000010703 silicon Substances 0.000 abstract description 11
- 239000001257 hydrogen Substances 0.000 abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 5
- 238000004090 dissolution Methods 0.000 abstract description 4
- 238000001816 cooling Methods 0.000 abstract description 2
- 229910052681 coesite Inorganic materials 0.000 abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract 2
- 239000000377 silicon dioxide Substances 0.000 abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 2
- 229910052682 stishovite Inorganic materials 0.000 abstract 2
- 229910052905 tridymite Inorganic materials 0.000 abstract 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000002844 melting Methods 0.000 description 10
- 230000008018 melting Effects 0.000 description 10
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 230000008030 elimination Effects 0.000 description 3
- 238000003379 elimination reaction Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 238000007664 blowing Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000002109 crystal growth method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- -1 hydrogen compound Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Landscapes
- Crystals, And After-Treatments Of Crystals (AREA)
- Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
- Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、多結晶のリチャージ装
置およびリチャージ方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a polycrystalline recharging device and method.
【０００２】[0002]
【従来の技術】半導体素子の基板には主として高純度シ
リコンが用いられているが、この高純度シリコンの製造
方法の一つとして、るつぼ内の原料融液から円柱状の単
結晶を引き上げるチョクラルスキー法（以下ＣＺ法とい
う）が用いられている。ＣＺ法においては、るつぼ内に
原料多結晶を充填し、前記るつぼの外周を取り巻くヒー
タによって原料を加熱溶解した上、シードチャックに取
り付けた種子結晶を融液に浸漬し、シードチャックおよ
びるつぼを同方向または逆方向に回転しつつシードチャ
ックを引き上げて、単結晶を成長させる。2. Description of the Related Art High-purity silicon is mainly used as a substrate for semiconductor devices. One of the methods for producing this high-purity silicon is to use a Czochral for pulling a cylindrical single crystal from a raw material melt in a crucible. The ski method (hereinafter referred to as the CZ method) is used. In the CZ method, a raw material polycrystal is filled in a crucible, the raw material is heated and melted by a heater surrounding the outer periphery of the crucible, and then the seed crystal attached to the seed chuck is immersed in a melt to make the seed chuck and the crucible the same. The seed chuck is pulled up while rotating in the opposite direction or in the opposite direction to grow a single crystal.
【０００３】近年は、半導体ウェーハの直径が大型化
し、６インチを超える大径ウェーハが要求されるように
なり、単結晶の直径も６インチ以上のものが主流になり
つつある。このため単結晶製造装置も大型化し、１サイ
クル当たりの処理量も増大する傾向にある。しかし、単
結晶製造装置の大型化に伴って単結晶成長工程における
所要時間が長くなるとともに、その前後工程、たとえば
原料多結晶の溶解所要時間や、成長した単結晶を炉外に
取り出した後、るつぼ、ヒータ等が清掃可能な温度に下
がるまでの冷却所要時間等も従来に比べて長くなってい
る。これらは単結晶の生産性を低下させる要因となって
いる。In recent years, the diameter of semiconductor wafers has increased, and large-diameter wafers exceeding 6 inches have been demanded. Single crystal diameters of 6 inches or more are becoming the mainstream. For this reason, the single-crystal manufacturing apparatus also tends to be large-sized, and the throughput per cycle tends to increase. However, as the size of the single crystal manufacturing apparatus becomes larger, the time required for the single crystal growth step becomes longer, and the steps before and after that, for example, the time required for melting the raw material polycrystal and after taking out the grown single crystal out of the furnace, The time required for cooling until the temperature at which the crucible, heater, etc., can be cleaned becomes longer than before. These are factors that reduce the productivity of single crystals.
【０００４】単結晶の生産性低下を解決する手段の一つ
として、リチャージ法が知られている。これは、融液か
ら単結晶を引き上げた後、原料多結晶を再度チャージし
て溶解し、再度単結晶を成長させる工程を数回繰り返す
方法で、炉内部品の冷却時間やチャンバ清掃時間等を数
バッチ分省略することができる。また、通常は単結晶１
本分の引き上げごとに１個必要とする石英るつぼも、数
本の単結晶に対して１個の割合となり、製造コストが低
減する。The recharge method is known as one of means for solving the decrease in the productivity of single crystals. This is a method of pulling a single crystal out of the melt, recharging and melting the raw material polycrystal, and then growing the single crystal again several times. It can be omitted for several batches. Also, usually single crystal 1
The number of quartz crucibles required for each pulling of one is one for several single crystals, and the manufacturing cost is reduced.
