JPS6220156B2 - - Google Patents
Info
- Publication number
- JPS6220156B2 JPS6220156B2 JP15987177A JP15987177A JPS6220156B2 JP S6220156 B2 JPS6220156 B2 JP S6220156B2 JP 15987177 A JP15987177 A JP 15987177A JP 15987177 A JP15987177 A JP 15987177A JP S6220156 B2 JPS6220156 B2 JP S6220156B2
- Authority
- JP
- Japan
- Prior art keywords
- sio
- furnace
- carbon
- sic
- chamber
- 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
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 25
- 229910052799 carbon Inorganic materials 0.000 claims description 21
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 238000010438 heat treatment Methods 0.000 claims description 18
- 239000000758 substrate Substances 0.000 claims description 17
- 238000005192 partition Methods 0.000 claims description 8
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 5
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 27
- 229910010271 silicon carbide Inorganic materials 0.000 description 27
- 239000007789 gas Substances 0.000 description 23
- 239000000463 material Substances 0.000 description 14
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000000377 silicon dioxide Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Chemical Vapour Deposition (AREA)
Description
【発明の詳細な説明】
本発明はSiCコーテイング用加熱炉の改良に関
するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an improvement in a heating furnace for SiC coating.
従来、被処理基材表面にSiCをコーテイングす
る方法としては、(1)外部からC源とSi源とからな
る原料ガスを導入し、常圧下で加熱せしめて被処
理基材表面にSiC層を形成する方法、(2)被処理基
材が炭素の場合、外部からSi源のみからなる原料
ガスを導入し、常圧下で加熱して基材のCとSiと
を直接反応させてSiC層を形成する方法、等が採
用されている。 Conventionally, the method of coating SiC on the surface of a substrate to be treated is as follows: (1) A raw material gas consisting of a C source and a Si source is introduced from the outside and heated under normal pressure to form a SiC layer on the surface of the substrate to be treated. (2) When the substrate to be treated is carbon, a raw material gas consisting only of a Si source is introduced from the outside and heated under normal pressure to directly react the C and Si of the substrate to form a SiC layer. The method of forming the material is adopted.
しかしながら、上記(1)の方法にあつては、被処
理基材へのSiC膜のくい込みが少なく、均一、均
質なSiC膜を形成できないため、使用中にSiC膜
の剥離、クラツク等が生じる欠点がある。また、
この方法に用いるSi源は比較的低温で気化する必
要があるため、一般に高価なハロゲン珪素を用い
なければならない。 However, in the case of method (1) above, the SiC film does not penetrate into the substrate to be treated, and a uniform and homogeneous SiC film cannot be formed, so the disadvantage is that the SiC film may peel off or crack during use. There is. Also,
Since the Si source used in this method needs to be vaporized at a relatively low temperature, expensive halogen silicon must generally be used.
一方、上記(2)の方法は被処理基材(カーボン基
材)にSiを直接反応させるため強固なSiC膜を形
成できるが、そのSiC膜の厚さが制限され、使用
範囲が限られる。また、形成されるSiC膜の性状
はカーボン基材の組織、特性に大きく左右され、
緻密なSiC膜を形成するには使用するカーボン基
材を厳格に精選しなければならず、コストの高騰
化を招く。 On the other hand, in the method (2) above, a strong SiC film can be formed because Si is directly reacted with the substrate to be treated (carbon substrate), but the thickness of the SiC film is limited and the range of use is limited. In addition, the properties of the SiC film formed are greatly influenced by the structure and characteristics of the carbon base material.
In order to form a dense SiC film, the carbon base material used must be carefully selected, leading to an increase in costs.
本発明は上記欠点を解消するためになされたも
ので、高価なSi源を用いず、かつ被処理基材を精
選することなく、被処理基材に密着性が良好で、
緻密性、均一性、均質性の優れたSiC膜を形成し
得るSiCコーテイング用加熱炉を提供しようとす
るものである。 The present invention was made in order to eliminate the above-mentioned drawbacks, and it is possible to achieve good adhesion to the substrate to be treated without using an expensive Si source and without carefully selecting the substrate to be treated.
The present invention aims to provide a heating furnace for SiC coating that can form a SiC film with excellent density, uniformity, and homogeneity.
以下、本発明の一実施例を図面を参照して説明
する。 Hereinafter, one embodiment of the present invention will be described with reference to the drawings.
