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JPH0317770B2 - - Google Patents
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JPH0317770B2 - - Google Patents

Info

Publication number
JPH0317770B2
JPH0317770B2 JP22394582A JP22394582A JPH0317770B2 JP H0317770 B2 JPH0317770 B2 JP H0317770B2 JP 22394582 A JP22394582 A JP 22394582A JP 22394582 A JP22394582 A JP 22394582A JP H0317770 B2 JPH0317770 B2 JP H0317770B2
Authority
JP
Japan
Prior art keywords
reaction
wall material
reaction chamber
chamber
transparent quartz
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
Application number
JP22394582A
Other languages
Japanese (ja)
Other versions
JPS59115739A (en
Inventor
Yosha Iida
Takao Hasegawa
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.)
Tokuyama Corp
Original Assignee
Tokuyama Corp
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 Tokuyama Corp filed Critical Tokuyama Corp
Priority to JP22394582A priority Critical patent/JPS59115739A/en
Publication of JPS59115739A publication Critical patent/JPS59115739A/en
Publication of JPH0317770B2 publication Critical patent/JPH0317770B2/ja
Granted legal-status Critical Current

Links

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0006Controlling or regulating processes
    • B01J19/0013Controlling the temperature of the process
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00074Controlling the temperature by indirect heating or cooling employing heat exchange fluids
    • B01J2219/00087Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
    • B01J2219/00094Jackets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00051Controlling the temperature
    • B01J2219/00132Controlling the temperature using electric heating or cooling elements
    • B01J2219/00135Electric resistance heaters

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Silicon Compounds (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)

Description

【発明の詳細な説明】 本発明は反応室内に設けた芯棒に化学反応によ
つて生成する結晶を付着させるような反応に特に
適した新規な反応装置に関する。詳しくはガス入
口及びガス出口を有する室枠と壁材で反応室を構
成し、該反応室内に電導性棒の両端が1対の電源
端子に接続されて構成された通電部を設け且つ壁
材は外面に反射膜を設けた透明石英で構成してな
る反応装置である。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a novel reaction apparatus particularly suitable for a reaction in which crystals produced by a chemical reaction are attached to a core rod provided in a reaction chamber. Specifically, a reaction chamber is constituted by a chamber frame having a gas inlet and a gas outlet, and a wall material, a current-carrying part configured by connecting both ends of a conductive rod to a pair of power terminals is provided in the reaction chamber, and a wall material is provided. is a reaction device made of transparent quartz with a reflective film on its outer surface.

反応装置は対象反応に応じて種々のものが知ら
れている。例えば反応室内に設けた芯棒に高温下
で化学反応を起し、生成する結晶を該芯棒に付着
成長させる反応例えば反応室内でトリクロルシラ
ンを水素で還元,熱分解し、シリコンを予め設け
た芯棒に、成長させる反応等の反応装置は耐食性
で、耐熱性のものが使用されている。更に具体的
にはガス入口及びガス出口を有する室枠と壁材で
反応室を構成し、該反応室内に電導性棒の両端が
1対の電源端子に接続されて構成された反応装置
が知られている。この場合電源から通電される電
流は、電導性棒の抵抗のため、該電導性棒で熱エ
ネルギーに代えられ、高温の反応温度を保持す
る。また上記高温下での反応はしばしば腐食性ガ
スの発生を伴う。従つて壁材は耐食性で耐熱性で
あるステンレス又は不透明石英が使用されてい
る。しかし後者即ち不透明石英を壁材としようと
すれば壁材自身が熱を吸収するため熱源のロスを
まぬがれることが出来ない。
Various types of reaction apparatuses are known depending on the target reaction. For example, a reaction in which a chemical reaction occurs under high temperature on a core rod installed in a reaction chamber, and the resulting crystals adhere to and grow on the core rod. For example, trichlorosilane is reduced and thermally decomposed with hydrogen in the reaction chamber, and silicon is pre-prepared. Corrosion-resistant and heat-resistant materials are used for the core rod and reaction equipment used for growth reactions. More specifically, a reaction apparatus is known in which a reaction chamber is constructed of a chamber frame and a wall material having a gas inlet and a gas outlet, and both ends of a conductive rod are connected to a pair of power supply terminals in the reaction chamber. It is being In this case, the electric current supplied from the power supply is converted into thermal energy by the conductive rod due to its resistance, thereby maintaining a high reaction temperature. Furthermore, the above-mentioned reactions at high temperatures often involve the generation of corrosive gases. Therefore, the wall material is made of corrosion-resistant and heat-resistant stainless steel or opaque quartz. However, if the latter, that is, opaque quartz, is used as a wall material, the wall material itself absorbs heat, making it impossible to avoid heat source loss.

