JPH0688214A - Vapor deposition plating method - Google Patents
Vapor deposition plating methodInfo
- Publication number
- JPH0688214A JPH0688214A JP24062392A JP24062392A JPH0688214A JP H0688214 A JPH0688214 A JP H0688214A JP 24062392 A JP24062392 A JP 24062392A JP 24062392 A JP24062392 A JP 24062392A JP H0688214 A JPH0688214 A JP H0688214A
- Authority
- JP
- Japan
- Prior art keywords
- vapor deposition
- evaporation
- raw materials
- materials
- amount
- 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.)
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、Ｃｒ，Ｍｇ，Ｍｎ若し
くはそれらの合金等の塑性変形能に劣る難加工性材料を
用いてイオンプレーティングや真空蒸着の様に電子ビー
ム加熱方式による蒸着めっきを行う際、安定して連続的
に操業を行うことのできる蒸着めっき方法に関するもの
である。尚、本発明における難加工性材料とは、塑性変
形能に劣り通常の伸線加工や圧延加工によっては、供給
が容易な線状材、棒状材、板材等の形に加工することが
困難であるものを広く包含する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention uses vapor-deposition plating by electron beam heating such as ion plating or vacuum vapor deposition using a difficult-to-process material such as Cr, Mg, Mn or alloys thereof having poor plastic deformability. The present invention relates to a vapor deposition plating method capable of performing stable and continuous operation when performing. Incidentally, the difficult-to-work material in the present invention is inferior in plastic deformability, and by ordinary wire drawing or rolling, it is difficult to process into a shape such as a linear material, a rod-shaped material, or a plate material which can be easily supplied. Broadly embraces something.
【０００２】[0002]
【従来の技術】真空蒸着めっきを実施するに際しては、
蒸着すべき金属材料を適当な加熱手段を用いて加熱・蒸
発させ、生成した金属蒸気を基材上に凝着させることに
よって蒸着皮膜を形成している。上記加熱手段として
は、電子ビーム加熱，レーザービーム加熱，抵抗加熱，
高周波誘導加熱等様々なものが用いられているが、高い
蒸発速度が得られることや高融点の金属の蒸発が可能で
ある利点を有することから、高出力，高エネルギー密度
を有する電子ビームによる加熱が多用されている。2. Description of the Related Art When performing vacuum deposition plating,
The metal material to be vapor-deposited is heated and vaporized by using an appropriate heating means, and the produced metal vapor is adhered to the substrate to form a vapor-deposited film. As the heating means, electron beam heating, laser beam heating, resistance heating,
Although various materials such as high-frequency induction heating are used, heating with an electron beam having a high output and a high energy density is possible because of the advantages that a high evaporation rate can be obtained and a metal with a high melting point can be evaporated. Is often used.
【０００３】ところで真空中で上記の加熱手段によって
金属材料を加熱・蒸発させる場合、純Ａｌ，純Ｚｎ等の
金属材料の融点は、蒸気圧が十分に高められる温度より
もかなり低いので、通常の実施手段としては、るつぼ等
の原料槽内でまず金属材料を溶融し、更に昇温すること
によって当該溶融金属浴の表面から金属原子を蒸発させ
ていく。従って蒸発有効面積は溶融金属浴の表面積で決
まり、高真空下における蒸発量は熱エネルギーによって
一義的にコントロールすることができる。By the way, when a metal material is heated and vaporized by the above heating means in vacuum, the melting point of the metal material such as pure Al and pure Zn is considerably lower than the temperature at which the vapor pressure is sufficiently increased, and therefore, it is usual. As an implementation means, first, a metal material is melted in a raw material tank such as a crucible, and further heated to evaporate metal atoms from the surface of the molten metal bath. Therefore, the effective evaporation area is determined by the surface area of the molten metal bath, and the evaporation amount under high vacuum can be uniquely controlled by thermal energy.
【０００４】このように蒸着法は幅広い分野で応用され
ている技術であり、純Ａｌ、純Ｚｎ等の材料では既に連
続生産が実用化されている。言うまでもなく、このよう
な連続生産においては、長期にわたって安定した蒸発量
を確保するために蒸発によって減少する蒸着原料の補給
が必要であるが、これらの金属は加工が容易で且つ電子
ビーム加熱により容易に溶融浴を形成するので、蒸着原
料をワイヤー状に加工する等の方法によって蒸発槽への
原料供給が比較的容易に行なえる。また補給速度の調整
も、蒸着原料の減少速度を計測し、ワイヤーを送給する
ピンチローラー等の回転速度にフィードバックさせる方
法などにより容易に行なえる。As described above, the vapor deposition method is a technique applied in a wide range of fields, and continuous production has already been put into practical use for materials such as pure Al and pure Zn. Needless to say, in such continuous production, it is necessary to replenish the evaporation raw materials that decrease due to evaporation in order to secure a stable evaporation amount over a long period of time, but these metals are easy to process and easy to electron beam heat. Since the melting bath is formed in the above, the raw material can be supplied to the evaporation tank relatively easily by a method such as processing the vapor deposition raw material into a wire shape. Also, the replenishment speed can be easily adjusted by a method of measuring the decrease rate of the vapor deposition material and feeding it back to the rotation speed of a pinch roller or the like for feeding the wire.
【０００５】しかし、塑性加工が難しい難加工性材料を
溶融浴に供給する場合には、原料補給が容易な形状に蒸
着原料を加工することが困難であり、蒸着原料の供給機
構の上で大きな制約を受ける。また特殊なプロセスを用
いて蒸着原料の加工を行なう場合にはそのためのコスト
上昇が問題となってくる。However, when a difficult-to-process material that is difficult to plastically process is supplied to the melting bath, it is difficult to process the vapor deposition material into a shape in which the raw material can be easily replenished. Be restricted. Further, when the vapor deposition material is processed by using a special process, the cost increase for that purpose becomes a problem.
【０００６】一方、難加工性材料のなかでも、ＣｒやＭ
ｇ等の昇華性金属は、安定した原料供給を行なった場合
においても、その蒸発量の安定性が問題となる。即ちこ
れら昇華性金属は、高真空条件の下では当該金属の融点
未満の温度でも高い蒸気圧を示すので、熱エネルギーを
加えた場合、溶融の始まっていない蒸着原料表面からの
蒸発が進行する。このときは蒸着原料表面全体が蒸発有
効面積となり、該蒸発有効面積は金属材料の比表面積に
よって著しく変わってくるばかりでなく、蒸発の進行に
伴って蒸着原料が小さくなるにつれて該蒸発有効面積は
経時的に変化する。従って加える熱エネルギーを一定に
保っても、単位面積当たりの投入エネルギー量、即ちパ
ワー密度が変化するため、総金属材料表面からの総蒸発
量を一定に維持することは困難である。また加熱源であ
る電子ビームの入射角度が蒸着原料形状の変化と共に変
動するために、電子ビームの吸収効率が変化して蒸着原
料表面温度も変動するという問題点を抱えている。On the other hand, among difficult-to-process materials, Cr and M
Sublimable metals such as g have a problem in the stability of the amount of evaporation even when a stable raw material is supplied. That is, since these sublimable metals show a high vapor pressure even under a temperature lower than the melting point of the metal under high vacuum conditions, when heat energy is applied, evaporation from the surface of the vapor deposition material where melting has not started progresses. At this time, the entire surface of the evaporation material becomes the evaporation effective area, and the evaporation effective area not only significantly changes depending on the specific surface area of the metal material, but also the evaporation effective area changes with time as the evaporation material becomes smaller as the evaporation progresses. Change. Therefore, even if the applied heat energy is kept constant, it is difficult to keep the total amount of evaporation from the surface of the total metal material constant because the amount of input energy per unit area, that is, the power density changes. Further, since the incident angle of the electron beam, which is a heating source, changes with the change of the shape of the vapor deposition material, there is a problem that the absorption efficiency of the electron beam changes and the surface temperature of the vapor deposition material also varies.
【０００７】上記の様な昇華性材料蒸着の問題点を解決
する方法として、合金化することによってより低い温度
で溶融浴化するようになる元素を昇華性材料に添加して
合金浴状態からの蒸着を可能にする技術（特開昭62-208
65号公報）等が提唱されている。例えば、昇華性材料で
あるＣｒを蒸着する場合、Ｚｒと合金させることによっ
て溶融Ｚｒ−Ｃｒ合金浴の状態からのＣｒ蒸着が可能と
なる。この方法によれば、蒸発面は常にフラットな溶融
面となり、蒸着原料形状の変化の問題を解決することが
できる。As a method for solving the above problems of vapor deposition of a sublimable material, an element capable of forming a molten bath at a lower temperature by alloying is added to a sublimable material to remove the element from the alloy bath state. Technology that enables vapor deposition (JP-A-62-208)
No. 65) is proposed. For example, when Cr, which is a sublimable material, is vapor-deposited, alloying with Zr makes it possible to vapor-deposit Cr from the state of a molten Zr—Cr alloy bath. According to this method, the evaporation surface is always a flat melting surface, and it is possible to solve the problem of the change in the shape of the vapor deposition material.
【０００８】[0008]
【発明が解決しようとする課題】このように、塑性変形
能に劣る難加工性材料のうち、昇華性材料に固有の、電
子ビームによって加熱される蒸発面形状が変化するとい
う問題に関しては種々の技術開発が行なわれているが、
原料供給を安定化するという問題は未解決であった。As described above, among the difficult-to-work materials having poor plastic deformability, there are various problems inherent to sublimable materials such that the shape of the evaporation surface heated by the electron beam changes. Technology is being developed,
The problem of stabilizing the supply of raw materials has not been solved.
【０００９】本発明は以上の様な状況に鑑みてなされた
ものであって、その目的は、難加工性材料を蒸着原料と
して用いた場合に、安定して原料を供給し操業しうるよ
うな蒸着めっき方法を提供しようとするものである。The present invention has been made in view of the above circumstances, and an object thereof is to stably supply a raw material when a difficult-to-process material is used as a vapor deposition raw material. It is intended to provide a vapor deposition plating method.
【００１０】[0010]
【課題を解決するための手段】上記課題を解決すること
のできた本発明の蒸着めっき方法は、電子ビーム加熱方
式により、少なくとも１種類の難加工性材料を含む蒸着
原料を用いて連続的に蒸着めっきを施すにあたり、該蒸
着原料の溶融浴に補給される該難加工性材料を、粉状、
粒状若しくは塊状体とし、且つ粒径１mm未満のものを５
重量％以下として操業することに要旨を有する。The vapor deposition plating method of the present invention, which has been able to solve the above-mentioned problems, continuously vapor-deposits a vapor deposition raw material containing at least one kind of difficult-to-process material by an electron beam heating method. In applying the plating, the difficult-to-process material supplied to the molten bath of the vapor deposition raw material is powdered,
Granular or agglomerate with a particle size of less than 1 mm 5
It has the gist of operating at a weight percent or less.
【００１１】[0011]
【作用】本発明において蒸着される対象となる被処理材
は特に限定されず、金属の他プラスチック、紙等の非金
属等いずれにも適用される。またその形状も限定される
ものではなく、板状、波板状、棒状管状、線状等いずれ
であってもよい。The material to be vapor-deposited in the present invention is not particularly limited, and may be applied to any metal such as plastic and non-metal such as paper. Further, the shape thereof is not limited, and may be any of a plate shape, a corrugated plate shape, a rod-like tube shape, a linear shape and the like.
【００１２】尚、本発明における塑性変形能に劣る難加
工性材料とは、ワイヤ状等への加工の困難な材料を広く
包含し、例えばＣｒ，Ｍｇ等の昇華性金属もしくはそれ
らの合金の他、ＳｉＯ2 ，Ａ2 Ｏ3 などの酸化物系のセ
ラミックス等が挙げられる。The hard-to-work material having poor plastic deformability in the present invention includes a wide range of hard-to-work materials, such as sublimable metals such as Cr and Mg or alloys thereof. , Oxide-based ceramics such as SiO 2 , A 2 O 3 and the like.