図中1は円筒状の炉本体で、この炉内には該炉
内を上下に区画する仕切板2が介装され、この仕
切板2によつて上部に反応室3、下部にSiO含有
ガスの生成室4が形成されている。この仕切板2
には前記各室3,4の連通路を形成するように多
数の連通孔5…5が設けられている。そして、上
記反応室3内には円筒状の黒鉛発熱体6が配設さ
れ、この発熱体6と被処理基材としての炭素基材
16の間に内部構造体としての炭素製板状体7
a,7bを設置している。一方、上記SiO生成室
4内にはSiO含有ガス生成原料としての珪石など
のシリカと炭素とを収容するたとえば黒鉛製の容
器8が設置されており、この容器8の外周囲には
コイル状発熱体が巻装されている。 In the figure, 1 is a cylindrical furnace body, and a partition plate 2 is interposed in this furnace to divide the inside of the furnace into upper and lower parts. A generation chamber 4 is formed. This partition plate 2
A large number of communication holes 5...5 are provided in the chambers 3 and 4 to form communication paths between the chambers 3 and 4. A cylindrical graphite heating element 6 is disposed in the reaction chamber 3, and a carbon plate 7 as an internal structure is disposed between this heating element 6 and a carbon base material 16 as a substrate to be treated.
A and 7b are installed. On the other hand, a container 8 made of graphite, for example, that accommodates silica such as silica stone and carbon as a raw material for generating a SiO-containing gas is installed in the SiO generation chamber 4, and a coil-shaped heat generating The body is wrapped.
なお、この容器8は炉本体1の下部側壁に設け
られた開閉蓋(図示せず)から出し入れされるよ
うになつている。 The container 8 is adapted to be taken in and taken out through an opening/closing lid (not shown) provided on the lower side wall of the furnace body 1.
また、上記炉本体1の上端にはフランジ10が
設けられており、このフランジ10に水冷蓋11
をシリコンゴム製のOリング12を介して気密に
固定している。この水冷蓋11には上記反応室3
と連通するように排気管13が挿着されており、
かつ該排気管13には前記反応室3内のガスを排
気して減圧にする減圧装置、たとえば真空ポンプ
14が介装されている。なお、図中の15は炉本
体1を保護するためにその内壁面に設けられた遮
蔽体である。 Further, a flange 10 is provided at the upper end of the furnace body 1, and a water cooling lid 11 is attached to this flange 10.
are airtightly fixed via an O-ring 12 made of silicone rubber. This water-cooled lid 11 has the reaction chamber 3
An exhaust pipe 13 is inserted so as to communicate with the
Further, the exhaust pipe 13 is provided with a pressure reducing device, for example, a vacuum pump 14, which exhausts the gas in the reaction chamber 3 to reduce the pressure. Note that 15 in the figure is a shield provided on the inner wall surface of the furnace body 1 to protect it.
次に、上述した構造のSiCコーテイング用加熱
炉の作用を説明する。 Next, the operation of the SiC coating heating furnace having the above-described structure will be explained.
まず、炉内の反応室3に被処理基材としての炭
素基材16を装填し、SiO含有ガスの生成室4に
設置された珪石粉17、炭素粉18を収容した容
器8の外周囲に設けられたコイル状発熱体9に通
電すると、次のような反応が主として起こり、
SiO含有ガスが生成される。 First, a carbon substrate 16 as a substrate to be treated is loaded into the reaction chamber 3 in the furnace, and the outer periphery of the container 8 containing the silica powder 17 and carbon powder 18 installed in the SiO-containing gas generation chamber 4 is heated. When electricity is applied to the provided coil-shaped heating element 9, the following reactions mainly occur.
SiO-containing gas is produced.
SiO2+C→SiO+CO
こうしてSiO含有ガスを生成させると共に、反
応室3の筒状黒鉛発熱体6に通電し、同時に真空
ポンプ14を作動させると、詳細な現象は説明で
きないがおそらく次のような現象が起つているも
のと推察される。すなわち生成室4から矢印に示
す如く反応室3内に流入したSiO含有ガスは高温
度に加熱された反応室3の内部構造体としての炭
素製板状体7a,7bと反応してSiガス、COガ
ス等が生成される。この生成過程において、反応
室3内の炭素基材16にSiガスが直接反応した
り、該炭素基材16の表面付近でSiガスとCOガ
スとが反応して、該基材16表面にSiC膜が形成
される。上記板状体はSiO含有ガス等から加熱器
を保護する役目も果し、加熱器がSiO含有ガス等
と反応して酸化消耗する事を防止すると共に、加
熱器表面にSiC膜が形成されることによつて起こ
る反応室内の温度ムラを抑制し、反応室内を均一
温度下に保つことができ均一なSiC膜が形成でき
る。しかも本発明の加熱炉を使用して製造した
SiC形成物は上記生成ガスの反応過程において、
反応室3内が真空ポンプ14の排気作用により減
圧化され、生成ガスの反応物が炭素基材16表面
に一度に多量析出せず、徐々に析出するため、炭
素基材16表面に緻密で均質、均一のSiC膜を形
成できると共に、炭素基材に対するSiC膜の密着
性を向上できる。 SiO 2 +C→SiO+CO In this way, SiO-containing gas is generated, and if the cylindrical graphite heating element 6 in the reaction chamber 3 is energized and the vacuum pump 14 is operated at the same time, the detailed phenomenon cannot be explained, but it is probably as follows. It is assumed that this is occurring. That is, the SiO-containing gas flowing into the reaction chamber 3 from the generation chamber 4 as shown by the arrow reacts with the carbon plates 7a and 7b serving as the internal structure of the reaction chamber 3 heated to a high temperature, thereby producing Si gas, CO gas etc. are generated. In this generation process, Si gas reacts directly with the carbon base material 16 in the reaction chamber 3, or Si gas and CO gas react near the surface of the carbon base material 16, resulting in the formation of SiC on the surface of the base material 16. A film is formed. The plate-shaped body also serves to protect the heater from SiO-containing gas, etc., and prevents the heater from reacting with SiO-containing gas and being consumed by oxidation, and also forms a SiC film on the heater surface. This suppresses the temperature unevenness within the reaction chamber that occurs due to this, and allows the inside of the reaction chamber to be kept at a uniform temperature, making it possible to form a uniform SiC film. Moreover, it was manufactured using the heating furnace of the present invention.
In the reaction process of the above-mentioned generated gas, the SiC formation is
The inside of the reaction chamber 3 is depressurized by the evacuation action of the vacuum pump 14, and the reactants of the generated gas do not precipitate in large quantities on the surface of the carbon base material 16 at once, but gradually, so that they are dense and homogeneous on the surface of the carbon base material 16. , a uniform SiC film can be formed, and the adhesion of the SiC film to the carbon substrate can be improved.
なお、本発明の加熱炉における板状体は上記実
施例の如き炭素材料に限定されず、炭化珪素材料
にしてもよい。この場合、詳細な説明はできない
が、炭素製の場合と同様に、生成室4から矢印に
示す如く反応室3内に流入したSiO含有ガスは高
温度に加熱された炭化珪素製板状体と反応し、Si
ガス、COガス等が生成される。この様に生成さ
れたSi源、C源のガスが炭素基材16と直接反応
したり、基材表面付近でSiガスとCOガスが反応
したりして炭素基材の表面にSiC膜が形成され
る。 Note that the plate-shaped body in the heating furnace of the present invention is not limited to the carbon material as in the above embodiments, but may be made of a silicon carbide material. In this case, although a detailed explanation cannot be given, as in the case of carbon, the SiO-containing gas flowing from the generation chamber 4 into the reaction chamber 3 as shown by the arrow is a silicon carbide plate heated to a high temperature. reacts, Si
Gas, CO gas, etc. are generated. The Si source and C source gases generated in this way react directly with the carbon base material 16, or Si gas and CO gas react near the base material surface, forming a SiC film on the surface of the carbon base material. be done.
また、上記板状体の形状は板状のものを組合せ
たもの、または円筒状のもの等適宜形状にするこ
とは可能である。 Further, the shape of the plate-like body may be a combination of plate-like bodies, a cylindrical body, or any other suitable shape.
本発明の加熱炉における仕切板は、反応室及び
SiO含有ガス生成室を区画するものであればよ
く、その形状は特に板状である必要はなく、任意
の形状でよい。 The partition plate in the heating furnace of the present invention has a reaction chamber and
Any shape may be used as long as it partitions the SiO-containing gas generation chamber, and its shape does not need to be particularly plate-like, and may be any shape.
本発明の加熱炉における加熱器は上記実施例の
如く反応室と生成室とに別々設けずに、一体的な
もので各室の加熱を兼用してもよい。 The heater in the heating furnace of the present invention may not be provided separately for the reaction chamber and the production chamber as in the above-mentioned embodiments, but may be an integrated heater for heating each chamber.
