JPH0638121B2 - SiC quality mirror - Google Patents
SiC quality mirrorInfo
- Publication number
- JPH0638121B2 JPH0638121B2 JP62037597A JP3759787A JPH0638121B2 JP H0638121 B2 JPH0638121 B2 JP H0638121B2 JP 62037597 A JP62037597 A JP 62037597A JP 3759787 A JP3759787 A JP 3759787A JP H0638121 B2 JPH0638121 B2 JP H0638121B2
- Authority
- JP
- Japan
- Prior art keywords
- sic
- mirror
- coating
- present
- cvd
- 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
- 239000011248 coating agent Substances 0.000 claims description 19
- 238000000576 coating method Methods 0.000 claims description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 239000013078 crystal Substances 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000001237 Raman spectrum Methods 0.000 claims description 8
- 230000005284 excitation Effects 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 5
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 description 35
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 33
- 239000000463 material Substances 0.000 description 10
- 238000000034 method Methods 0.000 description 8
- 238000005498 polishing Methods 0.000 description 8
- 238000005229 chemical vapour deposition Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- 229910003902 SiCl 4 Inorganic materials 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052575 non-oxide ceramic Inorganic materials 0.000 description 1
- 239000011225 non-oxide ceramic Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- -1 silicon halide Chemical class 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 238000004901 spalling Methods 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
Landscapes
- Optical Elements Other Than Lenses (AREA)
- Chemical Vapour Deposition (AREA)
Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明はＣＶＤによるＳｉＣ質ミラーに関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a SiC-based mirror by CVD.
［従来の技術］ 近年、高温高強度材料として、窒化珪素、炭化珪素、サ
イアロン等の非酸化物セラミックス、あるいは酸化アル
ミニウム、酸化ジルコニウム等、いわゆるニューセラミ
ックスが急速にクローズアップされ、多くの研究や開発
がなされている。[Prior Art] In recent years, as high-temperature and high-strength materials, non-oxide ceramics such as silicon nitride, silicon carbide and sialon, or so-called new ceramics such as aluminum oxide and zirconium oxide have been rapidly highlighted, and many researches and developments have been made. Has been done.
これらセラミックスのうち、炭化珪素（以下「ＳｉＣ」
と略記する。）は、 軽い材料である。Of these ceramics, silicon carbide (hereinafter "SiC")
Is abbreviated. ) Is a light material.
常温から高温まで機械的強度が高く安定している。High mechanical strength and stability from room temperature to high temperature.
熱膨張が小さく熱伝導性が良いため耐スポーリング性
に優れる。Excellent in spalling resistance due to small thermal expansion and good thermal conductivity.
耐食性が極めて大きい。Extremely high corrosion resistance.
硬度が高く、耐摩耗性に優れる。High hardness and excellent wear resistance.
導電性があり電気素子としても使用できる。などの特
徴を有し、極めて重要な工業材料として注目されてい
る。It has conductivity and can be used as an electric element. It has characteristics such as the following, and is attracting attention as an extremely important industrial material.
とりわけ、ＣＶＤ法等の気相法によって製造されるＳｉ
Ｃは、緻密で高純度であることから、これらの特性が著
しく高いため、気相法ＳｉＣ膜で被覆することにより、
各種部材の特性を改良する方法が従来より提案されてい
る。そして、例えば特開昭５９−９９４０１にはＣＶＤ
によりβ−ＳｉＣ被膜を形成したミラーが記載されてい
る。In particular, Si manufactured by a vapor phase method such as a CVD method
Since C is dense and highly pure, these characteristics are extremely high. Therefore, by coating with a vapor-phase method SiC film,
Conventionally, methods for improving the characteristics of various members have been proposed. And, for example, in JP-A-59-99401, a CVD
Describes a mirror having a β-SiC coating formed thereon.
