JPH0525617A - Ion plating method - Google Patents

Ion plating method

Info

Publication number
JPH0525617A
JPH0525617A JP15829291A JP15829291A JPH0525617A JP H0525617 A JPH0525617 A JP H0525617A JP 15829291 A JP15829291 A JP 15829291A JP 15829291 A JP15829291 A JP 15829291A JP H0525617 A JPH0525617 A JP H0525617A
Authority
JP
Japan
Prior art keywords
ion plating
metal
plating method
coating
film
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.)
Granted
Application number
JP15829291A
Other languages
Japanese (ja)
Other versions
JP2667309B2 (en
Inventor
Katsumi Takiguchi
勝美 滝口
Masanori Oya
正規 大矢
Tatsuhiko Fujinuma
龍彦 藤沼
Kenichi Kobayashi
賢一 小林
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.)
Riken Corp
Japan Metals and Chemical Co Ltd
Original Assignee
Riken Corp
Japan Metals and Chemical 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 Riken Corp, Japan Metals and Chemical Co Ltd filed Critical Riken Corp
Priority to JP3158292A priority Critical patent/JP2667309B2/en
Publication of JPH0525617A publication Critical patent/JPH0525617A/en
Application granted granted Critical
Publication of JP2667309B2 publication Critical patent/JP2667309B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

PURPOSE:To inexpensively produce a uniform film at a high vapor deposition rate by using the sintered body or green compaction molding of a sublimatable metal as a material to be evaporated and coating the surface of a base material with this material by an HCD method. CONSTITUTION:The material 16 to be evaporated is the sintered body or green compaction molding of the sublimatable metal, such as Cr or Mn. This material is put into a crucible 15 and is irradiated with a focused electron beam emitted from an electron mirror 17. The electron beam is a lowvoltage-large current and increases the heating surface area of the material 16 to be evaporated by decreasing the current of a focusing coil 19, by which the large quantity evaporation of the sublimatable metal is allowed.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、耐摩耗性皮膜を被覆す
るイオンプレーティング法に関し、更に詳しくは、昇華
性金属の炭化物、窒化物、或いは炭窒化物の圧膜を高速
で得るイオンプレーティング法に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an ion plating method for coating an abrasion resistant film, and more particularly, to an ion plating method for obtaining a pressure film of a sublimable metal carbide, nitride or carbonitride at a high speed. Regarding the Ting method.

【0002】[0002]

【従来の技術と問題点】従来より、耐摩耗性皮膜を均一
に形成でき、しかも仕上げ加工が不要なほどの仕上り面
が得られる形成法として、PVD法(Physical Vaper D
epositon Prosess)が知られる。このPVD法に含まれ
る方法にイオンプレーティング法がある。このイオンプ
レーティング法は真空蒸着の一種であり、現在では、特
に摺動部材や切削工具等にとって重要な厚膜形成手段と
して極く一般的な表面処理法となっている。イオンプレ
ーティング法の利点としては、金属炭化物、金属窒化
物、金属酸化物のような金属化合物、或いはこれらの複
合物の皮膜処理が可能な点がある。更に、真空蒸着法で
形成された皮膜よりは母材との密着性が格段に優れてお
り、スパッタリング法よりも皮膜生成速度が非常に速い
といった利点があげられる。イオンプレーティング法
は、前述のような皮膜金属元素を蒸発材として高温で加
熱して蒸発させ、放電により蒸発金属原子、または雰囲
気ガス中の窒素、炭素、酸素等の原子をイオン化させ
る。これにより高電界で素材表面に引きつけて、皮膜金
属元素又はその化合物の皮膜を得る方法である。
2. Description of the Related Art Conventionally, PVD (Physical Vaper D) has been used as a forming method capable of uniformly forming an abrasion resistant film and obtaining a finished surface that does not require finishing.
epositon Prosess) is known. A method included in this PVD method is an ion plating method. This ion plating method is a kind of vacuum vapor deposition, and is now a very general surface treatment method as a thick film forming means which is particularly important for sliding members, cutting tools and the like. An advantage of the ion plating method is that a metal carbide, a metal nitride, a metal compound such as a metal oxide, or a composite of these compounds can be coated. Further, it has an advantage that the adhesion to the base material is remarkably superior to that of the film formed by the vacuum vapor deposition method, and the film formation rate is much faster than that of the sputtering method. In the ion plating method, the above-mentioned coating metal element is heated as an evaporating material at a high temperature to evaporate, and the evaporating metal atom or atoms such as nitrogen, carbon, oxygen in the atmospheric gas is ionized by discharge. This is a method of attracting the surface of the material with a high electric field to obtain a film of the film metal element or its compound.

【0003】[0003]

【考案が解決しようとする課題】ところで、こうした従
来のイオンプレーティング法は、蒸発材である皮膜金属
として、溶解により形成した塊(インゴット)、または
HIP法で形成したインゴットを用いている。そのた
め、本来、蒸発速度が速いとされるCr、Mnのような昇
華性金属であっても、蒸発速度が遅くなりかつ蒸発材と
して高価となる事情がある。従って、素材表面に皮膜金
属の厚膜を得ることは、生産性の低下はもとより、高価
な材料費と相まってコスト高を招く現状にある。従っ
て、本発明の目的は、従来法の課題を解消し、格段に速
い蒸着速度でかつ長く被覆が行えて生産コストの低減を
可能にし、被膜の均一性に優れて工業的利用価値の顕著
なイオンプレーティング法を提供することにある。
By the way, in such a conventional ion plating method, a lump (ingot) formed by melting or an ingot formed by the HIP method is used as a film metal which is an evaporation material. Therefore, even with sublimable metals such as Cr and Mn, which are supposed to have a high evaporation rate, the evaporation rate becomes slow and the evaporation material becomes expensive. Therefore, obtaining a thick film of the coating metal on the surface of the raw material is not only low in productivity but also high in cost due to high material cost. Therefore, the object of the present invention is to solve the problems of the conventional method, to enable coating at a markedly high vapor deposition rate and for a long time, to reduce the production cost, and to provide a coating with excellent uniformity and industrial value. It is to provide an ion plating method.

【0004】[0004]

【課題を解決するための手段】本発明によるイオンプレ
ーティング法は、昇華性金属の焼結体または圧粉成形体
を蒸発材とし、母材の表面にイオン化法のHCD法によ
って被覆する皮膜処理方法である。
The ion plating method according to the present invention is a film treatment in which a sintered body or a powder compact of a sublimable metal is used as an evaporation material and the surface of a base material is coated by the HCD method of the ionization method. Is the way.

【0005】[0005]

【作用】例えば、Cr、Mn等の昇華性金属による焼結
体、又は圧粉成形体を蒸発材として用い、母材の表面に
HCDイオンプレーティング法で被覆する。昇華性金属
の焼結体又は圧粉成形体を蒸発材として用いることによ
り、従来のイオンプレーティング法よりも格段に速い速
度で被覆が行え、特に膜厚を大きく形成しようとする場
合に顕著である。
For example, a sintered body of a sublimable metal such as Cr or Mn or a powder compact is used as an evaporation material, and the surface of the base material is covered by the HCD ion plating method. By using a sintered body or a powder compact of a sublimable metal as an evaporation material, coating can be performed at a speed significantly higher than that of the conventional ion plating method, which is remarkable especially when trying to form a large film thickness. is there.

【0006】[0006]

【実施例】以下、本発明によるイオンプレーティング法
の実施例を図面に基づいて説明する。図1は、本発明に
使用されるイオンプレーティング装置10の概略を示
す。本装置10はHCD法(Hollow Cathode Discharge)
に基づく。装置は真空ポンプにより減圧される真空槽1
1を有し、この内部には表面被覆される被着体の母材1
2が保持具13により回転可能に保持されている。母材
12は例えば外径85mm、厚さ2mmのSUS304によ
るパイプである。保持具13の上方には母材12を所定
温度に加熱するヒータ14が設置されている。また、保
持具13の下方には水冷銅式のルツボ15が設置され、
この内部には被覆金属(以下、蒸発材という)16が収
容されている。蒸発材16はCr、Mn等の昇華性金属に
よる焼結体、又は圧粉成形体を用いている。
Embodiments of the ion plating method according to the present invention will be described below with reference to the drawings. FIG. 1 schematically shows an ion plating apparatus 10 used in the present invention. This device 10 is an HCD method (Hollow Cathode Discharge)
based on. The equipment is a vacuum chamber 1 whose pressure is reduced by a vacuum pump.
1. The base material 1 of the adherend to be surface-coated
2 is rotatably held by a holder 13. The base material 12 is, for example, a pipe made of SUS304 having an outer diameter of 85 mm and a thickness of 2 mm. A heater 14 that heats the base material 12 to a predetermined temperature is installed above the holder 13. A water-cooled copper type crucible 15 is installed below the holder 13.
A coating metal (hereinafter referred to as an evaporation material) 16 is housed inside this. The evaporation material 16 is a sintered body of a sublimable metal such as Cr or Mn, or a powder compact.

【0007】また、真空槽11の側壁には、HCD型の
電子銃17、雰囲気ガス(N2ガス)の導入管18が取
り付けられている。ルツボ15の上方には集束コイル1
9が配置され、この集束コイル19によって電子銃17
から射出された電子ビームを蒸発材16に照射できるよ
う構成されている。
On the side wall of the vacuum chamber 11, an HCD type electron gun 17 and an atmosphere gas (N 2 gas) introducing pipe 18 are attached. The focusing coil 1 is provided above the crucible 15.
9 is arranged, and this focusing coil 19 causes an electron gun 17
The evaporation material 16 can be irradiated with an electron beam emitted from the evaporation material 16.

【0008】この装置において、母材12の皮膜形成態
様は、保持具13が駆動することによりこれに保持され
た被着材の母材12が回転する。この時、ヒータ14に
より回転中の母材12の加熱が行われる。電子銃17か
らは電子ビームが射出され、前述の蒸発材16に照射さ
れる。電子ビームは低電圧ー大電流であり、集束コイル
19の電流を低下させることで、蒸発材16の加熱表面
積を大きくでき、昇華性金属の大量蒸発が可能である。
また、電子ビームは10~2torr〜10~4torrといった具
合に低真空で作動するため、焼結体や圧粉成形体を蒸発
材16として用いた場合に生じ易いスプラッシュ等にお
いても通常に作動し続け、何ら問題を生じない。
In this apparatus, in the film forming mode of the base material 12, when the holder 13 is driven, the base material 12 of the adherend held by the holder 13 rotates. At this time, the rotating base material 12 is heated by the heater 14. An electron beam is emitted from the electron gun 17 and irradiates the evaporation material 16 described above. The electron beam has a low voltage and a large current, and by lowering the current of the focusing coil 19, the heating surface area of the evaporation material 16 can be increased and a large amount of sublimable metal can be evaporated.
Further, since the electron beam operates in a low vacuum such as 10 to 2 torr to 10 to 4 torr, it normally operates even in a splash or the like that is likely to occur when a sintered body or a powder compact is used as the evaporation material 16. Continue to work, no problems arise.

【0009】次に、以下の条件による具体例で形成され
た膜厚と、この条件で蒸発材16のみを従来の金属クロ
ム・インゴットに替えた場合に得られた膜厚との比較を
行った。 ・母材温度 400℃ ・電子ビーム出力 38Vー500A ・ルツボ仕様 径φ70:深さ100mm ・窒素ガス分圧 1×10 ̄torr ・蒸発材 金属クロム焼結体 ・被覆処理時間 30分〜120分
Next, a comparison was made between the film thickness formed in the specific example under the following conditions and the film thickness obtained when only the evaporation material 16 was replaced with the conventional metal chromium ingot under these conditions. .. -Base temperature 400 ° C., the electron beam output 38V over 500A-crucible Specifications diameter Fai70: depth 100 mm, the nitrogen gas partial pressure 1 × 10¯ 3 torr · evaporation material metallic chromium sintered-coating treatment time 30 to 120 minutes

【0010】図2は比較結果を示し、図の横軸は被覆処
理時間、縦軸は母材12であるパイプ外周に被覆された
CrーN膜の厚さをミクロン単位で示したものである。
図中、実線は本発明による蒸発材16としてクロム粉の
焼結体を用いた場合を示し、破線は従来法で前述のクロ
ム・インゴットを用いた場合である。
FIG. 2 shows the comparison results, in which the horizontal axis represents the coating treatment time and the vertical axis represents the thickness of the Cr--N film coated on the outer circumference of the pipe, which is the base material 12, in units of microns. ..
In the figure, the solid line shows the case where a sintered body of chromium powder is used as the evaporation material 16 according to the present invention, and the broken line shows the case where the aforementioned chromium ingot is used in the conventional method.

【0011】この図2から明らかなように、本発明によ
るイオンプレーティング法では、従来法とは格段に速い
蒸着速度で被覆が行え、長時間のイオンプレーティング
にあっても、その蒸着速度が低下のきざしを見せること
なく厚膜が得られることがわかる。特に、膜厚の大きい
領域ほど、本発明は著しく有利であることが理解できよ
う。
As is apparent from FIG. 2, the ion plating method according to the present invention can perform coating at a remarkably high vapor deposition rate as compared with the conventional method, and the vapor deposition rate can be improved even in the case of long-time ion plating. It can be seen that a thick film can be obtained without showing any signs of deterioration. In particular, it can be understood that the present invention is remarkably advantageous in a region having a large film thickness.

【0012】また、図3は、本発明によるイオンプレー
ティング法により作成したCrーN膜の断面のCr濃度
変化を電子プローブ微小部分析法(EPMA)により測
定した結果を示すグラフである。図4は従来のイオンプ
レーティング法にて作成したCrーN膜の断面のCr濃
度変化を同じくEPMAにより測定した結果を示す。図
3及び図4の比較により、本発明は従来に比べて被膜の
Cr濃度変化は少なく、ほぼ均質な被膜が得られること
が理解される。
FIG. 3 is a graph showing the result of measuring the Cr concentration change in the cross section of the Cr-N film prepared by the ion plating method according to the present invention by the electron probe microanalysis method (EPMA). FIG. 4 shows the result of measuring the Cr concentration change in the cross section of the Cr-N film formed by the conventional ion plating method by the same EPMA. By comparing FIG. 3 and FIG. 4, it is understood that the present invention has a smaller change in the Cr concentration of the coating as compared with the prior art, and a substantially uniform coating can be obtained.

【0013】なお、イオンプレーティング終了後は、設
備されている。スクレーパ機構等により容易にルツボ内
のクリーニングが可能である。このことから、生産性に
優れかつ安価に厚膜の形成が可能である。
After the ion plating is completed, the equipment is installed. The inside of the crucible can be easily cleaned by a scraper mechanism or the like. Therefore, it is possible to form a thick film with excellent productivity and at low cost.

【0014】[0014]

【発明の効果】以上説明したように、本発明によるイオ
ンプレーティング法は、Cr、Mn等の昇華性金属による
焼結体、又は圧粉成形体を蒸発材として用い、母材の表
面にHCD法で被覆する方法であり、従来のイオンプレ
ーティング法よりも格段に速い蒸着速度でかつ長く被覆
が行え、生産コストの低減が可能である。また、被膜の
均一性に優れていることから、その工業的利用価値は著
しく大きい。
As described above, in the ion plating method according to the present invention, a sintered body made of a sublimable metal such as Cr or Mn or a powder compact is used as an evaporation material, and HCD is formed on the surface of the base material. This is a method of coating, and the coating can be performed at a vapor deposition rate significantly longer than that of the conventional ion plating method, and the coating can be performed for a long time, and the production cost can be reduced. Further, since the coating film has excellent uniformity, its industrial utility value is remarkably large.

【図面の簡単な説明】[Brief description of drawings]

【図1】 本発明によるHCDイオンプレーティング法
に基づいた装置の概略図
FIG. 1 is a schematic diagram of an apparatus based on the HCD ion plating method according to the present invention.

【図2】 本発明のイオンプレーティング法と従来のイ
オンプレーティング法との膜厚形成速度を比較した結果
の性能曲線を示すグラフ
FIG. 2 is a graph showing a performance curve as a result of comparing the film thickness formation rates of the ion plating method of the present invention and the conventional ion plating method.

【図3】 本発明によるイオンプレーティング法により
作成したCrーN膜の断面のCr濃度変化を電子プロー
ブ微小部分析法(EPMA)により測定した結果を示す
グラフ
FIG. 3 is a graph showing a result of measuring a change in Cr concentration in a cross section of a Cr—N film formed by an ion plating method according to the present invention by an electron probe microanalysis method (EPMA).

【図4】 従来のイオンプレーティング法にて作成した
CrーN膜の断面のCr濃度変化を同じくEPMAによ
り測定した結果を示すグラフ
FIG. 4 is a graph showing the result of measuring the Cr concentration change in the cross section of the Cr—N film prepared by the conventional ion plating method by the same EPMA.

【符号の説明】[Explanation of symbols]

11...真空槽、 12...母材、 13...母
材保持具、 14...ヒータ、 15...水冷銅ル
ツボ、 16...蒸発材、 17...HCD電子ビ
ーム銃、 18...雰囲気ガス導入管、 19...
集束コイル
11. . . Vacuum chamber, 12. . . Base material, 13. . . Base material holder, 14. . . Heater, 15. . . Water-cooled copper crucible, 16. . . Evaporative material, 17. . . HCD electron beam gun, 18. . . Atmosphere gas introduction pipe, 19. . .
Focusing coil

───────────────────────────────────────────────────── フロントページの続き (72)発明者 藤沼 龍彦 千葉県市川市中山1−13−10 (72)発明者 小林 賢一 山形県西置賜郡小国町大字小国町390 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Tatsuhiko Fujinuma 1-13-10 Nakayama, Ichikawa City, Chiba Prefecture (72) Inventor Kenichi Kobayashi 390 Oguni Town, Oguni Town, Nishiokitama District, Yamagata Prefecture

Claims (1)

【特許請求の範囲】 【請求項1】昇華性金属の焼結体または圧粉成形体を蒸
発材とすることを特徴とするイオンプレーティング法。
Claim: What is claimed is: 1. An ion plating method, wherein a sublimable metal sintered body or a green compact is used as an evaporation material.
JP3158292A 1991-06-28 1991-06-28 Abrasion resistant film formation method by HCD ion plating Expired - Fee Related JP2667309B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP3158292A JP2667309B2 (en) 1991-06-28 1991-06-28 Abrasion resistant film formation method by HCD ion plating

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP3158292A JP2667309B2 (en) 1991-06-28 1991-06-28 Abrasion resistant film formation method by HCD ion plating

Publications (2)

Publication Number Publication Date
JPH0525617A true JPH0525617A (en) 1993-02-02
JP2667309B2 JP2667309B2 (en) 1997-10-27

Family

ID=15668422

Family Applications (1)

Application Number Title Priority Date Filing Date
JP3158292A Expired - Fee Related JP2667309B2 (en) 1991-06-28 1991-06-28 Abrasion resistant film formation method by HCD ion plating

Country Status (1)

Country Link
JP (1) JP2667309B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1334778A2 (en) 2002-02-08 2003-08-13 Fuji Photo Film Co., Ltd. Rod for a coating device, and process for producing the same

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS53114739A (en) * 1977-03-18 1978-10-06 Toyo Soda Mfg Co Ltd Molding of metal for surface coating and their preparation

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS53114739A (en) * 1977-03-18 1978-10-06 Toyo Soda Mfg Co Ltd Molding of metal for surface coating and their preparation

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP1334778A2 (en) 2002-02-08 2003-08-13 Fuji Photo Film Co., Ltd. Rod for a coating device, and process for producing the same

Also Published As

Publication number Publication date
JP2667309B2 (en) 1997-10-27

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