本発明は壁材の材質として透明石英を用い熱源
の吸収を防止すると共に該熱源を反応に関与させ
るために壁材の外面に反射膜を設けることによ
り、上記欠点を完全に解消しうることを知見し、
完成させたものである。
The present invention proposes that the above drawbacks can be completely eliminated by using transparent quartz as the material of the wall material and providing a reflective film on the outer surface of the wall material to prevent absorption of the heat source and to make the heat source participate in the reaction. I found out,
It has been completed.

即ち本発明はガス入口1及びガス出口2を有す
る室枠3と壁材4で反応室5を構成し、該反応室
内に電導性棒6の両端が1対の電源端子7に接続
されて構成された通電部を設け且つ壁材は外面に
反射膜を設けた透明石英で構成してなる反応装置
である。
That is, in the present invention, a reaction chamber 5 is constituted by a chamber frame 3 having a gas inlet 1 and a gas outlet 2 and a wall material 4, and both ends of a conductive rod 6 are connected to a pair of power supply terminals 7 in the reaction chamber. The reactor is equipped with a energized section, and the wall material is made of transparent quartz with a reflective film on the outer surface.

本発明を詳細に説明するため、以下添付図面に
準じ、且つトリクロルシランを水素によつて還
元,熱分解し、シリコンを製造する反応に適した
反応装置について説明するが、本発明は以下の説
明に限定されるものではなく、反応装置の対象反
応は如何なるものであつてもよい。
In order to explain the present invention in detail, a reaction apparatus suitable for the reaction of reducing and thermally decomposing trichlorosilane with hydrogen and producing silicon will be described below in accordance with the attached drawings. The target reaction of the reaction apparatus is not limited to, and any reaction may be performed.

添付図面第1図及び第2図はそれぞれ、本発明
の代表的な反応装置を示す断面図である。
The accompanying drawings, FIGS. 1 and 2, are each a cross-sectional view showing a typical reaction apparatus of the present invention.

本発明の反応装置はガス入口1及びガス出口2
を有する室枠3と壁材4とで反応室を構成してい
る。該ガス入口1及びガス出口2はそれぞれ1個
設けるのが一般的であるが、複数個設けてもよ
い。また該ガス入口1及びガス出口2の形状は特
に限定的ではない。例えばトリクロルシランと水
素とを予め混合して唯一のガス入口から反応室内
に供給してもよく、2重管以上の多重管を用いト
リクロルシラン,水素或いは必要に応じて稀釈ガ
スを別々の管から該管供給口又は反応室内で混合
されるように供給することも出来る。また室枠3
の材質も特に限定的ではなく耐食性 の良好な公知のものから適宜選択して実施すれ
ばよい。一般に好適に使用されるものを例示すれ
ば石英,金,銀,銅或いはステンレス等である。
The reactor of the present invention has a gas inlet 1 and a gas outlet 2.
A reaction chamber is constituted by a chamber frame 3 and a wall material 4. Although it is common to provide one gas inlet 1 and one gas outlet 2, a plurality of gas inlets 1 and gas outlets 2 may be provided. Further, the shapes of the gas inlet 1 and the gas outlet 2 are not particularly limited. For example, trichlorosilane and hydrogen may be mixed in advance and supplied into the reaction chamber from a single gas inlet, or trichlorosilane, hydrogen, or diluent gas, if necessary, may be supplied from separate tubes using multiple tubes of double or more. They can also be supplied so as to be mixed within the tube supply port or within the reaction chamber. Also room frame 3
The material is not particularly limited, and may be suitably selected from known materials with good corrosion resistance. Examples of materials that are generally preferably used include quartz, gold, silver, copper, and stainless steel.