［発明が解決しようとする問題点］ ＣＶＤによるＳｉＣ質ミラーの場合、基材表面に形成さ
れたＳｉＣ被膜を研磨仕上げしなければならないのであ
るが、従来のＳｉＣ質ミラーでは、遊離炭素を含有して
いるところから研磨しにくく、また、結晶性にも乏しい
ため、良好な反射率、散乱比を得るのが極めて困難であ
った。[Problems to be Solved by the Invention] In the case of a SiC-based mirror formed by CVD, the SiC coating formed on the surface of the base material must be polished and finished. However, the conventional SiC-based mirror does not contain free carbon. Since it is difficult to polish and the crystallinity is poor, it is extremely difficult to obtain good reflectance and scattering ratio.
［問題点を解決するための手段］ 本発明は、極めて研磨し易いＣＶＤ−ＳｉＣ質ミラーを
提供するものであって、 基材上にＣＶＤによるＳｉＣ被膜が形成された部材であ
って、アルゴンを励起源としたレーザのラマンスペクト
ルにおいて、遊離カーボンが実質的に認められず、ま
た、Ｓｉ：Ｃの比が実質的に１：１であることを特徴と
するＳｉＣ質ミラー、及び 全体がＣＶＤによるＳｉＣよりなり、該ＳｉＣはアルゴ
ンを励起源としたレーザのラマンスペクトルにおいて、
遊離カーボンが実質的に認められず、また、Ｓｉ：Ｃの
比が実質的に１：１であることを特徴とするＳｉＣ質ミ
ラー、 を要旨とするものである。[Means for Solving the Problems] The present invention provides a CVD-SiC-based mirror that is extremely easy to polish, and is a member in which a SiC coating film by CVD is formed on a base material. In the Raman spectrum of the laser used as the excitation source, substantially no free carbon was observed, and the ratio of Si: C was substantially 1: 1; In the Raman spectrum of a laser which is made of SiC, and which uses Ar as an excitation source,
It is a gist of a SiC-based mirror characterized in that substantially no free carbon is observed and the ratio of Si: C is substantially 1: 1.
［作用］ 本発明のＳｉＣ質ミラーは、遊離カーボンを含まず、Ｓ
ｉとＣが実質的に１：１の割合となっており、非常に研
磨し易く、しかも微細な結晶からなるため最終的な研磨
仕上りも極めて良好なものとなる。[Operation] The SiC mirror of the present invention does not contain free carbon and contains S
The ratio of i to C is substantially 1: 1 and it is very easy to polish, and since it is composed of fine crystals, the final polishing finish is also very good.
［実施例］ 以下に図面を参照して本発明の実施例を詳細に説明す
る。Embodiments Embodiments of the present invention will be described in detail below with reference to the drawings.
第１図は本発明の実施例に係るＳｉＣ被膜を有する部材
の部分断面図である。図示の如く、本実施例のＳｉＣ質
ミラーは、基材１上にＳｉＣ被膜２が形成された部材で
あって、アルゴンを励起源としたレーザのラマンスペク
トルにおいて、遊離カーボンが実質的に認められず、ま
た、Ｓｉ：Ｃの比が実質的に１：１であり、好ましくは
結晶粒径が１０μｍ以下のものである。FIG. 1 is a partial sectional view of a member having a SiC coating according to an embodiment of the present invention. As shown in the figure, the SiC mirror of this example is a member in which the SiC coating 2 is formed on the substrate 1, and free carbon is substantially observed in the Raman spectrum of a laser using argon as an excitation source. In addition, the ratio of Si: C is substantially 1: 1 and the crystal grain size is preferably 10 μm or less.
このように遊離カーボンを含まず、Ｓｉ：Ｃが１：１の
結晶性が高い被膜であり、かつ結晶が１０μｍ以下と微
細なため、極めて研磨が容易であり、最終的な仕上りが
良くなり、良好な反射率、散乱比が得られる。As described above, since the coating film does not contain free carbon and Si: C has a high crystallinity of 1: 1 and the crystal is as fine as 10 μm or less, it is extremely easy to polish and the final finish is improved. Good reflectance and scattering ratio can be obtained.