【００１３】以下発明の経緯に沿って本発明を詳述す
る。まず本発明においては、蒸着原料を溶融浴化する必
要がある。これは上記で述べた通り、蒸発面を常に一定
のフラットな溶融面とすることによって昇華性材料にお
ける蒸発量変動の問題を回避して安定した蒸発量を確保
し、高精度の付着量制御を行なうためである。以下、溶
融浴状態の蒸着原料への原料補給を前提として説明す
る。The present invention will be described in detail below along with the background of the invention. First, in the present invention, it is necessary to form the vapor deposition material into a molten bath. As mentioned above, this is to ensure a stable evaporation amount by avoiding the problem of evaporation amount fluctuation in sublimable materials by always making the evaporation surface a constant and flat melting surface, and to control the adhesion amount with high accuracy. This is to do it. Hereinafter, description will be made on the premise that the raw material is replenished to the vapor deposition raw material in the molten bath state.
【００１４】原料補給の方法を検討するにあたり、本発
明者らはまず、図１に示す装置を用いて粉末状材料の補
給を試みた。粉末状を選んだ理由は、特に活性な金属で
酸化による自己発熱を起こす恐れのある材料以外は、塑
性変形能に劣る材料であっても適当な粒度の粉末にして
使用することは可能であり、また材料の入手も容易に行
なえるためである。In examining the method of replenishing the raw materials, the present inventors first tried to replenish the powdery material using the apparatus shown in FIG. The reason why the powder form is selected is that it is possible to use a powder having an appropriate particle size even if the material has poor plastic deformability, except for a material that may cause self-heating due to oxidation, especially with an active metal. This is also because the materials can be easily obtained.
【００１５】その結果、以下のような問題点が判明し
た。即ち溶融浴表面は電子ビームにより高温に加熱され
ているが、その状態で粉末状の材料を供給したところ溶
融浴表面に粉末状材料が浮遊して流れ、粉末が溶融する
までの間溶融浴表面を覆う現象が観察された。また、電
子ビームを照射している場所に浮遊粉末材料が流れる
と、粉末状材料が急激に過度に加熱されて飛散する、ス
プラッシュと呼ばれる現象が激しく発生した。これらの
現象のメカニズムは明らかではないが、供給直後の粉末
状材料が溶融浴と濡れるまでにある程度の時間を要する
ためではないかと考えている。As a result, the following problems have been found. That is, the surface of the molten bath is heated to a high temperature by the electron beam, but when a powdered material is supplied in that state, the powdered material flows and floats on the surface of the molten bath until the powder melts. A phenomenon was observed to cover the. Further, when the floating powder material flows to the place where the electron beam is irradiated, a phenomenon called splash, in which the powder material is rapidly heated excessively and scattered, has occurred violently. Although the mechanism of these phenomena is not clear, it is thought that it may take some time before the powdered material immediately after being supplied gets wet with the melting bath.
【００１６】粉末状材料が溶融浴表面を覆うと実蒸発面
積が減少するために、蒸発量の減少をもたらす。またス
プラッシュの発生は製品表面に付着した場合に重大な品
質上の欠陥をもたらす。従って、溶融浴に供給する材料
は供給される溶融浴表面に浮遊して広がらないだけの十
分な大きさを必要とすることが明らかとなった。When the powdered material covers the surface of the molten bath, the actual evaporation area is reduced, resulting in a decrease in evaporation amount. Also, the generation of splash causes a serious quality defect when it adheres to the product surface. Therefore, it became clear that the material supplied to the molten bath needs to have a size large enough so as not to float and spread on the surface of the supplied molten bath.
【００１７】次に本発明者らは、供給材料の粒径に着目
して材料供給実験を行い、粒径が１mm未満の粉状もしく
は粒状材料がこのような浮遊現象を起こしやすいことを
見いだした。しかし、粉状、粒状もしくは塊状の材料か
ら、粒径が１mm未満のものを完全に除去することは困難
であり、供給材料の取扱い時に新たに発生することも考
えられる。そこで、本発明者らは、粒径が１mm未満の粉
状、粒状もしくは塊状の材料をどの程度まで供給される
原料中に含有することができるのかという観点から鋭意
研究開発を行い、粒径が１mm未満の粉状、粒状もしくは
塊状材の割合を５重量％未満、より望ましくは３重量％
未満とすることにより、このような供給材料の浮遊現象
を実用上問題とならないレベルに抑制できることを見い
だし、本発明を完成させた。ここで述べた粒径とは、例
えばＪＩＳ Ｚ8801において規定されるような標準ふる
いにて分別されるものを意味している。Next, the present inventors conducted a material supply experiment focusing on the particle size of the supplied material and found that a powdery or granular material having a particle size of less than 1 mm is likely to cause such a floating phenomenon. . However, it is difficult to completely remove powdery, granular, or lumpy materials having a particle size of less than 1 mm, and it is considered that new generation occurs when the feed material is handled. Therefore, the inventors of the present invention have conducted earnest research and development from the viewpoint of how much powdery, granular, or lumpy material having a particle size of less than 1 mm can be contained in the raw material to be supplied. Less than 5% by weight of powdery, granular or lump material less than 1 mm, more preferably 3% by weight
It was found that such a floating phenomenon of the feed material can be suppressed to a level not causing a problem in practice by setting the content to be less than the above, and the present invention has been completed. The particle size described here means that the particles are sorted by a standard sieve as specified in JIS Z8801, for example.
【００１８】理想的には、粒径が１mm未満の粉状、粒状
もしくは塊状材を含有しない材料を供給原料として用い
るべきであるが、工程上及びコスト上の困難が伴う。そ
こでその割合を上述のように制限することにより、スプ
ラッシュ発生及び蒸発量の変動ともに無視できる量に減
少させることが可能であることを見出したものである。
また、粒径１mm未満の粉状もしくは粒状材の減少させた
ことにより、比較的活性な金属を供給する場合において
も取扱いが容易になり、保管中の自然発火の危険性が減
少するなどの複次的な効果も期待できる。Ideally, a material having a particle size of less than 1 mm and containing no powdery, granular, or agglomerate material should be used as a feed material, but this is difficult in terms of process and cost. Therefore, the inventors have found that by limiting the ratio as described above, it is possible to reduce both the generation of splash and the fluctuation of the evaporation amount to a negligible amount.
In addition, by reducing the amount of powdery or granular material with a particle size of less than 1 mm, handling becomes easier even when supplying a relatively active metal, and the risk of spontaneous ignition during storage is reduced. The next effect can be expected.
【００１９】尚蒸着原料が複数の元素からなる合金浴で
ある場合には、供給原料の比重が合金浴の比重以上であ
ることが必須条件であり、合金浴の比重を下回る場合に
は、供給された材料が本発明で規定する条件を満たすも
のであっても供給された原料が溶融するまでの間に浮遊
する現象が生じる。その結果蒸発量の変動やスプラッシ
ュの発生を来す恐れがある。When the vapor deposition raw material is an alloy bath composed of a plurality of elements, it is essential that the specific gravity of the feed raw material is equal to or higher than the specific gravity of the alloy bath. Even if the supplied material satisfies the conditions specified in the present invention, a phenomenon occurs in which the supplied raw material floats before melting. As a result, the amount of evaporation may fluctuate and a splash may occur.
【００２０】ところで粒径は、特に供給装置から生じる
問題がない限り上述の規定を満たす範囲内で小さい方が
好ましいと考えることができる。即ち、溶融浴量と比較
して過大な原料を一度に供給する場合には、供給サイク
ルを長くする必要があるために、蒸発による溶融浴量の
減少及び原料供給による溶融浴量の増加によって起こる
溶融浴面高さや浴組成の変動が増加し、それに伴って蒸
発量や蒸気組成の変動も増加する傾向が見られる。ま
た、溶融浴が合金浴である場合には、合金浴表面の合金
組成が変動して各合金元素の蒸発量が変動する結果得ら
れる皮膜の組成が安定しないという影響が現れる。逆
に、粒径が上述の規定を満たす範囲内で小さい場合に
は、単位時間当たりの供給量を細かく制御することが可
能であり、その結果単位時間当たりの溶湯浴面高さの変
動量、合金浴表面の合金組成の変動量を抑えることが比
較的容易となる。By the way, it can be considered that the particle size is preferably as small as possible within the range satisfying the above-mentioned requirements unless there is a problem caused by the supply device. That is, when an excessively large amount of raw material is supplied at one time as compared with the amount of the molten bath, it is necessary to lengthen the supply cycle, so that the amount of the molten bath decreases due to evaporation and the amount of the molten bath increases due to the supply of the raw material. There is a tendency that the height of the molten bath and the composition of the bath increase, and the fluctuations of the evaporation amount and the vapor composition also increase. Further, when the melting bath is an alloy bath, the alloy composition on the surface of the alloy bath fluctuates, and the evaporation amount of each alloying element fluctuates. As a result, the composition of the resulting coating is not stable. On the contrary, when the particle size is small within the range satisfying the above-mentioned regulation, it is possible to finely control the supply amount per unit time, and as a result, the variation amount of the molten metal bath surface height per unit time, It becomes relatively easy to suppress the fluctuation amount of the alloy composition on the surface of the alloy bath.
【００２１】蒸発量の変動が無視できない量になる供給
原料の大きさの上限は、溶融浴を保持する蒸発槽の構
造、溶融浴の加熱に用いる電子ビームの出力、蒸発槽内
における原料の供給位置と電子ビーム加熱を行なってい
る領域の関係等供給原料以外の要因が複雑に影響してい
るために供給原料に関することだけで一義的に規定する
ことはできない。しかし本発明者らの供給実験結果か
ら、溶融浴量との比較において１回に供給される供給原
料の重量を溶湯量の３重量％以内、より望ましくは１重
量％以内に抑えることが好ましいと考えられる。The upper limit of the size of the feed material that causes the fluctuation of the evaporation amount to be a non-negligible amount is the structure of the evaporation tank holding the melting bath, the output of the electron beam used for heating the melting bath, the supply of the raw material in the evaporation tank. Since the factors other than the feed material such as the relationship between the position and the region where the electron beam heating is performed have complicated influences, it is not possible to unambiguously specify only the feed material. However, from the results of the feed experiment conducted by the present inventors, it is preferable that the weight of the feed material fed at one time in comparison with the amount of the molten bath is kept within 3 wt% of the amount of the molten metal, and more desirably within 1 wt%. Conceivable.
【００２２】本発明で用いる難加工性材料の製法は、ア
トマイズ法、焼結法、溶解材あるいは焼結材の粉砕等、
様々な方法が考えられるが、特にその製法により蒸着原
料表面に厚い酸化皮膜が形成されたり、不純物元素や固
溶ガスが大量に混入する等の劣悪な材料になるものでな
い限り制限されない。The manufacturing method of the difficult-to-process material used in the present invention includes atomizing method, sintering method, crushing of melted material or sintered material, and the like.
Various methods are conceivable, but the method is not particularly limited as long as a thick oxide film is formed on the surface of the vapor deposition material and a large amount of an impurity element or a solid solution gas is mixed, which is a poor material.
【００２３】また、本発明において規定した以外の蒸着
条件も特に制限されるものではなく、原料の溶融浴への
供給方法も溶融浴面上の電子ビームが照射されている領
域に直接原料を供給する等の本発明の趣旨に明らかに反
する方法を採用しない限り、特に制限されない。Further, the vapor deposition conditions other than those specified in the present invention are not particularly limited, and the method of supplying the raw material to the molten bath is such that the raw material is directly supplied to the region irradiated with the electron beam on the surface of the molten bath. The method is not particularly limited as long as a method that clearly violates the gist of the present invention is not adopted.
【００２４】本発明における蒸着原料としては、難加工
性材料を少なくとも１種類以上含むものであればよく、
他の成分は特に限定されない。例えば難加工性材料以外
にＡｌ，Ｚｎ，Ｃｒ，Ｔｉ等の金属もしくはそれらの合
金を含むものであっても勿論構わない。また難加工性材
料以外の蒸着原料の供給方法も特に限定されないが、ワ
イヤー状等に加工して供給する方法が供給量のコントロ
ールの点から好ましい。As the vapor deposition raw material in the present invention, any material may be used as long as it contains at least one kind of hardly workable material.
Other components are not particularly limited. For example, in addition to the hard-to-process material, a metal such as Al, Zn, Cr, or Ti or an alloy thereof may be included. The method of supplying the vapor deposition material other than the hard-to-process material is not particularly limited, but a method of processing it into a wire shape and supplying the same is preferable from the viewpoint of controlling the supply amount.
【００２５】以下に実施例を挙げて本発明を更に詳細に
説明するが、下記実施例は本発明を制限するものではな
く、前・後記の趣旨を逸脱しない範囲で変更実施するこ
とは全て本発明の技術的範囲に包含される。The present invention will be described in more detail with reference to the following examples, but the following examples are not intended to limit the present invention, and any changes or modifications made within the scope not departing from the gist of the preceding and the following will be covered by the present invention. It is included in the technical scope of the invention.
【００２６】[0026]
【実施例】図１に示す装置を用いて各種蒸着原料を供給
し、蒸着めっきを行った。なお、合金浴の場合には本発
明で規定する難加工性の蒸着原料以外の合金元素はワイ
ヤーの状態で供給した。また、難加工性の蒸着原料は、
ＪＩＳ Ｚ8801に規定される標準ふるいにより選別し
た。 ＜実験条件＞ 被処理材 ：Ａｌキルド鋼帯 蒸着室真空度 ：10-2 Ｐａ以下 蒸着材料の加熱源：電子ビーム 電子線出力 ：10〜70 KW 蒸発槽 ：セラミックス製るつぼEXAMPLES Various vapor deposition materials were supplied using the apparatus shown in FIG. 1 to perform vapor deposition plating. In the case of the alloy bath, the alloying elements other than the difficult-to-work vapor deposition material specified in the present invention were supplied in the state of a wire. In addition, the difficult-to-process evaporation material is
It was selected by a standard sieve specified in JIS Z8801. <Experimental conditions> Material to be treated: Al-killed steel strip Deposition degree in deposition chamber: 10 -2 Pa or less Heating source of deposition material: Electron beam Electron beam output: 10 to 70 KW Evaporation tank: Ceramic crucible
【００２７】＜評価項目＞ (1) スプラッシュ発生量 目視観察による ◎ 発生無し ○ 極少量の発生 × 発生 (2) 付着量の変動量 １供給サイクル間の付着量変動量を測定 ○ １g/m2未満 △ １〜２g/m2 × ２g/m2超<Evaluation items> (1) Splash generation amount Visual observation ◎ No generation ○ Very small amount generation × Occurrence (2) Fluctuation of adhesion amount 1 Measure fluctuation amount of adhesion amount during one supply cycle ○ 1 g / m 2 Less than △ 1-2 g / m 2 × more than 2 g / m 2
【００２８】[0028]
【表１】 [Table 1]
【００２９】表１のＮo.１〜18に示すように、本発明の
方法により、連続した材料供給を行うとともにスプラッ
シュの発生を抑制し安定した蒸発量を確保することが可
能となる。なお、Ｎo.６、18に示すように過大な供給材
料を用いた場合には、スプラッシュの発生には影響しな
いものの付着量の変動を起こす。一方、Ｎo.19〜23に示
すように本発明の請求範囲を超える割合で粒径１mm未満
の材料を含有している場合には、溶湯表面に浮遊する粉
状もしくは粒状材料の影響が無視できないものとなり、
スプラッシュの発生、付着量の変動等の悪影響が顕著に
なる。As shown in Nos. 1 to 18 of Table 1, by the method of the present invention, it is possible to continuously supply the material and suppress the generation of splash to secure a stable evaporation amount. In addition, as shown in Nos. 6 and 18, when an excessively large amount of the feed material is used, the amount of the adhering amount fluctuates although it does not affect the generation of splash. On the other hand, as shown in Nos. 19 to 23, when a material having a particle diameter of less than 1 mm is contained in a ratio exceeding the claimed range of the present invention, the influence of powdery or granular material floating on the surface of the molten metal cannot be ignored. Become a thing,
The adverse effects such as the occurrence of splash and the variation of the adhered amount become remarkable.
【００３０】[0030]
【発明の効果】本発明は、以上のように構成されてお
り、難加工性材料を蒸着原料として用いた場合、蒸発速
度の安定化を図り安定した連続蒸着が可能となる蒸着め
っき方法が得られた。EFFECTS OF THE INVENTION The present invention is configured as described above, and when a difficult-to-process material is used as a vapor deposition material, a vapor deposition plating method that stabilizes the evaporation rate and enables stable continuous vapor deposition is obtained. Was given.
【図１】本発明の蒸着めっき方法で用いる装置の一例を
示す概略図である。FIG. 1 is a schematic view showing an example of an apparatus used in the vapor deposition plating method of the present invention.
１ 被処理材 ２ 電子銃 ３ 電子ビーム ４ 蒸着原料溶融域 ５ 蒸発槽 ６ 蒸着原料 ７ バイブレーター ８ ガイドレール 1 Material to be treated 2 Electron gun 3 Electron beam 4 Evaporation material melting area 5 Evaporation tank 6 Evaporation material 7 Vibrator 8 Guide rail
───────────────────────────────────────────────────── フロントページの続き (72)発明者 綾部 東太 兵庫県加古川市金沢町１番地 株式会社神 戸製鋼所加古川製鉄所内 (72)発明者 加藤 淳 兵庫県加古川市金沢町１番地 株式会社神 戸製鋼所加古川製鉄所内 (72)発明者 三宅 昭二 兵庫県加古川市金沢町１番地 株式会社神 戸製鋼所加古川製鉄所内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Tota Ayabe 1 Kanazawa Town, Kakogawa City, Hyogo Prefecture Kamido Steel Works, Ltd. Inside the Kakogawa Steel Works (72) Atsushi Kato 1 Kanazawa Town, Kakogawa City, Hyogo Prefecture Kamizawa Co., Ltd. Toko Works Kakogawa Works (72) Inventor Shoji Miyake 1 Kanazawa-cho, Kakogawa City, Hyogo Prefecture Kadodo Works Kakogawa Works
Claims (1)
１種類の難加工性材料を含む蒸着原料を用いて連続的に
蒸着めっきを施すにあたり、該蒸着原料の溶融浴に補給
される該難加工性材料を、粉状、粒状若しくは塊状体と
し、且つ粒径１mm未満のものを５重量％以下として操業
することを特徴とする蒸着めっき方法。1. A refractory material that is replenished in a molten bath of the vapor deposition material when continuously performing vapor deposition plating using a vapor deposition material containing at least one kind of the refractory material by an electron beam heating method. In the form of powder, granules or agglomerates and having a particle size of less than 1 mm at 5% by weight or less.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24062392A JPH0688214A (en) | 1992-09-09 | 1992-09-09 | Vapor deposition plating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24062392A JPH0688214A (en) | 1992-09-09 | 1992-09-09 | Vapor deposition plating method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0688214A true JPH0688214A (en) | 1994-03-29 |
Family
ID=17062252
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP24062392A Withdrawn JPH0688214A (en) | 1992-09-09 | 1992-09-09 | Vapor deposition plating method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0688214A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6291031B1 (en) * | 1998-01-27 | 2001-09-18 | Matsushita Electric Industrial Co., Ltd. | Method for preparing optical recording medium and preparation apparatus therefor |
| JP2009235563A (en) * | 2008-03-03 | 2009-10-15 | Toho Titanium Co Ltd | Vapor-deposition material of metal oxide, production method therefor, and method for producing vapor-deposition film of metal oxide |
| WO2016198394A1 (en) * | 2015-06-08 | 2016-12-15 | Te Connectivity Germany Gmbh | Electrical contact element and method for altering mechanical and/or electrical properties of at least one area of such |
-
1992
- 1992-09-09 JP JP24062392A patent/JPH0688214A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6291031B1 (en) * | 1998-01-27 | 2001-09-18 | Matsushita Electric Industrial Co., Ltd. | Method for preparing optical recording medium and preparation apparatus therefor |
| JP2009235563A (en) * | 2008-03-03 | 2009-10-15 | Toho Titanium Co Ltd | Vapor-deposition material of metal oxide, production method therefor, and method for producing vapor-deposition film of metal oxide |
| WO2016198394A1 (en) * | 2015-06-08 | 2016-12-15 | Te Connectivity Germany Gmbh | Electrical contact element and method for altering mechanical and/or electrical properties of at least one area of such |
| CN107710511A (en) * | 2015-06-08 | 2018-02-16 | 泰连德国有限公司 | Electrical contact element and mechanical and/or electrical property the method for changing its at least one region |
| US10777912B2 (en) | 2015-06-08 | 2020-09-15 | Te Connectivity Germany Gmbh | Electrical contact element and method for altering mechanical and/or electrical properties of at least one area of such |
| CN107710511B (en) * | 2015-06-08 | 2021-07-20 | 泰连德国有限公司 | Electrical contact element and method for modifying the mechanical and/or electrical properties of at least one region of an electrical contact element |
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