JPH0686659B2 - Silicon carbide film manufacturing method - Google Patents
Silicon carbide film manufacturing methodInfo
- Publication number
- JPH0686659B2 JPH0686659B2 JP22775686A JP22775686A JPH0686659B2 JP H0686659 B2 JPH0686659 B2 JP H0686659B2 JP 22775686 A JP22775686 A JP 22775686A JP 22775686 A JP22775686 A JP 22775686A JP H0686659 B2 JPH0686659 B2 JP H0686659B2
- Authority
- JP
- Japan
- Prior art keywords
- gas
- acetylene
- silicon carbide
- film
- sic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03G—ELECTROGRAPHY; ELECTROPHOTOGRAPHY; MAGNETOGRAPHY
- G03G5/00—Recording members for original recording by exposure, e.g. to light, to heat, to electrons; Manufacture thereof; Selection of materials therefor
- G03G5/02—Charge-receiving layers
- G03G5/04—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor
- G03G5/08—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic
- G03G5/082—Photoconductive layers; Charge-generation layers or charge-transporting layers; Additives therefor; Binders therefor characterised by the photoconductive material being inorganic and not being incorporated in a bonding material, e.g. vacuum deposited
- G03G5/08214—Silicon-based
- G03G5/08278—Depositing methods
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明はアセチレン及びケイ素含有ガスを原料としたシ
リコンカーバイド膜の製法に係り、詳細にはアセチレン
生成用原料に溶解アセチレンを用いて低コスト化が達成
され且つ高品質なシリコンカーバイドが得られるように
なったシリコンカーバイド膜の製法に関するものであ
る。TECHNICAL FIELD The present invention relates to a method for producing a silicon carbide film using acetylene and a silicon-containing gas as raw materials, and more specifically, using dissolved acetylene as a raw material for producing acetylene to reduce costs. The present invention relates to a method for producing a silicon carbide film which has achieved the above and has been able to obtain a high quality silicon carbide film.
近年、薄膜生成技術の進展に伴って半導体特性を有する
シリコンカーバイド膜が生成されるようになり、この膜
がアモルファスシリコン膜に比べて大きなバンドギャッ
プをもつと共に耐熱性、耐熱衝撃性にも優れているので
短波長側で用いられる発光・受光素子として注目されて
いる。In recent years, with the progress of thin film formation technology, a silicon carbide film having semiconductor characteristics has been formed. This film has a larger band gap than an amorphous silicon film and is excellent in heat resistance and thermal shock resistance. Therefore, it is attracting attention as a light emitting / receiving element used on the short wavelength side.
このシリコンカーバイド膜は、例えばグロー放電分解法
により生成され、その生成用ガスはメタン、エタン、プ
ロパン、エチレンなどの炭素含有ガス、並びにシラン、
ジシランなどのケイ素含有ガスを組合わして用いられて
おり、これによってシリコンカーバイド（以下、SiCと
略す）半導体などが得られる。This silicon carbide film is produced by, for example, a glow discharge decomposition method, and the production gas is methane, ethane, propane, a carbon-containing gas such as ethylene, and silane,
It is used in combination with a silicon-containing gas such as disilane, whereby a silicon carbide (hereinafter abbreviated as SiC) semiconductor or the like can be obtained.
しかしながら、上記ガスを用いてSiC半導体膜を形成す
ると１μm/時以下という低い成膜速度となり、SiC半導
体を製作して実用化させるに当たっては高い成膜速度が
望まれる。例えば、電子写真感光体用にアモルファスシ
リコンカーバイド（以下、a-SiCと略す）光導電材料を
用いた場合、その光導電層の厚みえ約５〜30μｍにまで
大きくなり、その要求は多大である。However, when a SiC semiconductor film is formed using the above-mentioned gas, the film formation rate is as low as 1 μm / hour or less, and a high film formation rate is desired in manufacturing and putting the SiC semiconductor into practical use. For example, when an amorphous silicon carbide (hereinafter abbreviated as a-SiC) photoconductive material is used for an electrophotographic photoreceptor, the thickness of the photoconductive layer is increased to about 5 to 30 μm, and the demand is great. .
かかる要求に対して本発明者等は前記炭素含有ガスにア
セチレン（C2H2）を用いると著しく高い成膜速度が得ら
れることを見い出し、これによって得られたa-SiC光導
電層は電子写真感光体として実用化できることも知見し
た。In response to such a demand, the present inventors have found that when acetylene (C 2 H 2 ) is used as the carbon-containing gas, a remarkably high film formation rate can be obtained, and the a-SiC photoconductive layer obtained by this is an electron. We have also found that it can be put to practical use as a photographic photoreceptor.
このような薄膜生成用アセチレンには高純度に精製され
ている必要があり、これには高純度アセチレンボンベ
（純度100％ただし正確に表示すればシックスナインで
ある。また、分解爆発性があるため充填圧は0.5Kg/cm2
以下に設定される）を用いることができる。Acetylene for thin film formation needs to be highly purified, and it has a high purity acetylene cylinder (purity 100%, but it is Six Nine if it is accurately indicated. Pressure is 0.5 Kg / cm 2
(Set below) can be used.
しかしながら、上記アセチレンボンベはメタン、エタン
などの高純度圧縮ボンベに比べて充填圧が格段に小さ
く、常圧換算で比較した場合、そのガス容積が1/100以
下となり、これにより、消費されるボンベの数が著しく
多くなる。However, the above acetylene cylinder has a much smaller filling pressure than high-purity compressed cylinders such as methane and ethane, and when compared in terms of atmospheric pressure, the gas volume becomes 1/100 or less, which causes the cylinder to be consumed. The number of
例えば、アセチレンとシランの混合ガスをグロー放電分
解して約25μｍの厚みを持つa-SiC電子写真感光体を製
作した場合、47容積のアセチレンボンベ１本当たり約
３〜５本の感光体ドラムが成膜できるにすぎなく、その
結果、アセチレンボンベの取換え回数が多くなって製造
効率が著しく低下する。For example, when an a-SiC electrophotographic photosensitive member having a thickness of about 25 μm is produced by glow discharge decomposition of a mixed gas of acetylene and silane, about 3 to 5 photosensitive drums are used for one 47-volume acetylene cylinder. Only the film can be formed, and as a result, the number of times the acetylene cylinder is replaced becomes large and the production efficiency is significantly reduced.
また、一般的に半導体薄膜を製作するに際して反応室に
導入されるガスの流量は精密に制御する必要があり、そ
のためにはガスボンベの充填圧（一次圧）を0.5Kg/cm2
以上に設定しなくてはならない。これによってガス導入
系に接続されたマスフローコントローラを正常に作動さ
せてガスの流量を精密に制御することができる。Further, generally, when manufacturing a semiconductor thin film, it is necessary to precisely control the flow rate of gas introduced into the reaction chamber. For that purpose, the filling pressure (primary pressure) of the gas cylinder is 0.5 kg / cm 2
You must set the above. This allows the mass flow controller connected to the gas introduction system to operate normally and the gas flow rate to be precisely controlled.
しかしながら、上記アセチレンボンベの充填圧は0.5Kg/
cm2に満たないので所要の精密なガス流量に設定するこ
とが困難である。However, the filling pressure of the acetylene cylinder is 0.5 kg /
Since it is less than cm 2 , it is difficult to set the required precise gas flow rate.
即ち、このアセチレンボンベには元バルブと圧力調整器
が順次接続され、元バルブを開放して充填圧によってア
セチレンガスを放出させ、更に圧力調整器によって所要
のガス圧に低下させて二次圧とすることができるが、一
次圧が0.5Kg/cm2に満たないので、圧力調整器によって
二次圧をそれ以下のガス圧に設定することが困難とな
り、そのため、通常は圧力調整器の弁を全開にして二次
圧を一次圧と同一にする。このようにしてアセチレンボ
ンベを用いるとボンベ内の残余のガス量が減少するのに
伴ってマスフローコントローラに加わる圧力が低下し、
これにより、マスフローコントローラによって正確且つ
精密なガス流量制御が難しくなり、その結果、所要の半
導体特性を有する高品質なSiC半導体が得られない。That is, a main valve and a pressure regulator are sequentially connected to this acetylene cylinder, the main valve is opened to release the acetylene gas by the filling pressure, and further the pressure regulator lowers the gas pressure to a required level to make the secondary pressure. However, since the primary pressure is less than 0.5 Kg / cm 2 , it is difficult to set the secondary pressure to a gas pressure lower than that by the pressure regulator, and therefore the valve of the pressure regulator is usually used. Fully open to make the secondary pressure the same as the primary pressure. When the acetylene cylinder is used in this way, the pressure applied to the mass flow controller decreases as the residual gas amount in the cylinder decreases.
This makes it difficult to accurately and precisely control the gas flow rate by the mass flow controller, and as a result, a high-quality SiC semiconductor having the required semiconductor characteristics cannot be obtained.
本発明者等は上記事情に鑑みて鋭意研究に努めた結果、
造船工業等でガス溶接或いは切断用ガスとして最も多用
されている低コストの溶解アセチレンがSiC膜生成用ア
セチレン原料として用いられ得ることを見い出した。The present inventors, as a result of strenuous research in view of the above circumstances,
It has been found that low-cost molten acetylene, which is most often used as a gas for welding or cutting in the shipbuilding industry and the like, can be used as an acetylene raw material for producing a SiC film.
従って本発明は上記知見に基づいて完成されたものであ
り、その目的は高速成膜を達成したSiC膜の製法を提供
することにある。Therefore, the present invention has been completed based on the above findings, and an object thereof is to provide a method for producing a SiC film that achieves high-speed film formation.
本発明の他の目的はSiC膜の炭素源に低コストの溶解ア
セチレンを用いて原料コストを低減させると共に消費さ
せるボンベの数を少なくして作業能率を高め、これによ
って製造効率及び製造コストを改善したSiC膜の製法を
提供することにある。Another object of the present invention is to reduce the raw material cost by using low-cost dissolved acetylene as the carbon source of the SiC film and reduce the number of cylinders to be consumed to improve the work efficiency, thereby improving the manufacturing efficiency and the manufacturing cost. It is to provide a method of manufacturing the SiC film.
本発明の更に他の目的は薄膜生成用反応室へ導入される
アセチレンガスの流量を正確且つ精密に制御し、これに
よってSiC半導体特性を高めることができたSiC膜の製法
を提供することにある。Still another object of the present invention is to provide a method for producing a SiC film capable of accurately and precisely controlling the flow rate of acetylene gas introduced into a thin film forming reaction chamber, thereby improving the SiC semiconductor characteristics. .
本発明によれば、溶解アセチレンを出発原料にして得ら
れたアセチレンガス及びケイ素含有ガスから薄膜生成手
段によって基体上にSiCを生成するSiC膜の製法が提供さ
れる。According to the present invention, there is provided a method for producing a SiC film in which SiC is produced on a substrate by a thin film producing means from an acetylene gas and a silicon-containing gas obtained by using dissolved acetylene as a starting material.
以下、本発明を、ドラム状基体の周面にグロー放電分解
法によってa-SiC膜を形成し、これによって電子写真感
光体ドラムを製作する場合を例にとって第１図により詳
細に説明する。Hereinafter, the present invention will be described in detail with reference to FIG. 1 by taking as an example a case where an a-SiC film is formed on the peripheral surface of a drum-shaped substrate by a glow discharge decomposition method to manufacture an electrophotographic photosensitive drum.
図中、１は溶解アセチレンボンベ、２はシランボンベ
（純度100％のシランガスが充填されている）であり、
3,4はそれぞれ元バルブ、5,6はそれぞれの圧力調整器、
７は純化器、8,9はアセチレンガス及びシランガスのそ
れぞれを所定の流量でもって反応室10へ供給するための
マスフローコントローラであり、反応室10の内部には成
膜用ドラム基体11が基体支持台12の上に載置されてい
る。尚、13,14,15,16はそれぞれガス配管である。In the figure, 1 is a molten acetylene cylinder, 2 is a silane cylinder (filled with 100% pure silane gas),
3, 4 are the original valves, 5 and 6 are the respective pressure regulators,
Reference numeral 7 is a purifier, and 8 and 9 are mass flow controllers for supplying acetylene gas and silane gas to the reaction chamber 10 at predetermined flow rates. Inside the reaction chamber 10, a film-forming drum substrate 11 supports the substrate. It is mounted on the table 12. In addition, 13, 14, 15, and 16 are gas pipes, respectively.
溶解アセチレンボンベ１は鉄製の容器に木炭・アスベス
ト混合物、硅酸カルシュウムなどの多孔質物（これはマ
スと呼ばれている）を均一に詰め、或いは固型化したも
のにアセトン（又はDMF・・・デメチルホルムアマイ
ド）等の溶剤をマスの多孔度に応じて適量浸潤させ、更
に精製乾燥させたアセチレンガスが充填されたものであ
る。Dissolved acetylene cylinder 1 is an iron container in which a charcoal / asbestos mixture, porous material such as calcium silicate (this is called mass) is uniformly packed, or solidified into acetone (or DMF ... A solvent such as demethylformamide) is infiltrated in an appropriate amount in accordance with the porosity of the mass, and further purified and dried, and then filled with acetylene gas.
このように溶解アセチレンボンベ１の内部には不安定な
アセチレンが燃焼分解しないようにマスと溶剤が充填さ
れており、マスは容器内部を無数の微少空間に細分し、
たとえ一部に燃焼分解を起こしても速やかに分解生成物
を吸収し、分解が容器全般に伝播波及することを防止し
ており、一方、溶剤は分解熱を吸収したり、或いは分解
防止の安定剤としての作用も成している。Thus, the melted acetylene cylinder 1 is filled with a mass and a solvent so that unstable acetylene does not burn and decompose. The mass divides the inside of the container into a myriad of minute spaces,
Even if a part of the material undergoes combustion decomposition, it quickly absorbs the decomposition products and prevents the decomposition from propagating throughout the container, while the solvent absorbs the heat of decomposition or stabilizes the decomposition prevention. It also acts as an agent.
以上の如く、溶解アセチレンの安定性はマスと溶剤との
両者の完全な作用で安全が支えられている。As described above, the stability of dissolved acetylene is supported by the complete action of both the mass and the solvent.
この溶解アセチレンボンベ１の充填圧（一次圧）は約10
Kg/cm2であり、元バルブ３を開放するとアセチレンガス
と共に溶剤も気化し、この溶剤混入ガスが圧力調整器５
によって0.5〜2.0Kg/cm2に設定され、ガス配管13を介し
て純化器７に通される。The filling pressure (primary pressure) of this melting acetylene cylinder 1 is about 10
It is Kg / cm 2 , and when the main valve 3 is opened, the solvent is vaporized together with the acetylene gas, and the gas mixed with the solvent is the pressure regulator 5
Is set to 0.5 to 2.0 Kg / cm 2 and passed through the gas pipe 13 to the purifier 7.
この純度器７は上記溶剤混入ガス中のアセトンやDMFを
除外し、高純度のアセチレンに精製するものであり、本
例の電子写真感光体を製作するに当たってシックスナイ
ンの高純度アセチレンガスが得られることを確認した。This purifier 7 excludes acetone and DMF in the gas mixed with the solvent, and purifies it to high-purity acetylene. When manufacturing the electrophotographic photoreceptor of this example, high-purity acetylene gas of Six Nine can be obtained. It was confirmed.
このようにして得られたアセチレンガスは、ガス配管14
を介してマスフローコントローラ８に通じており、そし
て、このマスフローコントローラ８に加わるガスの圧力
（二次圧）は0.5〜2Kgの範囲内で一定値に設定され、こ
れにより、マスフローコントローラ８によってアセチレ
ンガスの流量を精密に制御することができる。The acetylene gas obtained in this way is fed to the gas pipe 14
Through the mass flow controller 8 and the pressure (secondary pressure) of the gas applied to the mass flow controller 8 is set to a constant value within the range of 0.5 to 2 Kg, whereby the mass flow controller 8 causes the acetylene gas to flow. The flow rate can be precisely controlled.
一方、元バルブ４を開放してシランガスボンベ２により
シランガスを放出し（一次圧60Kg/cm2）、アセチレンガ
スと同様に圧力調整器６によってガス圧を0.5〜2Kg/cm2
に設定し、マスフローコントローラ９を通じてシランガ
スの流量も精密に制御できる。On the other hand, the main valve 4 is opened to release the silane gas by the silane gas cylinder 2 (primary pressure 60 Kg / cm 2 ), and the gas pressure is adjusted to 0.5 to 2 Kg / cm 2 by the pressure regulator 6 like the acetylene gas.
And the flow rate of the silane gas can be precisely controlled through the mass flow controller 9.
かくして、流量制御された上記アセチレンガス及びシラ
ンガスはガス配管16で混合されながら反応室10の内部に
導入され、反応室10に設けられたグロー放電分解手段
（図示せず）によって混合ガスが分解し、基板周面にa-
SiC膜が５〜20μm/時の成膜速度で形成される。Thus, the flow rate-controlled acetylene gas and silane gas are introduced into the reaction chamber 10 while being mixed in the gas pipe 16, and the mixed gas is decomposed by glow discharge decomposition means (not shown) provided in the reaction chamber 10. , A-
A SiC film is formed at a film formation rate of 5 to 20 μm / hour.
上記の製法によれば、溶解アセチレンボンベの充填圧が
約10Kg/cm2と大きくなっており、そのために通常用いら
れる47容積のボンベで比較した場合、高純度アセチレ
ンボンベに比べて常圧換算で100倍以上のアセチレンが
充填されている。そこで、本発明者等が約25μｍの厚み
を持つa-SiC電子写真感光体を製作した場合、この47
容積の溶解アセチレンボンベ１本当たり約300〜500本の
感光体ドラムを成膜することができ、その結果、製造効
率を著しく高めることができる。According to the above-mentioned manufacturing method, the filling pressure of the dissolved acetylene cylinder is as large as about 10 kg / cm 2, and when compared with the cylinder of 47 volume normally used for that, it is converted to atmospheric pressure in comparison with the high-purity acetylene cylinder. It is filled with 100 times more acetylene. Therefore, when the present inventors manufacture an a-SiC electrophotographic photoreceptor having a thickness of about 25 μm,
About 300 to 500 photoconductor drums can be formed per one volume of dissolved acetylene cylinder, and as a result, the production efficiency can be remarkably increased.
尚、本例においては純化器により高純度アセチレンに精
製したが、溶剤の成分をSiC膜に含有させる目的で純化
器を用いなくてもよい。In this example, high-purity acetylene was purified by a purifier, but the purifier may not be used for the purpose of incorporating the solvent component into the SiC film.
以上の通り、本発明のSiC膜の製法によれば、ガス溶接
或いは切断用ガスとして多用されている低コストの溶解
アセチレンを用いてもSiC膜を大きな成膜速度で形成す
ることができ、これにより、消費されるボンベの数を少
なくして作業能率を高めることができ、その結果、製造
効率及び製造コストを改善したSiC膜の製法が提供され
る。As described above, according to the method for producing a SiC film of the present invention, it is possible to form a SiC film at a large film formation rate even when using low-cost dissolved acetylene that is often used as a gas welding or cutting gas. Thus, it is possible to reduce the number of cylinders consumed and increase work efficiency, and as a result, a method for producing a SiC film with improved production efficiency and production cost is provided.
また、本発明の製法によれば、SiC半導体膜などの高純
度SiCを薄膜生成技術によって形成するに当たって、そ
れに用いられるアセチレンガスの導入ガス流量を正確且
つ精密に制御することができ、これにより、高品質なa-
SiC半導体膜を形成することができ、その結果、導電
率、分光感度、光電変換特性等々の半導体特性を所要の
レベルにまで確実に高めることができる。Further, according to the manufacturing method of the present invention, in forming high-purity SiC such as a SiC semiconductor film by a thin film forming technique, the introduced gas flow rate of the acetylene gas used for it can be accurately and precisely controlled, and thus. High quality a-
An SiC semiconductor film can be formed, and as a result, semiconductor characteristics such as conductivity, spectral sensitivity, photoelectric conversion characteristics, etc. can be reliably increased to required levels.
第１図は本発明の実施例に用いられるグロー放電分解装
置の説明図である。 １……溶解アセチレンボンベ ２……シランボンベ ３、４……元バルブ ５、６……圧力調整器 ７……純化器 ８、９……マスフローコントローラFIG. 1 is an explanatory diagram of a glow discharge decomposition apparatus used in an embodiment of the present invention. 1 ... Melting acetylene cylinder 2 ... Silane cylinder 3, 4 ... Main valve 5, 6 ... Pressure regulator 7 ... Purifier 8, 9 ... Mass flow controller
───────────────────────────────────────────────────── フロントページの続き (72)発明者 竹村 仁志 滋賀県八日市市蛇溝町長谷野1166番地の６ 京セラ株式会社滋賀八日市工場内 (72)発明者 石櫃 鴻吉 滋賀県八日市市蛇溝町長谷野1166番地の６ 京セラ株式会社滋賀八日市工場内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Hitoshi Takemura, Hitoshi Takemura, Yagami-shi, Yoka-shi, Shiga No.6, 1166, Shiga-Yokaichi Plant, Kyocera Corporation (72) Inventor, Kokichi Ishigaki Hase-no, Jamizo-cho, Yoka-shi, Shiga Prefecture 6 at 1166 Kyocera Corporation Shiga Yokaichi Factory
Claims (3)
アセチレンガス及びケイ素含有ガスから薄膜生成手段に
よって基体上にシリコンカーバイドを生成することを特
徴とするシリコンカーバイド膜の製法。1. A process for producing a silicon carbide film, which comprises producing silicon carbide on a substrate by means of a thin film producing means from acetylene gas and silicon-containing gas obtained by using dissolved acetylene as a starting material.
リコンカーバイドであることを特徴とする特許請求の範
囲第（１）項記載のシリコンカーバイド膜の製法。2. The method for producing a silicon carbide film according to claim 1, wherein the silicon carbide is amorphous silicon carbide.
純化器を介して精製されることを特徴とする特許請求の
範囲第（１）項記載のシリコンカーバイド膜の製法。3. The method for producing a silicon carbide film according to claim 1, wherein the acetylene gas is purified from dissolved acetylene through a purifier.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22775686A JPH0686659B2 (en) | 1986-09-25 | 1986-09-25 | Silicon carbide film manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP22775686A JPH0686659B2 (en) | 1986-09-25 | 1986-09-25 | Silicon carbide film manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6383272A JPS6383272A (en) | 1988-04-13 |
| JPH0686659B2 true JPH0686659B2 (en) | 1994-11-02 |
Family
ID=16865881
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP22775686A Expired - Lifetime JPH0686659B2 (en) | 1986-09-25 | 1986-09-25 | Silicon carbide film manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0686659B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI273642B (en) * | 2002-04-19 | 2007-02-11 | Ulvac Inc | Film-forming apparatus and film-forming method |
-
1986
- 1986-09-25 JP JP22775686A patent/JPH0686659B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6383272A (en) | 1988-04-13 |
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| EXPY | Cancellation because of completion of term |