本発明において、基材１としては金属、セラミック、合
成樹脂等各種のものが採用できるが、黒鉛もしくは焼結
ＳｉＣが好適である。黒鉛は、非酸化性雰囲気中で極め
て高い耐熱性を有すると共に、高熱伝導率を有し、しか
も凹面鏡など複雑な形状のものも容易に作製できる。焼
結ＳｉＣは、ＳｉＣ被膜と熱膨張係数が一致もしくは近
似しているところから、得られるミラーの熱歪が小さ
い。また、高温の酸化性雰囲気でも安定である。このＳ
ｉＣ焼結体は、ホットプレスや反応焼結など各種の焼結
法によって得られる。In the present invention, various materials such as metals, ceramics, and synthetic resins can be used as the base material 1, but graphite or sintered SiC is preferable. Graphite has extremely high heat resistance in a non-oxidizing atmosphere, high thermal conductivity, and a complex shape such as a concave mirror can be easily manufactured. Since the coefficient of thermal expansion of sintered SiC is the same as or close to that of the SiC coating, the resulting strain of the mirror is small. It is also stable in a high temperature oxidizing atmosphere. This S
The iC sintered body can be obtained by various sintering methods such as hot pressing and reaction sintering.
また、この基材１上に上記のＳｉＣ被膜を形成するに
は、ＣＶＤ法によって容易に形成することができる。Moreover, in order to form the above-mentioned SiC film on this base material 1, it can be easily formed by a CVD method.
このＣＶＤ法の基本反応は良く知られてるところであ
り、例えばＳｉＣｌ４等のハロゲン化珪素とＣ３Ｈ８等
の炭化水素とをＨ２をキャリアガスとして流し、ＳｉＣ
を析出させるものである。The basic reaction of this CVD method is well known, and for example, a silicon halide such as SiCl 4 and a hydrocarbon such as C 3 H 8 are passed through H 2 as a carrier gas to obtain SiC.
Is deposited.
なお、本発明では珪素原料ガス及び炭素原子ガスとし
て、上記以外の各種のものを用い得る。In the present invention, various kinds of silicon source gas and carbon atom gas other than the above may be used.
上記実施例は基材上にＳｉＣ被膜を形成したミラーに関
するが、本発明では基材に相当する部分もすべてＣＶＤ
によって作成したものであっても良い。この場合、ＣＶ
Ｄ処理時間は、被膜のみをＣＶＤ法により形成したミラ
ーに比べ長くはなるものの、基材相当部分からミラー面
にかけて均一相となるため、熱歪が無く、温度変化の激
しい高温酸化性雰囲気でも極めて安定したものとなる。
さらに、焼結体固有の欠陥が無く、極めて高強度であ
る。Although the above examples relate to a mirror having a SiC film formed on a base material, in the present invention, all portions corresponding to the base material are formed by CVD.
It may be created by. In this case, CV
Although the D treatment time is longer than that of the mirror in which only the coating is formed by the CVD method, it has a uniform phase from the portion corresponding to the base material to the mirror surface, so that there is no thermal strain and it is extremely high even in a high temperature oxidizing atmosphere where the temperature changes drastically. It will be stable.
Furthermore, there is no defect peculiar to the sintered body, and the strength is extremely high.
本発明において、ＣＶＤによるＳｉＣは、その結晶粒径
が１０μｍ以下であるものが好適である。即ち、従来、
ＳｉＣ質ミラーにおいては結晶粒径が大きい程ＳｉＣの
結晶性が良く、反射率が向上するものと考えられていた
（例えば特開昭５９−９９４０１号第２頁左上欄）。し
かしながら、本発明の如くＳｉとＣとの比が実質的に
１：１である場合においては、ＳｉＣの結晶性が高く、
かつ研磨し易いところから反射率、散乱比を容易に向上
させることができる。しかも、結晶粒径が小さいと、加
工時の最小単位が小さく、そのため緻密な面が得やす
く、また、強度、熱衝撃特性が向上し、繰り返し高温下
におかれても熱歪が殆ど発生しないという優れた効果が
得られる。In the present invention, the SiC by CVD preferably has a crystal grain size of 10 μm or less. That is, conventionally
It has been considered that in a SiC mirror, the larger the crystal grain size, the better the crystallinity of SiC and the higher the reflectance (for example, JP-A-59-99401, page 2, upper left column). However, when the ratio of Si to C is substantially 1: 1 as in the present invention, the crystallinity of SiC is high,
In addition, the reflectance and the scattering ratio can be easily improved because it is easy to polish. Moreover, if the crystal grain size is small, the minimum unit during processing is small, so a dense surface can be easily obtained, and the strength and thermal shock properties are improved, and thermal strain hardly occurs even when repeatedly subjected to high temperatures. That is an excellent effect.
このＳｉＣ質ミラーを研磨する方法は特に限定されるも
のではなく、ホーニング、超仕上げ、研磨布加工、ラッ
ピング、ポリシング、バレル加工、超音波加工、ＥＥＭ
（エラスティックエミッションマシニング）、メカノケ
ミカルカルポリシング、フロートポリシングなど各種の
方法が採用できる。The method for polishing the SiC mirror is not particularly limited, and honing, superfinishing, polishing cloth processing, lapping, polishing, barrel processing, ultrasonic processing, EEM.
Various methods such as (elastic emission machining), mechanochemical polishing and float polishing can be adopted.
以下、具体例について説明する。Hereinafter, a specific example will be described.
本発明例として、凹面鏡形状の炭素製基材に、温度：１
５００℃、原料ガス：ＳｉＣｌ４及びＣ３Ｈ８、キャリ
アガス：Ｈ２、ガス流量：０．７／ｍｉｎなる条件の
下でＳｉＣ被膜を形成した。被膜表面のＳＥＭ観察の結
果、結晶粒径は３μｍであることが認められた。As an example of the present invention, a concave mirror-shaped carbon substrate is used, and the temperature:
A SiC film was formed under the conditions of 500 ° C., source gas: SiCl 4 and C 3 H 8 , carrier gas: H 2 , and gas flow rate: 0.7 / min. As a result of SEM observation of the coating surface, it was confirmed that the crystal grain size was 3 μm.
この被膜のアルゴンを励起源としたレーザのラマンスペ
クトルは第２図の通りであり、Ｓｉ：Ｃ比は実質的に
１：１である。The Raman spectrum of a laser using argon as an excitation source for this coating is as shown in FIG. 2, and the Si: C ratio is substantially 1: 1.
この被膜を回転研磨法で研磨したところ、反射率が９５
％以上、散乱の信号と雑音の強度比が１００００以上と
なった。When this coating was polished by the rotary polishing method, the reflectance was 95.
%, The intensity ratio of scattered signal and noise was 10,000 or more.
比較例として、第３図にラマンスペクトルを示すような
被膜を形成した。この比較例の被膜には多量の遊離カー
ボンが認められた。As a comparative example, a film having a Raman spectrum shown in FIG. 3 was formed. A large amount of free carbon was recognized in the coating of this comparative example.
この被膜を、上記本発明例と同様に研磨したところ、反
射率は９０％、散乱の信号と雑音の強度比は１０００以
下に過ぎなかった。また、結晶粒径は１５μｍであっ
た。When this coating was polished in the same manner as in the above-mentioned examples of the present invention, the reflectance was 90% and the intensity ratio of the scattered signal to the noise was only 1000 or less. The crystal grain size was 15 μm.
このように、本発明の部材は、極めて研磨し易い被膜を
有することが認められた。As described above, it was confirmed that the member of the present invention had a coating film that was extremely easy to polish.
また、上記本発明例と同一条件にて基材相当部分をもＣ
ＶＤ法によるＳｉＣ製としたミラーを製造した。そし
て、その表面を研磨したところ同一研磨時間にて上記本
発明例と同等の反射特性となった。In addition, under the same conditions as in the above-mentioned example of the present invention, a portion corresponding to the substrate is
A mirror made of SiC was manufactured by the VD method. When the surface was polished, the reflection characteristics were the same as those of the above-mentioned examples of the present invention in the same polishing time.
［発明の効果］ 以上詳述した通り、本発明のＳｉＣ質ミラーは、極めて
研磨し易く、良好な反射率、散乱比が得られる。また、
表面はＳｉＣ層であるため、ＳｉＣの優れた耐食性、耐
摩耗性を有する。[Advantages of the Invention] As described in detail above, the SiC mirror of the present invention is extremely easy to polish, and has good reflectance and scattering ratio. Also,
Since the surface is a SiC layer, it has excellent corrosion resistance and wear resistance of SiC.
第１図は本発明のＳｉＣ質ミラーの部分断面図、第２図
及び第３図はＳｉＣ被膜のラマンスペクトルである。 １…基材、２…被膜。FIG. 1 is a partial sectional view of the SiC mirror of the present invention, and FIGS. 2 and 3 are Raman spectra of the SiC coating. 1 ... Substrate, 2 ... Coating.
Claims (3)
れた部材であって、アルゴンを励起源としたレーザのラ
マンスペクトルにおいて遊離カーボンが実質的に認めら
れず、また、Ｓｉ：Ｃの比が実質的に１：１であること
を特徴とするＳｉＣ質ミラー。1. A member having a SiC coating formed by CVD on a substrate, wherein free carbon is not substantially observed in the Raman spectrum of a laser using argon as an excitation source, and the ratio of Si: C. Is a substantially 1: 1 SiC-based mirror.
であることを特徴とする特許請求の範囲第１項に記載の
ミラー。2. The mirror according to claim 1, wherein the SiC coating has a crystal grain size of 10 μm or less.
ｉＣはアルゴンを励起源としたレーザのラマンスペクト
ルにおいて、遊離カーボンが実質的に認められず、ま
た、Ｓｉ：Ｃの比が実質的に１：１であることを特徴と
するＳｉＣ質ミラー。3. The whole is made of SiC by CVD, and the S
iC is a SiC-based mirror characterized by having substantially no free carbon in the Raman spectrum of a laser using argon as an excitation source, and having a Si: C ratio of substantially 1: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62037597A JPH0638121B2 (en) | 1987-02-20 | 1987-02-20 | SiC quality mirror |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62037597A JPH0638121B2 (en) | 1987-02-20 | 1987-02-20 | SiC quality mirror |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63205603A JPS63205603A (en) | 1988-08-25 |
| JPH0638121B2 true JPH0638121B2 (en) | 1994-05-18 |
Family
ID=12501973
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62037597A Expired - Lifetime JPH0638121B2 (en) | 1987-02-20 | 1987-02-20 | SiC quality mirror |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0638121B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002037669A (en) * | 2000-07-28 | 2002-02-06 | Kyocera Corp | Silicon carbide material, plasma resistant member and semiconductor manufacturing equipment |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6036315A (en) * | 1983-08-10 | 1985-02-25 | Toray Ind Inc | Carbon fiber structure and secondary battery using it |
| JPS6236089A (en) * | 1985-08-09 | 1987-02-17 | 東芝セラミツクス株式会社 | Manufacture of ceramic product |
| JPS62241124A (en) * | 1986-04-11 | 1987-10-21 | Matsushita Electric Ind Co Ltd | magnetic recording medium |
-
1987
- 1987-02-20 JP JP62037597A patent/JPH0638121B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63205603A (en) | 1988-08-25 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |