JPS6033794B2 - sliding member - Google Patents

sliding member

Info

Publication number
JPS6033794B2
JPS6033794B2 JP13401480A JP13401480A JPS6033794B2 JP S6033794 B2 JPS6033794 B2 JP S6033794B2 JP 13401480 A JP13401480 A JP 13401480A JP 13401480 A JP13401480 A JP 13401480A JP S6033794 B2 JPS6033794 B2 JP S6033794B2
Authority
JP
Japan
Prior art keywords
silicon carbide
coating layer
sliding member
alumina
base
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
JP13401480A
Other languages
Japanese (ja)
Other versions
JPS5757873A (en
Inventor
三郎 田畑
安博 阿久根
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.)
Nippon Pillar Packing Co Ltd
National Institute of Advanced Industrial Science and Technology AIST
Original Assignee
Agency of Industrial Science and Technology
Nippon Pillar Packing Co Ltd
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 Agency of Industrial Science and Technology, Nippon Pillar Packing Co Ltd filed Critical Agency of Industrial Science and Technology
Priority to JP13401480A priority Critical patent/JPS6033794B2/en
Publication of JPS5757873A publication Critical patent/JPS5757873A/en
Publication of JPS6033794B2 publication Critical patent/JPS6033794B2/en
Expired legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23CCOATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/024Deposition of sublayers, e.g. to promote adhesion of the coating
    • C23C14/025Metallic sublayers

Landscapes

  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Sliding-Contact Bearings (AREA)

Description

【発明の詳細な説明】 本発明は、基体の表面部に、炭化ケイ素を物理蒸着によ
って被覆させた摺動部材に関するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a sliding member in which the surface of a base is coated with silicon carbide by physical vapor deposition.

従来、メカニカルシール、軸受、タービン、ポンプ部品
等の機械産業分野に供せられ、摺動する部分に用いられ
る摺動部村として、カーボン基体上に直接炭化ケイ素の
皮膜を形成せしめたものがある。
Conventionally, there are sliding parts used in mechanical industry fields such as mechanical seals, bearings, turbines, pump parts, etc., where a silicon carbide film is directly formed on a carbon substrate. .

しかしながら基体はカーボンを用いているため、皮膜で
ある炭化ケイ素に比して機械的強度(特にヤング率)が
小さいので、過酷な条件下において使用するとき、カー
ボン基体に歪等の不都合を生じる。このため皮膜として
形成された炭化ケイ素の皮膜を形成せしめたものが摺動
部村として広く産業用途に供せられようとするとき、負
荷条件等の適用範囲面から目づと制約される実状があっ
た。また近年、カーボン素材の価格アップにより、安価
な摺動部材を産業市場へ供することを鑑みると不適切に
なりつつある。そこで、発明者らは、価格安なアルミナ
(Aそ203)を基体として用いることに着目し、アル
ミナ基体上に炭化ケイ素を被覆する事により、機械的強
度の高い、価格安な炭化ケイ素複合体からなる摺動部材
が期待できる。しかし従釆の化学蒸着法では、蒸着温度
が高い事、およびキャリャ−ガスである水素の還元作用
によるアルミナ基体組織の破壊等により炭化ケイ素を被
覆することは技術的に困難であった。本発明は、係る事
情に鑑みなされたもので、アルミナ基体と炭化ケイ素被
覆層とが非常に強固に接合された構成となり、炭化ケイ
素被覆層に内部応力が生じなく、しかも優れた摺動特性
を有する摺動部材を提供しようとするものである。以下
に、本発明を詳細に説明する。アルミナ基体上に炭化ケ
イ素被覆層を形成せしめるにあたって、この異質な材料
どうしを接合するには熱風彰張差によって生じる欠陥を
出来るだけなくせる構成としなければならずまた内部応
力の生じない構成としなければらない。
However, since the base is made of carbon, its mechanical strength (particularly Young's modulus) is lower than that of silicon carbide, which is the coating, so when used under harsh conditions, the carbon base may suffer from distortion or other disadvantages. For this reason, when a silicon carbide film formed as a film is intended to be widely used in industrial applications as a sliding part, the actual situation is that it is severely restricted in terms of the scope of application such as load conditions. there were. Furthermore, in recent years, due to the rise in the price of carbon materials, it has become inappropriate to provide inexpensive sliding members to the industrial market. Therefore, the inventors focused on using cheap alumina (Aso 203) as a base, and by coating silicon carbide on the alumina base, they created a cheap silicon carbide composite with high mechanical strength. A sliding member consisting of the following can be expected. However, with the conventional chemical vapor deposition method, it is technically difficult to coat silicon carbide due to the high deposition temperature and the destruction of the alumina substrate structure due to the reducing action of hydrogen, which is a carrier gas. The present invention has been developed in view of the above circumstances, and has a structure in which the alumina base and the silicon carbide coating layer are extremely firmly bonded, so that no internal stress is generated in the silicon carbide coating layer, and moreover, it has excellent sliding properties. An object of the present invention is to provide a sliding member having the following features. The present invention will be explained in detail below. When forming a silicon carbide coating layer on an alumina substrate, in order to bond these dissimilar materials together, it is necessary to create a structure that can eliminate as much as possible defects caused by hot air tension differences, and a structure that does not generate internal stress. It doesn't fall apart.

このため炭化ケイ素被覆層が施こされるべきアルミナ基
体の表面部に予め金属被覆層を設ければ非常に良好であ
り、つまりァルミナ基体の表面にいわゆるメタライジン
グを施こす。このメタライズ材としては、鉄とニッケル
との合金、モリブデン、マンガン、或いはこれらの合金
等を意図するものである。特に本発明では炭化ケイ素の
結晶系が同じであるモリブデンやマンガンとモリブデン
の合金等を用いることが好ましい。そしてこのメタライ
ジングを施こしたアルミナ基体に、階動部材として好適
な炭化ケイ素被覆層をを物理蒸着によって形成したもの
である。この物理蒸着には、イオンプレーティング法、
真空蒸着法、スパッタリング法等があり、これらの物理
蒸着手段を用いても本発明に係る摺動部材を得ることは
可能かも知れないが、低温蒸着ができ、制御性の良いス
パック法が好適であり「特に蒸着速度が通常の5〜1M
音速し、マグネトロン型スパッタ法が最適である。この
スバッタ蒸着に従えば、酒動部材として必要な厚さが5
0仏m以上の炭化ケイ素被覆層をも自由に形成でき、し
かも500〜1000ooという極めて低温状態にて蒸
着できるので、炭化ケイ素被覆層に内部応力の発生や歪
を生じさせない。従って安定した繊密な炭化ケイ素被覆
層が出来る。しかもメタラィジングを施こしたアルミナ
基体上に蒸着するので、炭化ケイ素と金属がうまく接合
し、例えば、アルミナに直接炭化ケイ素を蒸着させた場
合のような剥離現象は全くなくすることができ、優れた
摺動部材が得られた。次に本発明を例示図面に基づきさ
らに説明する。
For this reason, it is very effective if a metal coating layer is previously provided on the surface of the alumina substrate on which the silicon carbide coating layer is to be applied, that is, so-called metallization is applied to the surface of the alumina substrate. This metallizing material is intended to be an alloy of iron and nickel, molybdenum, manganese, or an alloy thereof. In particular, in the present invention, it is preferable to use molybdenum, an alloy of manganese and molybdenum, etc., which have the same crystal system as silicon carbide. A silicon carbide coating layer suitable for use as a tiered member is formed on this metallized alumina base by physical vapor deposition. This physical vapor deposition method includes ion plating method,
There are vacuum evaporation methods, sputtering methods, etc., and although it may be possible to obtain the sliding member according to the present invention using these physical vapor deposition methods, the sputter method, which allows low-temperature evaporation and has good controllability, is preferable. Yes, especially when the deposition rate is 5 to 1M
Because of the speed of sound, magnetron sputtering is the most suitable method. According to this sputter deposition, the thickness required for the driving member is 5.
A silicon carbide coating layer with a thickness of 0 mm or more can be freely formed, and can be deposited at an extremely low temperature of 500 to 1000 oo, so that no internal stress or distortion occurs in the silicon carbide coating layer. Therefore, a stable and dense silicon carbide coating layer is produced. Moreover, since the vapor deposition is performed on the alumina substrate that has been subjected to metallization, the silicon carbide and metal are well bonded, and the peeling phenomenon that occurs when silicon carbide is directly vapor deposited on alumina, for example, can be completely eliminated, making it an excellent product. A sliding member was obtained. Next, the present invention will be further explained based on illustrative drawings.

第1図は、本発明に係る摺動部材であり、メカニカルシ
ールの密封環を意図した一例である。
FIG. 1 shows a sliding member according to the present invention, and is an example intended for a sealing ring of a mechanical seal.

この情動部村1の基体2はアルミナ(Aそ203)から
なるものである。
The base body 2 of this emotional part 1 is made of alumina (A-203).

3は金属被覆層であり、炭化ケイ素の被覆が施こされる
べきアルミナ基体の表面部を金属化いわゆるメタラィジ
ングを施こすことによって設けたものである。
Reference numeral 3 denotes a metal coating layer, which is provided by metallizing the surface portion of the alumina substrate to be coated with silicon carbide.

4は炭化ケイ素被覆層である。4 is a silicon carbide coating layer.

この炭化ケイ素被覆層4は、繊密でノンポーラスであり
、かつ均質的なものを得ることができるスバッタ蒸着に
よる。このような構成となす摺動部材1は、金属被覆層
3によって、アルミナ基体2と炭化ケイ素被覆層4とが
強固に接合され、しかも熱膨張差や熱歪等が金属被覆層
3によって緩和解消される構造となしたものである。そ
して、本発明に係る摺動部材を得るためのスバッタ蒸着
の好適な装置例を第2図で示した。この第2図において
、5は真空槽、6はケイ素ターゲット、7は永久磁石、
8はヒーター「9はメタラィジングを施こしたアルミナ
基体、10‘まを甫助電極、1 1と12は高周波電源
、13は直流電源、14はメインバルブ、15は自動圧
力調節装置、16はピコアンメータ、17は質量分析装
置、】8はアルゴンガス導入バルフ、19はアセチレン
ガス導入バルブを各々示すものである。このスパッタ装
置は形態上、マグトロン型スパッタ装置と称せられよう
。そしてこのスパッタ装置によって、第1図で示した摺
動部村を如何にして得られるかを説明すれば、まずアル
ミナ基体2に予め金属被覆層3を設けた素材則ちメタラ
ィジングを施こしたアルミナ基体9を真空槽5内に入れ
ておき、真空槽5を10‐6のrrオーダーまで真空に
引き、ヒーター8を500〜100000の範囲内にま
で昇温し「バルブ19よりアセチレンを10‐4〜10
‐5オーダ−まで導入し、さらにバルブ18よりアルゴ
ンを10‐3オーダーまで導入する。次に高周波電源竃
1または、直流電源13によってケイ素ターゲット6に
電力を印加し、スバッタ蒸着を開始する。このようにし
てメタラィジングを施こしたアルミナ基体9の金属被覆
層3の上に炭化ケイ素被覆層4が形成されてゆく。そし
て第1図の摺動部材1が出来る。尚、第2図のスパッタ
装置を用いれば、摺動部材1の炭化ケイ素被覆層4の炭
化ケイ素の組成を都合よく連続的に変えることが出来る
。例えば、最初過剰の遊離ケイ素を含む炭化ケイ素を蒸
着させつつ、次第に正規量論組成の炭化ケイ素へと連続
的に組成を変える事が出来る。つまりト第2図において
、質量分析計17により真空槽5内のアセチレン分圧を
検知し、その電気信号をピコアンメーター16に導き、
このピコアンメーター16の電流値がアセトン分圧に対
応するようになしている。従ってピコアンメーター16
の出力電流を任意に設定しておけば、自動圧力調節装置
15が、その出力電流に応じて作動し、自圧力調節装置
15に付いているバルブが開閉し、アセチレン分圧が低
圧から高圧へと自動制御され、過剰のケイ素を含む炭化
ケイ素から正規量論組成の炭化ケイ素へと炭化ケイ素被
覆層4を連続的にかつ精度良く、制御出来る。
This silicon carbide coating layer 4 is formed by sputter deposition, which is dense, nonporous, and homogeneous. In the sliding member 1 having such a structure, the alumina base 2 and the silicon carbide coating layer 4 are firmly joined by the metal coating layer 3, and the difference in thermal expansion, thermal strain, etc. is alleviated and eliminated by the metal coating layer 3. This is the structure that was created. FIG. 2 shows a preferred example of an apparatus for spatter deposition to obtain the sliding member according to the present invention. In this figure 2, 5 is a vacuum chamber, 6 is a silicon target, 7 is a permanent magnet,
8 is a heater, 9 is an alumina base with metallization, 10 is an auxiliary electrode, 1 1 and 12 are high frequency power supplies, 13 is a DC power supply, 14 is a main valve, 15 is an automatic pressure regulator, 16 is a pico ammeter, 17 is a mass spectrometer, 8 is an argon gas introduction valve, and 19 is an acetylene gas introduction valve.This sputtering apparatus may be called a magtron type sputtering apparatus in terms of form. To explain how to obtain the sliding part shown in FIG. 1, first, a metal coating layer 3 is provided on an alumina base 2, that is, an alumina base 9 that has been subjected to metallization is placed in a vacuum chamber. 5, the vacuum chamber 5 is evacuated to the order of 10-6 rr, the heater 8 is heated to within the range of 500 to 100,000, and the acetylene is evacuated from the valve 19 to 10-4 to 10
Argon is introduced up to -5 order, and then argon is introduced up to 10-3 order from valve 18. Next, power is applied to the silicon target 6 by the high frequency power source 1 or the DC power source 13 to start spatter deposition. In this way, a silicon carbide coating layer 4 is formed on the metal coating layer 3 of the alumina substrate 9 which has been subjected to metallization. Then, the sliding member 1 shown in FIG. 1 is completed. Incidentally, by using the sputtering apparatus shown in FIG. 2, the composition of silicon carbide in the silicon carbide coating layer 4 of the sliding member 1 can be conveniently and continuously changed. For example, it is possible to first deposit silicon carbide containing an excess of free silicon, and then gradually change the composition continuously to stoichiometric silicon carbide. In other words, in FIG.
The current value of this picoammeter 16 is made to correspond to the acetone partial pressure. Therefore picoammeter 16
If the output current is set arbitrarily, the automatic pressure regulator 15 will operate according to the output current, the valve attached to the automatic pressure regulator 15 will open and close, and the acetylene partial pressure will change from low pressure to high pressure. This is automatically controlled, and the silicon carbide coating layer 4 can be continuously and precisely controlled from silicon carbide containing excess silicon to silicon carbide having a normal stoichiometric composition.

このような炭化ケイ素被覆層4となせば遊離ケイ素と金
属被覆層3の金属とが接合されやすくなり、密着性が一
層上昇した摺動部材1を得ることができた。次に実施例
を示す。実施例 基体として外径30脚×内径20帆×厚さ8肌のアルミ
ナ(Aそ203)の基体の一端面に通常行なわれている
手段によってモリブデン(Mo)メタライジングを施こ
した。
With such a silicon carbide coating layer 4, free silicon and the metal of the metal coating layer 3 are easily bonded to each other, making it possible to obtain a sliding member 1 with further improved adhesion. Next, examples will be shown. As an example substrate, molybdenum (Mo) metallization was applied to one end surface of an alumina (A-203) substrate having an outer diameter of 30 feet, an inner diameter of 20 feet, and a thickness of 8 skins by a conventional method.

そしてこのモリブデンからなる金属被覆層の上に炭化ケ
イ素の被覆を形成すべくスバッタ蒸着の操作条件として
、高周波電力:500W、アセチレン分圧:3×10‐
4のrr、アルゴン分圧:3×10‐3ton、アルミ
ナ基体温度:−‐50000、保持時間:180分にて
行った結果11.5〃m厚サの炭化ケイ素被覆層が得ら
れた。炭化ケイ素の表面は鏡面となしており、ビッカー
ス硬度値は3100kg/のあった。さらに得られた摺
動部材を鈴木式摩耗試験機にて相手村としてカーボンを
選び、100Hrのドライ摩耗試験をした結果、1/1
0000肌まで測定できる表面測定機で測定したが、摩
耗量はゼロであった。そして摺動部材の剥離強度をみる
ために引張強度200k9/地のェポキシ樹脂にて沼動
部材の両端面同志を接着し、引張り試験を行ったところ
ェポキシ樹脂部より破断した。この事から被覆層の剥離
強度は200kg/の以上と思われる。以上の如く、詳
述したように本発明に係る情動部材は、アルミナ基体と
炭化ケイ素被覆層とが金属被覆層を介して強固剥離強度
として200k9/雌以上に援合されており、同時にヤ
ングモジュラスの高い構成材のみを一体化せしめた構成
なので、高負荷(一般に2000kg/c材・m/s以
上)に耐え、かつスバッタ蒸着によって繊密な炭化ケイ
素被覆層のものが得られた。
In order to form a silicon carbide coating on this metal coating layer made of molybdenum, the operating conditions for spatter deposition were as follows: high frequency power: 500W, acetylene partial pressure: 3×10-
As a result, a silicon carbide coating layer with a thickness of 11.5 m was obtained. The surface of the silicon carbide was a mirror surface, and the Vickers hardness value was 3100 kg/. Furthermore, the obtained sliding member was subjected to a dry abrasion test for 100 hours using a Suzuki type abrasion tester with carbon as the partner material, and the result was 1/1.
The amount of wear was measured using a surface measuring device capable of measuring up to 0,000 skin, and the amount of wear was zero. Then, in order to check the peel strength of the sliding member, both end surfaces of the sliding member were adhered to each other with epoxy resin having a tensile strength of 200 k9/base, and when a tensile test was performed, the sliding member broke at the epoxy resin portion. From this, it is thought that the peel strength of the coating layer is 200 kg/or more. As described above, in the emotional member according to the present invention, the alumina base and the silicon carbide coating layer are bonded together through the metal coating layer to have a strong peel strength of 200 k9/female or more, and at the same time have a Young's modulus of Since it is a structure in which only constituent materials with high efficiencies are integrated, it can withstand high loads (generally 2000 kg/c material/m/s or more), and a dense silicon carbide coating layer can be obtained by sputter deposition.

しかも安価なアルミナを基体として用いており、簡便に
製造出来るので、産業市場へ直ちに供することの出来る
摺動部材である。
Furthermore, since inexpensive alumina is used as the base material and it can be easily manufactured, the sliding member can be immediately provided to the industrial market.

また、この摺動部材は耐摩耗性が極めて優れているので
、メカニカルシールの密封環、軸受のすべり面、タービ
ン、ポンプ等の摺動部分や他の一般キカィ部品に適用す
れば前述した種々の効果を発揮できる。
In addition, since this sliding member has extremely high wear resistance, it can be applied to the sealing rings of mechanical seals, sliding surfaces of bearings, sliding parts of turbines, pumps, etc., and other general parts. It can be effective.

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

第1図は、本発明に係る摺動部材の部分斜視図、第2図
は、第1図の摺動部材を製造するためのスパッタ装置の
概略断面図である。 1・・・摺敷部材、2・・・アルミナ基体、3・・・金
属被覆層、4・・・炭化ケイ素被覆層。 第1図 第2図
FIG. 1 is a partial perspective view of a sliding member according to the present invention, and FIG. 2 is a schematic sectional view of a sputtering apparatus for manufacturing the sliding member of FIG. 1. DESCRIPTION OF SYMBOLS 1...Sliding member, 2...Alumina base, 3...Metal coating layer, 4...Silicon carbide coating layer. Figure 1 Figure 2

Claims (1)

【特許請求の範囲】[Claims] 1 スパツタ蒸着によつて、炭化ケイ素の被覆が施こさ
れるべき、アルミナ基体の表面部に金属被覆層を設けて
炭化ケイ素を形成させてなる摺動部材。
1. A sliding member in which a metal coating layer is provided on the surface of an alumina substrate to be coated with silicon carbide by sputter deposition to form silicon carbide.
JP13401480A 1980-09-25 1980-09-25 sliding member Expired JPS6033794B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP13401480A JPS6033794B2 (en) 1980-09-25 1980-09-25 sliding member

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP13401480A JPS6033794B2 (en) 1980-09-25 1980-09-25 sliding member

Publications (2)

Publication Number Publication Date
JPS5757873A JPS5757873A (en) 1982-04-07
JPS6033794B2 true JPS6033794B2 (en) 1985-08-05

Family

ID=15118349

Family Applications (1)

Application Number Title Priority Date Filing Date
JP13401480A Expired JPS6033794B2 (en) 1980-09-25 1980-09-25 sliding member

Country Status (1)

Country Link
JP (1) JPS6033794B2 (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS60245829A (en) * 1984-05-21 1985-12-05 Sankyo Kasei Kk Complex sliding member
JPH0679992B2 (en) * 1987-06-17 1994-10-12 日本碍子株式会社 Metal-ceramic composite
JPS6413280U (en) * 1987-07-15 1989-01-24

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JPS5757873A (en) 1982-04-07

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