本発明で用いる壁材4は透明石英9であること
が必須である。この理由は熱エネルギーが石英に
吸収されて発熱することを防ぐためである。しか
し単に透明石英を使用すると反応に関与する熱エ
ネルギーは全て反応室外へ飛散するので、かかる
不利を防止する手段として本発明にあつては、壁
材を構成する透明石英の外面に反射膜8を設け
る。該反射膜は反応に関与する熱エネルギーが透
明石英を通過しても反射することによつて反応熱
源として利用することにより、より効率よく該エ
ネルギーを利用するために設けられたものであ
る。一般に該反射膜の材質は特に限定されない
が、壁材と出来るだけ一体化して使用するのがよ
く、また出来るだけ反射率の良好なものがよく、
耐熱性である必要がある。このような理由から
金,銀,銅或いはアルミニウム等の金属膜が好適
に使用される。該反射膜を透明石英の外面に設け
る手段は特に限定的ではなく、如何ある手段を採
用してもよい。一般には特に壁材の透明石英の外
面に真空蒸着,スパツタリング,無電界メツキ等
の手段で一体化したものが最も効果的である。
It is essential that the wall material 4 used in the present invention is transparent quartz 9. The reason for this is to prevent thermal energy from being absorbed by the quartz and generating heat. However, if transparent quartz is simply used, all the thermal energy involved in the reaction will be scattered outside the reaction chamber, so as a means to prevent this disadvantage, in the present invention, a reflective film 8 is provided on the outer surface of the transparent quartz that constitutes the wall material. establish. The reflective film is provided in order to use the thermal energy involved in the reaction more efficiently by reflecting it even if it passes through the transparent quartz and using it as a heat source for the reaction. In general, the material of the reflective film is not particularly limited, but it is preferable to use it as integrated with the wall material as possible, and it is also preferable that it has as good a reflectance as possible.
Must be heat resistant. For this reason, metal films such as gold, silver, copper, or aluminum are preferably used. The means for providing the reflective film on the outer surface of the transparent quartz is not particularly limited, and any means may be employed. In general, it is most effective to integrate the material onto the outer surface of the transparent quartz wall material by means such as vacuum deposition, sputtering, or electroless plating.

本発明の反応室内には電導性棒6の両端が1対
の電源端子7に接続されて構成された通電部を設
けることが必要である。該電導性棒は特に限定さ
れないがトリクロルシランの還元熱分解によつて
生じたシリコンが付着し、成長していく芯材の役
目と通電時に該電導性棒自身が有する抵抗のため
発熱し、電流を熱エネルギーへ変換する役目をは
たす意味でシリコンの多結晶又は単結晶からなる
棒が最も好適である。勿論電導性のものであれば
上記シリコン以外にも例えばタンタル棒等も必要
に応じて使用出来る。
In the reaction chamber of the present invention, it is necessary to provide a current-carrying section in which both ends of a conductive rod 6 are connected to a pair of power supply terminals 7. Although the conductive rod is not particularly limited, silicon produced by reductive thermal decomposition of trichlorosilane adheres to it and acts as a growing core material, and when electricity is applied, it generates heat due to the resistance of the conductive rod itself. A rod made of polycrystalline or single-crystalline silicon is most suitable because it serves to convert energy into thermal energy. Of course, in addition to the above-mentioned silicon, for example, a tantalum bar or the like can be used if necessary as long as it is conductive.

以上の説明から明らかな如く、電源端子に連結
された電導性棒6によつて電流が熱エネルギーに
変換され、反応温度を保持出来る。該熱エネルギ
ーは壁材の透明石英は通過するが該壁材の外面に
設けられた反射膜の作用により、再び反応室にフ
イードバツクされ、輻射熱として十分に効率よく
利用される。
As is clear from the above explanation, the electrical current is converted into thermal energy by the conductive rod 6 connected to the power supply terminal, and the reaction temperature can be maintained. The thermal energy passes through the transparent quartz wall material, but is fed back to the reaction chamber again by the action of the reflective film provided on the outer surface of the wall material, and is utilized efficiently as radiant heat.

尚第1図は電導性棒6をコ字型にセツトした反
応装置を、第2図は電導性棒6が1本の棒状とな
つている代表的な実施態様を示す説明図である。
図中、10は電導性棒の保持員を示す。また室枠
3は非電導性の材料とするが電源端子7との間に
絶縁体を設けて電導性材料とすることは言うまで
もない。
In addition, FIG. 1 is an explanatory view showing a reaction apparatus in which the conductive rod 6 is set in a U-shape, and FIG. 2 is an explanatory view showing a typical embodiment in which the conductive rod 6 is set in the shape of one rod.
In the figure, 10 indicates a holder for the conductive rod. Further, although the chamber frame 3 is made of a non-conductive material, it goes without saying that an insulator is provided between it and the power supply terminal 7 to make it a conductive material.

熱分解反応に使用する反応装置は高熱を発生す
るために電力多消費型の代表的なものであつた
が、本発明の完成により著しく電力消費量が小さ
い例えば従来のものの60%程度の電力消費の反応
装置となり、工業的に計り知れない寄与をなす。
The reactor used for the thermal decomposition reaction was a typical type that consumed a lot of power because it generated high heat, but with the completion of the present invention, the power consumption is significantly lower, for example, about 60% of that of conventional equipment. reaction equipment, making an immeasurable contribution to industry.

実施例 第1図に示す構成において、壁材は透明石英容
器の内径400mm,高さ1900mm,肉厚20mmのものを
用い、銀鏡反応を用いて外壁に厚さ約0.1mmの銀
薄膜を付着させた。1対の電極を300mmの間隔で
配置し、U字型のシリコン多結晶棒(5mmφ)を
表面温度を1150℃に保ちながらトリクロルシラン
と水素とを1:10の割合で予め混合し、反応室に
供給し、トリクロルシランの還元・熱分解反応を
実施した。生成したシリコンはU字型のシリコン
多結晶棒を高さ1500mm,最大直径200mmまで成長
させた。この時の所要電力は15000キロワツト時
であつた。また比較のため上記壁材の材質を不透
明石英とした以外は同じ条件で多結晶棒を作製し
た所25000キロワツト時であつた。
Example In the configuration shown in Figure 1, the wall material was a transparent quartz container with an inner diameter of 400 mm, a height of 1900 mm, and a wall thickness of 20 mm.A thin silver film of about 0.1 mm in thickness was attached to the outer wall using a silver mirror reaction. Ta. A pair of electrodes are placed at a spacing of 300 mm, and a U-shaped polycrystalline silicon rod (5 mmφ) is premixed with trichlorosilane and hydrogen at a ratio of 1:10 while maintaining the surface temperature at 1150°C. The reduction and thermal decomposition reaction of trichlorosilane was carried out. The resulting silicon was grown into a U-shaped polycrystalline silicon rod with a height of 1,500 mm and a maximum diameter of 200 mm. The power required at this time was 15,000 kilowatt hours. For comparison, a polycrystalline bar was manufactured under the same conditions except that the material for the wall material was opaque quartz, and the power consumption was 25,000 kilowatt hours.

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

第1図及び第2図は本発明の反応装置の代表的
なものを示す断面図である。 図中、1はガス入口、2はガス出口、3は室
枠、4は壁材、5は反応室、6は電導性棒、7は
電源端子、8は反射膜、9は透明石英である。
FIGS. 1 and 2 are cross-sectional views showing typical reactors of the present invention. In the figure, 1 is a gas inlet, 2 is a gas outlet, 3 is a chamber frame, 4 is a wall material, 5 is a reaction chamber, 6 is a conductive rod, 7 is a power terminal, 8 is a reflective film, and 9 is transparent quartz. .

Claims (1)

【特許請求の範囲】 1 ガス入口1及びガス出口2を有する室枠3と
壁材4で反応室5を構成し、該反応室内に電導性
棒6の両端が1対の電源端子7に接続されて構成
された通電部を設け且つ壁材は外面に反射膜8を
設けた透明石英9で構成してなる反応装置。 2 壁材が反射膜と透明石英とを一体化したもの
である特許請求の範囲1記載の反応装置。
[Scope of Claims] 1 A reaction chamber 5 is constituted by a chamber frame 3 having a gas inlet 1 and a gas outlet 2 and a wall material 4, and both ends of a conductive rod 6 are connected to a pair of power terminals 7 in the reaction chamber. A reaction device is provided with a current-carrying part configured as shown in FIG. 2. The reaction device according to claim 1, wherein the wall material is an integral part of a reflective film and transparent quartz.
JP22394582A 1982-12-22 1982-12-22 reactor Granted JPS59115739A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP22394582A JPS59115739A (en) 1982-12-22 1982-12-22 reactor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP22394582A JPS59115739A (en) 1982-12-22 1982-12-22 reactor

Publications (2)

Publication Number Publication Date
JPS59115739A JPS59115739A (en) 1984-07-04
JPH0317770B2 true JPH0317770B2 (en) 1991-03-08

Family

ID=16806157

Family Applications (1)

Application Number Title Priority Date Filing Date
JP22394582A Granted JPS59115739A (en) 1982-12-22 1982-12-22 reactor

Country Status (1)

Country Link
JP (1) JPS59115739A (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5651104B2 (en) * 2009-02-27 2015-01-07 株式会社トクヤマ Polycrystalline silicon rod and manufacturing apparatus thereof
DE102011084137A1 (en) 2011-10-07 2013-04-11 Wacker Chemie Ag Apparatus and method for depositing polycrystalline silicon

Also Published As

Publication number Publication date
JPS59115739A (en) 1984-07-04

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