【０００５】[0005]
【発明が解決しようとする課題】リチャージのため粒状
の原料多結晶を融液に供給すると、前記粒状多結晶は融
液面に浮遊する状態となる。融液内に発生したＳｉＯガ
スは前記粒状多結晶によって冷却され、ＳｉＯアモルフ
ァスが形成される。そして、粒状多結晶の溶解の進行に
つれて前記ＳｉＯアモルファスが徐々に融液内に取り込
まれ、溶解せずに残存する。また、前記ＳｉＯアモルフ
ァスの一部はＳｉＯ2 となり、白色透明の浮遊物として
融液表面に残存する。前記ＳｉＯアモルファスやＳｉＯ
2 のパーティクルは、単結晶引き上げの際に単結晶崩れ
を引き起こす原因となる。When granular raw material polycrystals are supplied to the melt for recharging, the granular polycrystals float on the surface of the melt. The SiO gas generated in the melt is cooled by the granular polycrystal to form SiO amorphous. Then, as the dissolution of the granular polycrystal progresses, the SiO amorphous is gradually taken into the melt and remains without being dissolved. Further, a part of the SiO amorphous becomes SiO 2 and remains on the surface of the melt as a white transparent suspended matter. SiO amorphous or SiO
The particles of No. 2 cause the collapse of the single crystal when pulling the single crystal.
【０００６】単結晶の成長に当たり、不活性ガスに少量
の水素ガスを添加して炉内に導入し、融液に含まれる酸
素その他の不純物元素と水素とを結合させ、水素化合物
として雰囲気ガス中に放出させることによって結晶欠陥
を減少させる単結晶の成長方法が、特開昭６１−１７８
４９５で提示されている。しかしこの方法ではリチャー
ジ中に発生するＳｉＯアモルファスを効果的に排除する
ことはできない。また、原料多結晶が溶解して融液とな
るまでの間、炉内に水素ガスを流入させる単結晶成長方
法が特開平２−１６４７８８で提示されている。この場
合、カーボンヒータに含まれる不純物を還元させるには
有効であるが、水素ガスが融液面上に効果的に供給され
ないので、ＳｉＯアモルファスを排除することはできな
い。In the growth of a single crystal, a small amount of hydrogen gas is added to an inert gas and introduced into the furnace to combine oxygen and other impurity elements contained in the melt with hydrogen to form a hydrogen compound in the atmosphere gas. A method for growing a single crystal, in which crystal defects are reduced by releasing it into the crystal, is disclosed in JP-A-61-178.
495 is presented. However, this method cannot effectively eliminate SiO amorphous generated during recharging. Further, Japanese Patent Laid-Open No. 2-164788 discloses a single crystal growth method in which hydrogen gas is allowed to flow into a furnace until the raw material polycrystal is melted to form a melt. In this case, it is effective to reduce the impurities contained in the carbon heater, but since hydrogen gas is not effectively supplied onto the melt surface, SiO amorphous cannot be excluded.
【０００７】特開平３−１１５１８５による単結晶の成
長方法はＨ2 分圧が０．５気圧以上のＨ2 雰囲気中で微
小欠陥密度の小さいシリコン単結晶を成長させるもので
あるが、この場合も水素ガスは融液面上に効果的に供給
されない。概して、水素ガス雰囲気中で行う粒状多結晶
の溶解においては、融液から発生したＳｉＯアモルファ
スを効果的に排除することはできない。従って、水素ガ
スを融液面に強制的に供給する必要がある。[0007] While growing method of a single crystal according to JP-A 3-115185 are those H 2 partial pressure is growing smaller silicon single crystal having very small defect density in an H 2 atmosphere for 0.5 atm, again Hydrogen gas is not effectively supplied on the melt surface. In general, in the dissolution of granular polycrystals performed in a hydrogen gas atmosphere, SiO amorphous generated from the melt cannot be effectively removed. Therefore, it is necessary to forcibly supply hydrogen gas to the melt surface.
【０００８】特開平４−１０８６８５による単結晶引き
上げ装置は、融液中にガス供給パイプを浸漬し、このパ
イプから融液内に不活性ガスを供給して融液を上下方向
に攪拌することによって融液の組成を均一に保持するも
のである。しかし融液の攪拌は、融液面上に浮遊するＳ
ｉＯアモルファスの排除に好ましくない影響を与える。
また、特開平４−２２４１９１では、るつぼ内で融解す
る原料多結晶に加熱した気体を吹きつけて原料多結晶の
昇温を促進し、融液生成後は融液中に前記気体を吹き込
んで攪拌し、融液温度を均一化するとともに原料多結晶
の溶解所要時間を短縮する方法が提示されている。この
方法は粒状多結晶のリチャージに関するものではなく、
ＳｉＯアモルファスの排除には何ら効果がない。更に、
融液の攪拌は、ＳｉＯアモルファスの排除に悪影響を与
える。The apparatus for pulling a single crystal according to Japanese Patent Laid-Open No. 4-108685 is prepared by immersing a gas supply pipe in a melt, supplying an inert gas into the melt from this pipe, and stirring the melt in the vertical direction. It holds the composition of the melt uniformly. However, the agitation of the melt causes S floating on the melt surface.
This has an unfavorable effect on the elimination of iO amorphous.
Further, in JP-A-4-224191, a heated gas is blown to a raw material polycrystal melted in a crucible to accelerate the temperature rise of the raw material polycrystal, and after the melt is generated, the gas is blown into the melt and stirred. However, a method of making the melt temperature uniform and shortening the time required for melting the raw material polycrystal has been proposed. This method is not about recharging granular polycrystals,
It has no effect on the elimination of SiO amorphous. Furthermore,
Agitation of the melt adversely affects the elimination of SiO amorphous.
【０００９】従来、粒状多結晶のリチャージにおいて水
素ガスを供給する手段は提案されていない。本発明は、
融液内で発生したＳｉＯガスがリチャージした原料多結
晶に触れて冷却されることによってＳｉＯアモルファス
を形成することに着目し、前記ＳｉＯガスあるいはＳｉ
Ｏアモルファスを効果的に排除し、単結晶崩れの発生を
防止することができるような多結晶のリチャージ装置お
よびリチャージ方法を提供することを目的としている。Conventionally, no means has been proposed for supplying hydrogen gas in recharging a granular polycrystal. The present invention is
Focusing on the fact that the SiO gas generated in the melt touches the recharged raw material polycrystal to be cooled to form a SiO amorphous, the SiO gas or Si
An object of the present invention is to provide a polycrystal recharging device and a recharging method capable of effectively eliminating O-amorphous and preventing single crystal collapse.
【００１０】[0010]
【課題を解決するための手段】上記目的を達成するため
本発明に係る多結晶のリチャージ装置は、粒状の原料多
結晶をるつぼ内に供給する原料供給管と、この原料供給
管から放出されて融液面に浮遊する前記原料多結晶に水
素ガスもしくは水素ガスを含む不活性ガスを吹きつける
ガス供給管とを備える構成とし、このような構成におい
て、原料供給管の軸心に沿って、前記原料供給管を取り
巻くようにガス供給管を設けてもよく、原料供給管と、
ガス供給管とを同一の管で構成してもよい。To achieve the above object, a polycrystal recharging device according to the present invention is provided with a raw material supply pipe for supplying granular raw material polycrystal into a crucible, and a raw material supply pipe for discharging the raw material polycrystal. The raw material polycrystal floating on the melt surface is provided with a gas supply pipe for blowing hydrogen gas or an inert gas containing hydrogen gas, and in such a configuration, along the axis of the raw material supply pipe, A gas supply pipe may be provided so as to surround the raw material supply pipe,
The gas supply pipe may be the same pipe.
【００１１】また、本発明に係る多結晶のリチャージ方
法は、チョクラルスキー法を用いる半導体単結晶の製造
において、融液から単結晶を引き上げた後、炉外から粒
状の原料多結晶を原料供給管を介してるつぼ内に供給す
るに当たり、前記原料多結晶をリチャージする直前から
リチャージした原料多結晶の溶解が完了するまでの間、
水素ガスもしくは水素ガスを含む不活性ガスを前記原料
供給管から放出されて融液面に浮遊する原料多結晶に吹
きつけることを特徴としている。Further, in the method of recharging a polycrystal according to the present invention, in manufacturing a semiconductor single crystal using the Czochralski method, after pulling a single crystal from a melt, a granular raw material polycrystal is fed from the outside of the furnace. When supplying into the crucible via a tube, from just before recharging the raw material polycrystal to completion of melting of the recharged raw material polycrystal,
It is characterized in that hydrogen gas or an inert gas containing hydrogen gas is discharged from the raw material supply pipe and sprayed onto the raw material polycrystal floating on the melt surface.
【００１２】[0012]
【作用】上記構成によれば、粒状の原料多結晶をるつぼ
内に供給する原料供給管と、水素ガスもしくは水素ガス
を含む不活性ガスを吹きつけるガス供給管とを設置し、
原料多結晶をリチャージする直前からリチャージした原
料多結晶の溶解が完了するまでの間、融液面に浮遊する
前記原料多結晶に水素ガスもしくは水素ガスを含む不活
性ガスを吹きつけることにしたので、融液内に発生した
ＳｉＯガスは、 ＳｉＯ＋Ｈ2 →Ｓｉ＋Ｈ2Ｏ に示すように水素ガスによって還元され、シリコンと水
とに分解される。水は水蒸気として炉外に排出される。
ガス供給管の軸心に沿って前記ガス供給管の内側に原料
供給管を設けた場合、あるいは原料供給管とガス供給管
とを同一の管で構成した場合は、粒状の原料多結晶に強
制的かつ効果的に水素ガスを吹きつけることができるの
で、ＳｉＯガスは容易に分解される。According to the above structure, the raw material supply pipe for supplying the granular raw material polycrystal into the crucible and the gas supply pipe for blowing the hydrogen gas or the inert gas containing the hydrogen gas are installed.
Since it was decided to blow hydrogen gas or an inert gas containing hydrogen gas to the raw material polycrystals floating on the melt surface from immediately before recharging the raw material polycrystals until the completion of melting of the recharged raw material polycrystals. The SiO gas generated in the melt is reduced by hydrogen gas as shown by SiO + H 2 → Si + H 2 O, and decomposed into silicon and water. Water is discharged outside the furnace as steam.
When a raw material supply pipe is provided inside the gas supply pipe along the axis of the gas supply pipe, or when the raw material supply pipe and the gas supply pipe are made of the same pipe, the granular raw material polycrystal is forced. Since the hydrogen gas can be blown effectively and effectively, the SiO gas is easily decomposed.
【００１３】[0013]
【実施例】以下に本発明に係る多結晶のリチャージ装置
およびリチャージ方法の実施例について、図面を参照し
て説明する。図１は請求項２に基づくリチャージ装置を
装着した単結晶製造装置の模式的部分断面図で、チャン
バ１内にはるつぼ軸２によって回転ならびに昇降するる
つぼ３と、このるつぼ３を取り巻くヒータ４および保温
筒５が設置されている。チャンバ１の外側には図示しな
い原料供給装置が設けられ、この原料供給装置に取着さ
れた原料供給管６はチャンバ１を貫通して前記るつぼ３
の周縁部近傍上方に開口している。また、前記原料供給
管６を開閉するバルブ７の下方に、原料供給管６を取り
巻くようにガス供給管８が設けられ、ガス供給管８の上
端にはガス導入管９が接続されている。Embodiments of the polycrystal recharging device and recharging method according to the present invention will be described below with reference to the drawings. FIG. 1 is a schematic partial sectional view of a single crystal manufacturing apparatus equipped with a recharging device according to a second aspect of the present invention. A crucible 3 that rotates and moves up and down by a crucible shaft 2 in a chamber 1, a heater 4 surrounding the crucible 3 and A heat insulating cylinder 5 is installed. A raw material supply device (not shown) is provided outside the chamber 1, and a raw material supply pipe 6 attached to the raw material supply device penetrates the chamber 1 and the crucible 3 is provided.
The upper part of the opening is open near the periphery of A gas supply pipe 8 is provided below the valve 7 that opens and closes the raw material supply pipe 6 so as to surround the raw material supply pipe 6, and a gas introduction pipe 9 is connected to the upper end of the gas supply pipe 8.
【００１４】単結晶の引き上げが終了するとバルブ７を
開放し、原料供給管６を介して原料供給装置からるつぼ
３内に粒状の原料多結晶を供給する。このとき、ガス導
入管９からガス供給管８に水素ガスもしくは水素ガスを
含む不活性ガスを送り、前記ガスは下方に吹き出す。ガ
スの供給は、リチャージが終了して粒状の原料多結晶の
溶解が完了するまでの間、継続して行われる。原料供給
管６から放出された前記原料多結晶１０は融液１１の表
面に浮遊し、これに前記ガスが吹きつけられることによ
り、融液内に発生して上昇するＳｉＯガスは還元されて
シリコンと水とに分解され、水は水蒸気として炉外に排
出される。水素ガスもしくは水素ガスを含む不活性ガス
の供給量は、融液１１の表面に浮遊する原料多結晶１０
の隅々まで十分に前記ガスが行きわたり、ＳｉＯガスあ
るいはＳｉＯアモルファスを完全に還元できる程度の量
であることが望ましい。また、本装置は融液中に浸漬し
たガス供給管から融液内に水素ガスもしくは水素ガスを
含む不活性ガスを供給するものではないので、ガスによ
る融液の攪拌が起こらず、従って融液内でのＳｉＯガス
発生を助長しない。When the pulling of the single crystal is completed, the valve 7 is opened and the granular raw material polycrystal is supplied from the raw material supply device into the crucible 3 through the raw material supply pipe 6. At this time, hydrogen gas or an inert gas containing hydrogen gas is sent from the gas introduction pipe 9 to the gas supply pipe 8, and the gas is blown out downward. The gas is continuously supplied until the recharge is completed and the dissolution of the granular raw material polycrystal is completed. The raw material polycrystal 10 released from the raw material supply pipe 6 floats on the surface of the melt 11 and the gas is blown onto the raw material polycrystal 10 to reduce the SiO gas generated and rising in the melt to reduce silicon. Is decomposed into water and water, and the water is discharged as steam to the outside of the furnace. The supply amount of hydrogen gas or an inert gas containing hydrogen gas is such that the raw material polycrystal 10 floating on the surface of the melt 11
It is desirable that the amount be such that the above-mentioned gas can be sufficiently spread to all the corners and that the SiO gas or the SiO amorphous can be completely reduced. Further, since the present apparatus does not supply hydrogen gas or an inert gas containing hydrogen gas into the melt from the gas supply pipe immersed in the melt, stirring of the melt by the gas does not occur, and therefore the melt It does not promote the generation of SiO gas inside.
【００１５】直径１６インチのるつぼに塊状のシリコン
多結晶を４５ｋｇ装填し、これを溶解した後、ＣＺ法に
より直径６インチの単結晶２０ｋｇを引き上げて炉内か
ら取り出した。次にヒータ出力を２０％アップし、るつ
ぼ位置を上方に設定した状態で粒状のシリコン多結晶の
リチャージを行った。このときの粒状多結晶の供給速度
は１ｋｇ／分とし、水素ガスと不活性ガスとの混合ガス
を供給しつつ２０分間で２０ｋｇをリチャージした。前
記混合ガスは、水素とアルゴンとの比が１：９で、粒状
多結晶のリチャージ終了後、粒状多結晶が全溶するまで
の間、約１．５時間にわたって供給を継続した。粒状多
結晶が全溶したとき、融液面に白色透明の浮遊物は認め
られず、２本目の単結晶（直胴部の長さ８００ｍｍ）を
崩れることなく成長させることができた。A crucible having a diameter of 16 inches was charged with 45 kg of agglomerated silicon polycrystal, and after melting this, 20 kg of a single crystal having a diameter of 6 inches was pulled up by the CZ method and taken out from the furnace. Next, the heater output was increased by 20%, and the granular silicon polycrystal was recharged with the crucible position set to the upper side. The supply rate of the granular polycrystal at this time was 1 kg / min, and 20 kg was recharged in 20 minutes while supplying a mixed gas of hydrogen gas and an inert gas. The mixed gas had a ratio of hydrogen to argon of 1: 9, and was continuously supplied for about 1.5 hours after the completion of the recharge of the granular polycrystal and until the granular polycrystal was completely dissolved. When all the granular polycrystals were completely melted, white and transparent suspended matter was not observed on the melt surface, and the second single crystal (the length of the straight barrel portion was 800 mm) could be grown without breaking.
【００１６】上記の実施例と比較するため、直径１６イ
ンチのるつぼに塊状のシリコン多結晶を４５ｋｇ装填、
溶解し、ＣＺ法により直径６インチの単結晶２０ｋｇを
引き上げて炉内から取り出した後、ヒータ出力を２０％
アップし、るつぼ位置を上方に設定した状態で粒状のシ
リコン多結晶のリチャージを行った。ただし、水素を含
む混合ガスは供給しなかった。粒状多結晶が全溶した
後、融液面には白色透明の浮遊物が認められた。これ
は、粒状多結晶の溶解途中に融液から発生したＳｉＯガ
スが融液面に浮遊する粒状多結晶に触れて冷却され、Ｓ
ｉＯアモルファスが形成された後、前記アモルファスか
ら析出したＳｉＯ2 の細片であると考えられる。その
後、前記浮遊物が消滅するまで約３０分間溶解を継続し
た上、直径６インチの単結晶を引き上げようとしたが、
３７０ｍｍの位置で単結晶崩れが発生した。これは、融
液内にＳｉＯ2 のパーティクルが残存していたため単結
晶崩れを誘発したものと考えられる。For comparison with the above-mentioned embodiment, a crucible having a diameter of 16 inches was loaded with 45 kg of massive silicon polycrystals.
After melting and pulling out 20 kg of a 6-inch diameter single crystal by the CZ method and taking it out of the furnace, the heater output was 20%.
Up, the granular silicon polycrystal was recharged with the crucible position set to the upper side. However, the mixed gas containing hydrogen was not supplied. After all the granular polycrystals were completely dissolved, white and transparent suspended matter was observed on the melt surface. This is because the SiO gas generated from the melt during the melting of the granular polycrystals comes into contact with the granular polycrystals floating on the surface of the melt and is cooled.
It is considered to be a piece of SiO 2 deposited from the amorphous amorphous material after the io-amorphous material is formed. After that, the melting was continued for about 30 minutes until the suspended matter disappeared, and a single crystal having a diameter of 6 inches was tried to be pulled.
Single crystal collapse occurred at a position of 370 mm. It is considered that this is because the particles of SiO 2 remained in the melt, which caused the collapse of the single crystal.
【００１７】請求項１に基づくリチャージ装置は原料供
給管とガス供給管とがそれぞれ独立に配設されており、
請求項３に基づくリチャージ装置は原料供給管とガス供
給管とが同一の管で構成されている。ガス供給管の機能
は、いずれの場合も請求項２の場合と同じであり、リチ
ャージされて融液面に浮遊する原料多結晶に水素ガスも
しくは水素ガスを含む不活性ガスを吹きつけるものであ
るので、詳細説明を省略する。In the recharging device according to the first aspect, the raw material supply pipe and the gas supply pipe are arranged independently of each other,
In the recharging device according to the third aspect, the raw material supply pipe and the gas supply pipe are the same pipe. In any case, the function of the gas supply pipe is the same as in the case of claim 2, and hydrogen gas or an inert gas containing hydrogen gas is blown to the raw material polycrystals that are recharged and float on the melt surface. Therefore, detailed description is omitted.
【００１８】[0018]
【発明の効果】以上説明したように本発明によれば、粒
状の原料多結晶のリチャージ開始から溶解完了までの
間、水素ガスもしくは水素ガスを含む不活性ガスを融液
面に浮遊する原料多結晶に吹きつけるリチャージ装置お
よびリチャージ方法を用いることにしたので、融液内に
発生するＳｉＯガスは水素ガスによって還元され、Ｓｉ
ＯアモルファスやＳｉＯ2 を形成することがない。従っ
て、リチャージ法適用時における単結晶崩れの発生を防
止することができ、単結晶化率の向上すなわち単結晶生
産能率を引き上げることが可能となる。As described above, according to the present invention, from the start of recharging of the granular raw material polycrystal to the completion of melting, hydrogen gas or an inert gas containing hydrogen gas is suspended in the melt surface. Since it was decided to use a recharging device and a recharging method for spraying onto the crystal, the SiO gas generated in the melt was reduced by hydrogen gas,
It does not form O-amorphous or SiO 2 . Therefore, it is possible to prevent the occurrence of single crystal collapse when the recharging method is applied, and it is possible to improve the single crystallization rate, that is, increase the single crystal production efficiency.
【図１】請求項２に基づくリチャージ装置を装着した単
結晶製造装置の模式的部分断面図である。FIG. 1 is a schematic partial cross-sectional view of a single crystal manufacturing apparatus equipped with a recharge device according to claim 2.
３ るつぼ ６ 原料供給管 ８ ガス供給管 １０ 原料多結晶 １１ 融液 3 Crucible 6 Raw material supply pipe 8 Gas supply pipe 10 Raw material polycrystal 11 Melt
Claims (4)
原料供給管と、この原料供給管から放出されて融液面に
浮遊する前記原料多結晶に水素ガスもしくは水素ガスを
含む不活性ガスを吹きつけるガス供給管とを備えている
ことを特徴とする多結晶のリチャージ装置。1. A raw material supply pipe for supplying granular raw material polycrystal into a crucible, and hydrogen gas or an inert gas containing hydrogen gas in the raw material polycrystal discharged from the raw material supply pipe and floating on the melt surface. And a gas supply pipe for spraying the gas.
給管を取り巻くようにガス供給管を設けたことを特徴と
する請求項１の多結晶のリチャージ装置。2. The polycrystal recharging device according to claim 1, wherein a gas supply pipe is provided along the axis of the raw material supply pipe so as to surround the raw material supply pipe.
で構成したことを特徴とする請求項１の多結晶のリチャ
ージ装置。3. The polycrystal recharging device according to claim 1, wherein the raw material supply pipe and the gas supply pipe are formed of the same pipe.
晶の製造において、融液から単結晶を引き上げた後、炉
外から粒状の原料多結晶を原料供給管を介してるつぼ内
に供給するに当たり、前記粒状の原料多結晶をリチャー
ジする直前からリチャージした原料多結晶の溶解が完了
するまでの間、水素ガスもしくは水素ガスを含む不活性
ガスを前記原料供給管から放出されて融液面に浮遊する
原料多結晶に吹きつけることを特徴とする多結晶のリチ
ャージ方法。4. In the production of a semiconductor single crystal using the Czochralski method, after pulling a single crystal from a melt, when supplying a granular raw material polycrystal from the outside of a furnace into a crucible through a raw material supply pipe, Immediately before the granular raw material polycrystal is recharged until the recharged raw material polycrystal is completely dissolved, hydrogen gas or an inert gas containing hydrogen gas is discharged from the raw material supply pipe and floats on the melt surface. A method of recharging a polycrystal characterized by spraying a raw polycrystal.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05287622A JP3085567B2 (en) | 1993-10-22 | 1993-10-22 | Polycrystalline recharge apparatus and recharge method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP05287622A JP3085567B2 (en) | 1993-10-22 | 1993-10-22 | Polycrystalline recharge apparatus and recharge method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07118089A true JPH07118089A (en) | 1995-05-09 |
| JP3085567B2 JP3085567B2 (en) | 2000-09-11 |
Family
ID=17719641
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP05287622A Expired - Fee Related JP3085567B2 (en) | 1993-10-22 | 1993-10-22 | Polycrystalline recharge apparatus and recharge method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3085567B2 (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0945529A1 (en) * | 1998-03-26 | 1999-09-29 | Leybold Systems GmbH | Crystal pulling apparatus |
| EP0945528A1 (en) * | 1998-03-26 | 1999-09-29 | Leybold Systems GmbH | Crystal pulling apparatus |
| JP2006312115A (en) * | 2005-05-06 | 2006-11-16 | Tokyo Electric Power Co Inc:The | Gas pressure-filling apparatus and gas pressure-filling method |
| JP2007284320A (en) * | 2006-04-20 | 2007-11-01 | Sharp Corp | Solid melting apparatus and method for feeding raw material |
| EP2072645A2 (en) | 2007-12-19 | 2009-06-24 | Schott AG | Method for producing a monocrystalline or polycrystalline semiconductor material |
| DE102008022882A1 (en) | 2008-05-08 | 2009-11-05 | Schott Ag | Producing monocrystalline or polycrystalline semiconductor material using a vertical gradient freeze method, involves introducing lumpy semiconductor raw material into a melting crucible, melting there, and directionally solidifying |
| US20100107966A1 (en) * | 2008-11-05 | 2010-05-06 | Memc Electronic Materials, Inc. | Methods for preparing a melt of silicon powder for silicon crystal growth |
-
1993
- 1993-10-22 JP JP05287622A patent/JP3085567B2/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0945529A1 (en) * | 1998-03-26 | 1999-09-29 | Leybold Systems GmbH | Crystal pulling apparatus |
| EP0945528A1 (en) * | 1998-03-26 | 1999-09-29 | Leybold Systems GmbH | Crystal pulling apparatus |
| JP2006312115A (en) * | 2005-05-06 | 2006-11-16 | Tokyo Electric Power Co Inc:The | Gas pressure-filling apparatus and gas pressure-filling method |
| JP2007284320A (en) * | 2006-04-20 | 2007-11-01 | Sharp Corp | Solid melting apparatus and method for feeding raw material |
| JP4762776B2 (en) * | 2006-04-20 | 2011-08-31 | シャープ株式会社 | Solid melting equipment |
| EP2072645A2 (en) | 2007-12-19 | 2009-06-24 | Schott AG | Method for producing a monocrystalline or polycrystalline semiconductor material |
| US8101019B2 (en) | 2007-12-19 | 2012-01-24 | Schott Ag | Method for producing a monocrystalline or polycrystalline semiconductor material |
| EP2072645B2 (en) † | 2007-12-19 | 2014-12-24 | Schott AG | Method for producing a monocrystalline or polycrystalline semiconductor material |
| DE102008022882A1 (en) | 2008-05-08 | 2009-11-05 | Schott Ag | Producing monocrystalline or polycrystalline semiconductor material using a vertical gradient freeze method, involves introducing lumpy semiconductor raw material into a melting crucible, melting there, and directionally solidifying |
| US20100107966A1 (en) * | 2008-11-05 | 2010-05-06 | Memc Electronic Materials, Inc. | Methods for preparing a melt of silicon powder for silicon crystal growth |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3085567B2 (en) | 2000-09-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4103593B2 (en) | Recharge tube for solid polycrystalline raw material and method for producing single crystal using the same | |
| JPH11189495A (en) | Silicon single crystal and its production | |
| TWI422716B (en) | Crystal growing method | |
| US20100139549A1 (en) | Quartz Glass Crucible for Pulling Silicon Single Crystal and Method of Manufacturing Quartz Glass Crucible for Pulling Silicon Single Crystal | |
| JP3085567B2 (en) | Polycrystalline recharge apparatus and recharge method | |
| JP2001233629A (en) | Method of producing quartz glass crucible | |
| WO2000052235A1 (en) | Method for producing silicon single crystal | |
| WO2023051616A1 (en) | Crystal pulling furnace for pulling monocrystalline silicon rod | |
| JP4788445B2 (en) | Pulling method of silicon single crystal | |
| JP3832536B2 (en) | Method for producing silicon single crystal and pulling machine | |
| JPH1149597A (en) | Quartz crucible for pulling up silicon single crystal | |
| JPH1192276A (en) | Apparatus for producing semiconductor single crystal and production of semiconductor single crystal | |
| JPH11195565A (en) | Silicon wafer and method of growing crystal | |
| JPH0748200A (en) | Production of single crystal | |
| JPS5933552B2 (en) | crystal growth equipment | |
| CN109576778A (en) | A method of reducing the impurity content that CZ method prepares monocrystalline | |
| JP3885245B2 (en) | Single crystal pulling method | |
| JP4330230B2 (en) | Single crystal growth method | |
| JP4807130B2 (en) | Pulling method of silicon single crystal | |
| JPH0640592Y2 (en) | Silicon single crystal growth equipment | |
| JP2004292288A (en) | Method for melting raw material for silicon single crystal | |
| JP2531875B2 (en) | Method for producing compound semiconductor single crystal | |
| JPH09241091A (en) | Device for growing single crystal and method for growing the same | |
| JP2009173503A (en) | Single crystal pulling device and method for manufacturing single crystal | |
| JPH1192275A (en) | Apparatus for producing semiconductor single crystal and production of semiconductor single crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |