JPS62158859A - Pretreatment - Google Patents

Pretreatment

Info

Publication number
JPS62158859A
JPS62158859A JP15986A JP15986A JPS62158859A JP S62158859 A JPS62158859 A JP S62158859A JP 15986 A JP15986 A JP 15986A JP 15986 A JP15986 A JP 15986A JP S62158859 A JPS62158859 A JP S62158859A
Authority
JP
Japan
Prior art keywords
substrate
ion bombardment
inert gas
adhesion
gas
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.)
Pending
Application number
JP15986A
Other languages
Japanese (ja)
Inventor
Kazuo Kanehiro
金廣 一雄
Tadashi Igarashi
五十嵐 廉
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.)
Sumitomo Electric Industries Ltd
Original Assignee
Sumitomo Electric Industries 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 Sumitomo Electric Industries Ltd filed Critical Sumitomo Electric Industries Ltd
Priority to JP15986A priority Critical patent/JPS62158859A/en
Publication of JPS62158859A publication Critical patent/JPS62158859A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To improve adhesive strength of dry plating, by subjecting a metallic substrate to ion bombardment by use of inert gas and then to ion bombardment by use of hydrogen gas. CONSTITUTION:Prior to the application of dry plating to the metallic substrate of copper (alloy), etc., ion bombardment is first applied by use of inert gas such as argon gas, etc., so as to remove adsorbates on the oxides at the substrate surface, such as oil, dust, etc., followed by ion bombardment by use of hydrogen gas, so that adsorbate-free oxides at the substrate surface are removed by reduction and the metallic-substrate surface is provided with high cleanliness. According to the above method, adhesive strength between the dry-plated film and substrate can be improved by means of short-time treatment without causing distortion in the substrate.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は金属基板に乾式メッキを施すにあたシ、該基板
表面を清浄化するための前処理方法に関するものである
。本発明の前処理方法はrC用リードフレーム等に適用
して非常に有利である。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a pretreatment method for cleaning the surface of a metal substrate before performing dry plating on the substrate. The pretreatment method of the present invention is very advantageous when applied to lead frames for rC and the like.

〔従来の技術〕[Conventional technology]

一般に乾式メッキでの要求特性としては、膜質、基板−
被膜間密着性、蒸着速度など品質面、及び経済面に対し
て多岐に渡っているか、と少わけ品質面では、基板間密
着性、経済面では、タクトタイムが重要である。
In general, the required characteristics for dry plating include film quality, substrate
There are a wide range of factors in terms of quality, such as adhesion between films and deposition rate, as well as economic aspects.In terms of quality, adhesion between substrates and economic terms, takt time is important.

従来、物理蒸着(pvn)法や化学蒸着(OVD)法に
よル乾式メッキを行なう場合、基板−被膜間の密着性を
確保する為に真空容器内で基板の加熱、不活性ガス中で
のイオンボンバード(ionbombarcl)  等
により基板のクリーニングを施していた。しかしながら
、これら方法は、基板加熱によるガス放出やアルゴンイ
オン等による表面吸着物の破壊は生じるものの、金属基
板表面に生じた酸化物等の強固な附着力を有する物質に
対しては、十分な破壊が行なわれず、結果的に基板−被
展間の密着性劣化につながっていもこの現象は、特に基
板材質が銅若しくは銅合金の場合に顕著であシ、銅もし
くは鋼合金基板に密着性の優れた被膜を得ることは非常
に困難であった。
Conventionally, when dry plating is performed using physical vapor deposition (PVN) or chemical vapor deposition (OVD), the substrate is heated in a vacuum chamber or heated in an inert gas to ensure adhesion between the substrate and the coating. The substrate was cleaned using ion bombardment or the like. However, although these methods cause the destruction of surface adsorbed substances due to gas release due to substrate heating and argon ions, etc., these methods are sufficient to destroy substances with strong adhesion such as oxides formed on the surface of metal substrates. This phenomenon is especially noticeable when the substrate material is copper or copper alloy, and even if the adhesion between the substrate and the workpiece is deteriorated, this phenomenon is particularly noticeable when the substrate material is copper or copper alloy. It was very difficult to obtain such a coating.

この対応策として、基板温度を極端に上げる、不活性ガ
ス中でのイオンボンバード時間を長くする、あるいは基
板を真空容器内に入れる前に酸洗等を施す等の所謂前処
理強化を行っているのが現状である。
As countermeasures to this problem, so-called pretreatment enhancements are being taken, such as extremely raising the substrate temperature, lengthening the ion bombardment time in an inert gas, or subjecting the substrate to pickling before placing it in a vacuum container. is the current situation.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

ところで、上述の方法によシ、密着性はある程度向上は
するものの、基板温度の上昇は、基板に熱歪を4えたシ
真空度によっては残留酸素による表面酸化の問題や設備
的負荷も大きい。
By the way, although the above-mentioned method improves the adhesion to some extent, the increase in substrate temperature causes problems such as surface oxidation due to residual oxygen and heavy equipment load depending on the degree of vacuum due to thermal strain on the substrate.

また、基板の酸洗等を採シ入れる事は、工程を複雑化す
るばかシか、コスト的にも非常に不利となる。また、不
活性ガス中のイオンボンバード時間を長くすることは、
タクトタイムが長くなシコストが高くなると共に基板が
プラズマに長時間さらされる事から、基板温度の上昇や
蒸着室壁面の汚れが基板に再付着する所謂逆スパッター
現象が生じ、良い前処理方法とは言い難い。以上述べた
如〈従来の方法では品質面、経済面で種々の問題を抱え
ているのである。
In addition, introducing pickling of the substrate will not only complicate the process but also be extremely disadvantageous in terms of cost. In addition, increasing the ion bombardment time in inert gas
As the takt time is longer, the cost is higher, and the substrate is exposed to plasma for a longer period of time, the substrate temperature rises and the so-called reverse sputtering phenomenon occurs in which dirt from the deposition chamber wall re-adheres to the substrate. It's hard to say. As mentioned above, conventional methods have various problems in terms of quality and economy.

そこで、本発明は、上記欠点を解消した金属基板の表面
をり17−ニングする前処理方法で、特に銅もしくは鋼
合金基板にも有効な方法を提供することを目的としてい
る。すなわち、本発明の目的は乾式メッキを行なうに際
して基板表面のクリーニングを簡便で且つ短時間で処理
し、銅もしくは銅合金基板においても基板−wt膜間の
密着性を著しく、且つ確実に向上せしめる前処理方法を
提供するにある。なお、こζで言う乾式メッキとは、真
空蒸着、イオンブレーティング、スパッタリング等の物
理蒸着及びプラズーrf応用したものも含む化学蒸着を
指す。
SUMMARY OF THE INVENTION Therefore, an object of the present invention is to provide a pretreatment method for annealing the surface of a metal substrate that eliminates the above-mentioned drawbacks, and is particularly effective for copper or steel alloy substrates. That is, the purpose of the present invention is to process the cleaning of the substrate surface simply and in a short time when performing dry plating, and to significantly and reliably improve the adhesion between the substrate and the wt film even on copper or copper alloy substrates. To provide a processing method. Note that the dry plating referred to here refers to physical vapor deposition such as vacuum deposition, ion blating, and sputtering, and chemical vapor deposition including those using plasma RF.

〔問題点を解決するための手段〕[Means for solving problems]

本発明は金属基板に乾式メッキ法を用いて被膜を施すに
あたシ予め該基板表面全清浄化する前処理方法において
、まず不活性ガスを用いてイオンボンバードを行い、次
に水素ガスを用いてイオンボンバードを行う、こと′t
−特徴とする前処理方法であり、これによシ上記目的を
達成する。本発明の特に好ましい実M態様としては、金
属基板が銅もしくは銅合金基板である上記方法、あるい
は乾式メッキ法が物理蒸着法もしくは化学蒸着法である
上記方法が挙げられる。
In the present invention, in a pretreatment method for completely cleaning the surface of a metal substrate before applying a coating using a dry plating method, ion bombardment is first performed using an inert gas, and then hydrogen gas is used To perform an ion bombardment
- A pretreatment method characterized by this, which achieves the above objectives. Particularly preferred embodiments of the present invention include the above method in which the metal substrate is a copper or copper alloy substrate, or the above method in which the dry plating method is a physical vapor deposition method or a chemical vapor deposition method.

すなわち、本発明は、真空容器内で乾式メンキするに先
立って、鋼若しくは鋼合金からなる金属基板表面をクリ
ーニングする前処理方法において、先ず不活性ガス、例
えばアルゴンガス等によ勺、イオンボンバードを行ない
、金属基板表面の酸化物上の油分や塵埃等の吸着物を、
原子賀曾の重いアルゴン等のイオンで除去する。
That is, the present invention provides a pretreatment method for cleaning the surface of a metal substrate made of steel or steel alloy prior to dry peeling in a vacuum container, in which the surface is first subjected to ion bombardment using an inert gas such as argon gas, etc. This process removes adsorbed substances such as oil and dust on the oxide on the surface of the metal substrate.
Remove with heavy ions such as argon.

然る後に、水素ガスのイオンボンバードによ)、金属基
板表面の吸着物のない酸化物を還元除去し、金属基板表
面を極めて高い清浄度にするものである。
Thereafter, by ion bombardment of hydrogen gas), oxides free of adsorbed substances on the surface of the metal substrate are reduced and removed, thereby making the surface of the metal substrate extremely highly clean.

この場合、水素ガスによるイオンボンバードのみでは、
水素自体の原子質量が極端に低い事から、基板上の油分
や塵埃等を除去する事は不可能であシ、下地の酸化物を
完全に還元する事はできない。これはすなわち、金属基
板表面のクリーニングを十分行なえないことであシ、基
板−被膜間の密着8:を安定、向上させる事はできない
In this case, ion bombardment using hydrogen gas alone will
Since the atomic mass of hydrogen itself is extremely low, it is impossible to remove oil, dust, etc. from the substrate, and it is impossible to completely reduce the underlying oxide. In other words, the surface of the metal substrate cannot be sufficiently cleaned, and the adhesion between the substrate and the film cannot be stabilized or improved.

従って、本発明によると、従来法の単一のイオンボンバ
ードや基板加熱等では達成できなかった金属基板表面の
クリーニングが十分に行なえる。また、本発明は、上述
したように、2段階のイオンボンバードを実施している
が、その優先度は明らかに存在し、先ず不活性ガスを用
い次に水素ガスを用いてイオンボンバードを行うことが
必須である。例えば、水素ガスイオンボンバードを不活
性ガスイオンボンバードよシ先に実施した場合には、水
素ガスイオンボンバードによシ酸化物上に強固な吸着物
のない部分の酸化物が還元除去され、その後の不活性ガ
スのイオンボンバードによシ、部分的に残っている酸化
物上の強固な吸着物を除去することになる。この事は、
金属基板表面上に部分的に酸化物を残す事であシ、また
、水素ガスのイオンボンバードによ)酸化物が除去され
たクリーンな表面が再びアルゴンイオンでボンバードさ
れる事から、逆スパンター効果で新らたな吸着物が生じ
、結果的には清浄度の高い基板表面が得られず、基板−
被膜間の密着性を向上せしむることかできないのである
Therefore, according to the present invention, the metal substrate surface can be sufficiently cleaned, which could not be achieved by conventional methods such as single ion bombardment or substrate heating. Furthermore, as described above, in the present invention, ion bombardment is performed in two stages, but there is clearly a priority between first performing ion bombardment using inert gas and then using hydrogen gas. is required. For example, if hydrogen gas ion bombardment is performed before inert gas ion bombardment, the oxide in the portions of the silicon oxide that do not have strong adsorbents is reduced and removed by hydrogen gas ion bombardment, and the subsequent Ion bombardment with an inert gas will partially remove the stubborn adsorbates on the remaining oxide. This thing is
By partially leaving oxides on the surface of the metal substrate, the clean surface from which oxides have been removed (by hydrogen gas ion bombardment) is bombarded again with argon ions, creating a reverse spunter effect. new adsorbed substances are generated, and as a result, a highly clean substrate surface cannot be obtained, and the substrate
The only thing that can be done is to improve the adhesion between the coatings.

以上説明したように、本発明では、鋼若しくは銅合金か
らなる金属基板表面の吸着物、酸化物を完全に除去する
事が可能であシ、また、上述のような前処理中に基板表
面を汚す事もなく、清浄度の高い基板表面が得られる。
As explained above, in the present invention, it is possible to completely remove adsorbed substances and oxides from the surface of a metal substrate made of steel or copper alloy, and it is also possible to completely remove adsorbed substances and oxides from the surface of a metal substrate made of steel or copper alloy. A highly clean substrate surface can be obtained without contamination.

その後、引きつづき、物理蒸着や化学蒸着によ勺被膜を
形成する事によシ、基板−被膜間の密着性を著しく向上
せしむることかできるのである。
Thereafter, the adhesion between the substrate and the coating can be significantly improved by subsequently forming a protective coating by physical vapor deposition or chemical vapor deposition.

尚、本発明は、イオンボンバードによる前処理であるが
、従来のイオンボンバードと異なる点について再び強調
するならば、 1)従来の単一イオンボンバードでUす(,2段階のイ
オンボンバードを実施している、2)゛ その2段階と
は、不活性ガス及び水素ガスのイオンボンバードである
、 3)また、2段階のイオンボンバードを実施するにab
、工程的に優先度が規定され、不活性ガスのイオンボン
バード実施後に水素ガスのイオンボンバードが実施され
ねばならない、の諸点である。
Although the present invention involves pretreatment by ion bombardment, the points that are different from conventional ion bombardment are as follows: 1) Conventional single ion bombardment is performed (2-stage ion bombardment is performed). 2) The two stages are ion bombardment using inert gas and hydrogen gas. 3) Also, to carry out the two stage ion bombardment,
, priority is defined in terms of process, and ion bombardment of hydrogen gas must be performed after ion bombardment of inert gas.

本発明における不活性ガスを用いるイオンボンバードは
、例えばアルゴンガスを用い、10−3〜10  To
rr、 D C〜IKV、 〜5分程度の条件で行えば
十分である。また水素ガスを用いるイオンボンバードも
10 〜10  Torr、  DO%IKV、〜5分
程度の条件で行えばよい。
Ion bombardment using an inert gas in the present invention uses, for example, argon gas and
It is sufficient to carry out the test under conditions of about 5 minutes. Ion bombardment using hydrogen gas may also be performed under conditions of 10 to 10 Torr, DO% IKV, and about 5 minutes.

以下本発明の効果を実施例を用いて説明する。The effects of the present invention will be explained below using Examples.

〔実施例〕〔Example〕

板厚0.25m5長さ2001m、巾1501)mのリ
ン青銅からなる基板を用い、該基板上に表1注に示す如
くの条件の前処理を行なった後、基板温度50Cでアル
ゴンガスを導入しつつ、3X10Torrの真空度によ
シムlの直流イオンブレーティングを行ない、厚さ4μ
lの被IIIを得た。
Using a substrate made of phosphor bronze with a thickness of 0.25 m, a length of 2001 m, and a width of 1501) m, the substrate was pretreated under the conditions shown in the notes in Table 1, and then argon gas was introduced at a substrate temperature of 50 C. At the same time, the shim was subjected to DC ion blating at a vacuum level of 3 x 10 Torr, and the thickness was 4 μm.
1 of analytes III were obtained.

該基板に180度折多曲げテスト密着性を実施したとこ
ろ、表1に示す結果が得られた。
When the substrate was subjected to a 180 degree bending test for adhesion, the results shown in Table 1 were obtained.

表1の評価欄は次の基準で示しである。The evaluation column in Table 1 is based on the following criteria.

歪二平面上に折シ曲げテスト後の基板をその中央部で該
平面と接触するよう載置したときの、該平面と基板端部
の距離(基板のソリ量)をhとするとき、 h<0.5wxのものを○、 0.3關≦h≦0.5 yntのものをΔ、h > 0
.5 ynのものをXとした。
When the board after the bending test is placed on two distorted planes so that the center part contacts the plane, and the distance between the plane and the edge of the board (the amount of warpage of the board) is h, h ○ for <0.5wx, Δ for 0.3≦h≦0.5 ynt, h > 0
.. 5 yn was designated as X.

密着性二粘着テープを被膜に貼シつけ、ひき剥すビーリ
ングテス)t−行った。使用粘着テープの接着強度は1
0kP/1M2であシ、このテストをサンプル数50で
行ったときの剥れ数が 0のものを○ 〜10のものをΔ 〜1)のものを×とした・ 総合評価二上記の歪及び密着性の評価のいずれか悪い方
を以って総合評価とした。例え ば下記の如くである 歪 密着性 総合評価 XOX Δ     ×        X OΔ   Δ 表1よシ下記1)〜す 1)前処理方法か基板加熱のみでは良好な基板−被膜間
密着性が得られないばかシか、基板に歪を生じる。
A beading test was carried out by applying adhesive tape to the film and peeling it off. The adhesive strength of the adhesive tape used is 1
0kP/1M2, when this test was conducted with 50 samples, those with 0 peeling number were ○, those with ~10 were Δ, and those with ~1) were ×.・Overall evaluation 2 The above distortion and The overall evaluation was based on whichever of the adhesion evaluations was worse. For example, the following strain Adhesion Comprehensive evaluation XOX Δ × Otherwise, the board may be distorted.

2)アルゴンイオンボンバードのみの前処理では、長時
間処理しても安定した密着性は得られず、また、基板に
歪を生じる。
2) Pretreatment using only argon ion bombardment does not provide stable adhesion even after long-term treatment, and also causes distortion in the substrate.

3)水素イオンボンバードのみの前処理では、安定した
密着性ρ;得られない。
3) Stable adhesion ρ cannot be obtained with pretreatment using only hydrogen ion bombardment.

4)本発明によれば、短時間処理で、基板に歪を生じせ
しめる事なく良好な密着性が得られる。
4) According to the present invention, good adhesion can be obtained in a short time without causing distortion to the substrate.

の事実を見出す事ができた。I was able to find out the facts.

尚、本発明を実施するに当り、基板加熱、基板への電子
線照射等を併用することは勿論良い。
Incidentally, in carrying out the present invention, it is of course possible to use substrate heating, electron beam irradiation to the substrate, etc. in combination.

表  1 注)アルゴンボンバード: 5 X 10−3Torr
 DCIKV水素ボンバード:同上 〔発明の効果〕 本発明は、以上詳記したように、金属基板、特に銅着し
くは銅合金からなる基板の表面に不活性ガスのイオンボ
ンバードを行ない然る後に、水素ガスのイオンボンバー
ドを行なうという簡単な操作によシ、基板に歪を生じせ
しむることなく短時間で極めて清浄度の高いクリーニン
グを行うことが可能で、基板と被膜間の密着性を著しく
向上せしめることができる。
Table 1 Note) Argon bombardment: 5 X 10-3 Torr
DCIKV Hydrogen Bombardment: Same as above [Effects of the Invention] As detailed above, the present invention performs ion bombardment of an inert gas on the surface of a metal substrate, particularly a substrate made of copper or a copper alloy, and then performs hydrogen bombardment. The simple operation of ion bombarding the substrate makes it possible to perform extremely clean cleaning in a short period of time without causing distortion to the substrate, significantly improving the adhesion between the substrate and the coating. You can force it.

Claims (3)

【特許請求の範囲】[Claims] (1)金属基板に乾式メッキ法を用いて被膜を施すにあ
たり予め該基板表面を清浄化する前処理方法において、
まず不活性ガスを用いてイオンボンバードを行い、次に
水素ガスを用いてイオンボンバードを行う、ことを特徴
とする前処理方法。
(1) In a pretreatment method for cleaning the surface of a metal substrate before applying a coating using a dry plating method,
A pretreatment method characterized by first performing ion bombardment using an inert gas, and then performing ion bombardment using hydrogen gas.
(2)金属基板が銅もしくは銅合金である特許請求の範
囲第(1)項に記載の前処理方法。
(2) The pretreatment method according to claim (1), wherein the metal substrate is copper or a copper alloy.
(3)乾式メッキ法が物理蒸着法もしくは化学蒸着法で
ある特許請求の範囲第(1)項記載の前処理方法。
(3) The pretreatment method according to claim (1), wherein the dry plating method is a physical vapor deposition method or a chemical vapor deposition method.
JP15986A 1986-01-07 1986-01-07 Pretreatment Pending JPS62158859A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP15986A JPS62158859A (en) 1986-01-07 1986-01-07 Pretreatment

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP15986A JPS62158859A (en) 1986-01-07 1986-01-07 Pretreatment

Publications (1)

Publication Number Publication Date
JPS62158859A true JPS62158859A (en) 1987-07-14

Family

ID=11466257

Family Applications (1)

Application Number Title Priority Date Filing Date
JP15986A Pending JPS62158859A (en) 1986-01-07 1986-01-07 Pretreatment

Country Status (1)

Country Link
JP (1) JPS62158859A (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01253947A (en) * 1988-04-04 1989-10-11 Hitachi Cable Ltd Pretreatment method for lead frame
WO2000029642A1 (en) * 1998-11-17 2000-05-25 Applied Materials, Inc. Removing oxides or other reducible contaminants from a substrate by plasma treatment
US6821571B2 (en) 1999-06-18 2004-11-23 Applied Materials Inc. Plasma treatment to enhance adhesion and to minimize oxidation of carbon-containing layers
DE10320472A1 (en) * 2003-05-08 2004-12-02 Kolektor D.O.O. Plasma treatment for cleaning copper or nickel
US6946401B2 (en) 1998-11-17 2005-09-20 Applied Materials, Inc. Plasma treatment for copper oxide reduction
US7604708B2 (en) 2003-02-14 2009-10-20 Applied Materials, Inc. Cleaning of native oxide with hydrogen-containing radicals
JP2012026038A (en) * 2011-07-21 2012-02-09 Yamaguchi Prefectural Industrial Technology Institute Plasma treatment apparatus and surface treatment method for base material

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01253947A (en) * 1988-04-04 1989-10-11 Hitachi Cable Ltd Pretreatment method for lead frame
WO2000029642A1 (en) * 1998-11-17 2000-05-25 Applied Materials, Inc. Removing oxides or other reducible contaminants from a substrate by plasma treatment
US6734102B2 (en) 1998-11-17 2004-05-11 Applied Materials Inc. Plasma treatment for copper oxide reduction
US6946401B2 (en) 1998-11-17 2005-09-20 Applied Materials, Inc. Plasma treatment for copper oxide reduction
US8183150B2 (en) 1998-11-17 2012-05-22 Applied Materials, Inc. Semiconductor device having silicon carbide and conductive pathway interface
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