本発明における被処理基材は上記実施例の如き
炭素材料に限らず、炭化珪素材料等から形成して
もよい。 The substrate to be treated in the present invention is not limited to the carbon material as in the above embodiments, but may be formed from a silicon carbide material or the like.
本発明の加熱炉構造はその他この発明の要旨を
逸脱しない範囲で種々変形実施できることは勿論
である。 It goes without saying that the heating furnace structure of the present invention can be modified in various other ways without departing from the gist of the present invention.
以上詳述した如く、本発明によれば、シリカと
炭素からなる極めて安価な原料より被処理基材に
密着性が良好で、緻密性、均一性、均質性の優れ
たSiC膜を形成し得る極めて実用価値の高いSiC
コーテイング用加熱炉を提供できるものである。 As detailed above, according to the present invention, it is possible to form a SiC film that has good adhesion to the substrate to be processed and has excellent density, uniformity, and homogeneity using extremely inexpensive raw materials made of silica and carbon. SiC with extremely high practical value
A heating furnace for coating can be provided.
図は本発明の一実施例を示すSiCコーテイング
用加熱炉の断面図である。
1……炉本体、2……仕切板、3……反応室、
4……生成室、6……黒鉛発熱体、7a,7b…
…炭素製板状体(内部構造体)、8……容器、9
……コイル状発熱体、16……被処理基材。
The figure is a sectional view of a heating furnace for SiC coating showing one embodiment of the present invention. 1... Furnace body, 2... Partition plate, 3... Reaction chamber,
4... Generation chamber, 6... Graphite heating element, 7a, 7b...
... Carbon plate-shaped body (internal structure), 8 ... Container, 9
... Coiled heating element, 16 ... Substrate to be treated.
Claims (1)
れ一部又は全部が炭素もしくはSiCからなる少く
とも仕切板と板状体から構成される内部構造体よ
りなり、前記仕切板が反応室とSiO含有ガスの生
成室とに炉内を区画すると共に各室の連通路を形
成するように介装され、前記SiO生成室にSiO含
有ガス生成原料の収納容器が設置され、前記反応
室及びSiO生成室を加熱するように設けられた加
熱器と前記反応室内を減圧にする減圧装置とを具
備し、少なくとも被処理基材と前記加熱器との間
に前記板状体を設けたことを特徴とするSiCコー
テイング用加熱炉。1 Consisting of a furnace body forming a furnace shell, and an internal structure provided inside the furnace and consisting of at least a partition plate and a plate-like body, the part or whole of which is made of carbon or SiC, and the partition plate is a reaction chamber. and a SiO-containing gas generation chamber are interposed to partition the inside of the furnace and form a communication path between each chamber, and a storage container for a SiO-containing gas generation raw material is installed in the SiO generation chamber, and A heater provided to heat the SiO generation chamber and a pressure reducing device for reducing the pressure in the reaction chamber are provided, and the plate-shaped body is provided between at least the substrate to be treated and the heater. Characteristic heating furnace for SiC coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15987177A JPS5490216A (en) | 1977-12-27 | 1977-12-27 | Heating furnace for sic coating process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15987177A JPS5490216A (en) | 1977-12-27 | 1977-12-27 | Heating furnace for sic coating process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5490216A JPS5490216A (en) | 1979-07-17 |
| JPS6220156B2 true JPS6220156B2 (en) | 1987-05-06 |
Family
ID=15703019
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15987177A Granted JPS5490216A (en) | 1977-12-27 | 1977-12-27 | Heating furnace for sic coating process |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5490216A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0633951B2 (en) * | 1986-07-15 | 1994-05-02 | イビデン株式会社 | High temperature heating furnace |
| US5116679A (en) * | 1988-07-29 | 1992-05-26 | Alcan International Limited | Process for producing fibres composed of or coated with carbides or nitrides |
| CN102473516B (en) * | 2009-07-10 | 2015-09-09 | 日立金属株式会社 | The manufacture method of R-Fe-B rare-earth sintering magnet and vapour control parts |
| JP5737547B2 (en) * | 2009-09-04 | 2015-06-17 | 東洋炭素株式会社 | Method for producing silicon carbide-coated graphite particles and silicon carbide-coated graphite particles |
-
1977
- 1977-12-27 JP JP15987177A patent/JPS5490216A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5490216A (en) | 1979-07-17 |
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