JP2006183098A - Method for forming vapor deposition film - Google Patents

Method for forming vapor deposition film Download PDF

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JP2006183098A
JP2006183098A JP2004378205A JP2004378205A JP2006183098A JP 2006183098 A JP2006183098 A JP 2006183098A JP 2004378205 A JP2004378205 A JP 2004378205A JP 2004378205 A JP2004378205 A JP 2004378205A JP 2006183098 A JP2006183098 A JP 2006183098A
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vapor deposition
processed
cylindrical barrel
deposited
vapor
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JP4483574B2 (en
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Yoshio Fujiwara
好雄 藤原
Nobuhiro Misumi
信弘 三角
Fumitaka Asakura
文隆 朝倉
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Hitachi Metals Ltd
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Neomax Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for efficiently forming a vapor deposition film even on the surface of a large-size article to be treated, while preventing the article from causing chipping and the deposited film from exfoliating. <P>SOLUTION: An apparatus for forming the vapor deposition film has a section for evaporating a vapor deposition material, and a cylindrical barrel having a porous peripheral surface for accommodating the article on the surface of which the vapor deposition material is vapor-deposited, in a vacuum treatment chamber. The cylindrical barrel is laterally installed and rotates around a horizontal axis of rotation. The method for forming the vapor deposition film includes vapor-depositing the vapor deposition material on the surface of the article with the use of the apparatus, through (1) accommodating many articles and many metal spring members in the cylindrical barrel, or through (2) accommodating many articles in a cylindrical barrel having a metal spring installed so as to keep tension. <P>COPYRIGHT: (C)2006,JPO&NCIPI

Description

本発明は、希土類系永久磁石などの被処理物の表面にアルミニウムなどの蒸着被膜を形成する方法に関する。   The present invention relates to a method for forming a deposited film such as aluminum on the surface of an object to be processed such as a rare earth permanent magnet.

Ｎｄ−Ｆｅ−Ｂ系永久磁石に代表されるＲ−Ｆｅ−Ｂ系永久磁石などの希土類系永久磁石は、高い磁気特性を有しており、今日様々な分野で使用されている。しかしながら、希土類系永久磁石は、大気中で酸化腐食されやすい金属種（特にＲ）を含む。それ故、表面処理を行わずに使用した場合には、わずかな酸やアルカリや水分などの影響によって表面から腐食が進行して錆が発生し、それに伴って、磁気特性の劣化やばらつきを招くことになる。さらに、磁気回路などの装置に組み込んだ磁石に錆が発生した場合、錆が飛散して周辺部品を汚染する恐れがある。以上の点に鑑み、希土類系永久磁石に優れた耐食性を付与することを目的として、その表面にアルミニウムや亜鉛などの金属蒸着被膜を形成することが行われている。特に、アルミニウム被膜は、耐食性や量産性に優れていることに加え、部品組み込み時に必要とされる接着剤との接着信頼性に優れている（接着剤が本質的に有する破壊強度に達するまでに被膜と接着剤との間で剥離が生じにくい）ので、強い接着強度が要求される希土類系永久磁石に対しても広く適用されている。   Rare earth permanent magnets such as R-Fe-B permanent magnets represented by Nd-Fe-B permanent magnets have high magnetic properties and are used in various fields today. However, rare earth-based permanent magnets contain metal species (particularly R) that are susceptible to oxidative corrosion in the atmosphere. Therefore, when used without surface treatment, corrosion progresses from the surface due to the influence of slight acid, alkali, moisture, etc., and rust is generated, resulting in deterioration and dispersion of magnetic properties. It will be. Furthermore, when rust is generated in a magnet incorporated in a device such as a magnetic circuit, the rust may be scattered and contaminate peripheral components. In view of the above points, for the purpose of imparting excellent corrosion resistance to rare earth-based permanent magnets, forming a metal vapor-deposited film such as aluminum or zinc on the surface thereof has been performed. In particular, the aluminum coating has excellent corrosion resistance and mass productivity, as well as excellent adhesion reliability with the adhesive required when assembling parts (by reaching the fracture strength inherent to the adhesive). Therefore, it is also widely applied to rare earth permanent magnets that require high adhesive strength.

希土類系永久磁石の表面に金属蒸着被膜を形成するために使用される、真空処理室内に、蒸着材料の蒸発部と、その表面に蒸着材料が蒸着される被処理物を収容するための多孔性周面を有する筒型バレルを備え、筒型バレルを横設して水平方向の回転軸線を中心に回転させながら被処理物の表面に蒸着材料を蒸着させる蒸着被膜形成装置としては、例えば、特許文献１に記載の装置がある。図１は、その一例の、図略の真空排気系に連なる真空処理室１の内部の模式的正面図（一部透視図）である。その室内上方には、水平方向の回転軸線上の回転シャフト６を中心に回転自在とした支持部材７が２個併設されており、この支持部材７の回転シャフト６の周方向の外方に６個のステンレス製のメッシュ金網で形成された円筒形バレル５が支持軸８によって公転自在に環状に支持されている（図２は円筒形バレル５の一例を示す模式的斜視図であり、図３は支持部材７に支持された円筒形バレル５の一例を示す模式的斜視図である）。また、その室内下方には、蒸着材料であるアルミニウムを蒸発させる蒸発部であるボート２が、支持テーブル３上に立設されたボート支持台４上に複数個配置されている。支持テーブル３の下方内部には、蒸着材料であるアルミニウムのワイヤー９が繰り出しリール１０に巻回保持されている。アルミニウムワイヤー９の先端はボート２の内面に向かって臨ませた耐熱性の保護チューブ１１によってボート２の上方に案内されている。保護チューブ１１の一部には切り欠き窓１２が設けられており、この切り欠き窓１２に対応して設けられた繰り出しギア１３がアルミニウムワイヤー９に直接接触し、アルミニウムワイヤー９を繰り出すことによってボート２内にアルミニウムが絶えず供給されるように構成されている。そして、この装置によれば、被処理物である希土類系永久磁石３０を円筒形バレル５内に多数収容し、矢示のごとく回転シャフト６を中心に支持部材７を回転させると、支持部材７の回転シャフト６の周方向の外方に支持軸８によって支持されている円筒形バレル５は、これに対応して、回転シャフト６を中心に公転運動し、図略の加熱手段によって所定温度に加熱されたボート２から蒸発させたアルミニウムが、円筒形バレル５内の希土類永久磁石３０の表面に蒸着され、アルミニウム被膜が形成される。
特開２００１−３３５９２１号公報 Porous to house the evaporation part of the evaporation material and the object to be evaporated on the surface in the vacuum processing chamber, which is used to form a metal evaporation film on the surface of the rare earth permanent magnet For example, as a vapor deposition film forming apparatus that includes a cylindrical barrel having a peripheral surface, deposits a vapor deposition material on the surface of an object to be processed while rotating the horizontal barrel about the horizontal barrel axis, for example, a patent There is a device described in Document 1. FIG. 1 is a schematic front view (partially perspective view) of the inside of a vacuum processing chamber 1 connected to an unillustrated evacuation system, as an example. Two support members 7 that are rotatable about a rotation shaft 6 on a horizontal rotation axis are provided in the upper part of the room, and the support member 7 has 6 on the outer side in the circumferential direction of the rotation shaft 6. A cylindrical barrel 5 formed of a stainless steel mesh wire mesh is supported in an annular manner by a support shaft 8 so as to revolve freely (FIG. 2 is a schematic perspective view showing an example of the cylindrical barrel 5, FIG. Is a schematic perspective view showing an example of a cylindrical barrel 5 supported by a support member 7). A plurality of boats 2, which are evaporation sections for evaporating aluminum as a deposition material, are arranged on a boat support base 4 erected on a support table 3 below the room. Inside the support table 3, an aluminum wire 9 as a vapor deposition material is wound and held on a supply reel 10. The tip of the aluminum wire 9 is guided above the boat 2 by a heat-resistant protective tube 11 facing the inner surface of the boat 2. A cutout window 12 is provided in a part of the protective tube 11, and a feeding gear 13 provided corresponding to the cutout window 12 is in direct contact with the aluminum wire 9, and the aluminum wire 9 is fed out so that the boat is The aluminum is constantly supplied into the interior 2. According to this apparatus, when a large number of rare earth permanent magnets 30 as objects to be processed are accommodated in the cylindrical barrel 5 and the support member 7 is rotated around the rotary shaft 6 as indicated by the arrows, the support member 7 Corresponding to this, the cylindrical barrel 5 supported by the support shaft 8 on the outer side in the circumferential direction of the rotary shaft 6 revolves around the rotary shaft 6 and is heated to a predetermined temperature by heating means (not shown). Aluminum evaporated from the heated boat 2 is deposited on the surface of the rare earth permanent magnet 30 in the cylindrical barrel 5 to form an aluminum film.
JP 2001-335921 A

図１に示す蒸着被膜形成装置は、大量処理が可能であり、生産性に優れたものである。しかしながら、希土類系永久磁石のサイズが大きくなると（例えば縦４０ｍｍ×横１５ｍｍ×厚み５ｍｍを超えるような板状磁石）、時として、蒸着被膜形成時に、磁石の欠けや、いったん形成された蒸着被膜の磁石からのはがれ（被膜ハガレ）が顕著となり、生産性の悪化を引き起こす場合がある。
そこで本発明は、サイズの大きい被処理物に対しても、被処理物の欠けや被膜ハガレの発生率を抑えて、その表面に蒸着被膜を効率的に形成することができる、蒸着被膜形成方法を提供することを目的とする。 The vapor deposition film forming apparatus shown in FIG. 1 is capable of mass processing and is excellent in productivity. However, when the size of the rare earth permanent magnet increases (for example, a plate-shaped magnet exceeding 40 mm in length, 15 mm in width, and 5 mm in thickness), sometimes, when a vapor-deposited film is formed, the magnet is missing or once the vapor-deposited film is formed. Peeling from the magnet (coating peeling) becomes prominent and may cause deterioration in productivity.
Accordingly, the present invention provides a vapor deposition film forming method capable of efficiently forming a vapor deposition film on a surface of a large size object to be processed while suppressing the occurrence of chipping or film peeling. The purpose is to provide.

本発明者らは、上記の点に鑑みて鋭意研究を重ねた結果、図１に示す蒸着被膜形成装置を用いて被処理物の表面に蒸着被膜を形成する際、円筒形バレル内に金属製スプリング部材を多数収容するか、円筒形バレル内に金属製スプリングをテンションを付加して架設することで、円筒形バレル内での被処理物の自由運動を制御することにより、被処理物の欠けや被膜ハガレの発生率を抑えて、その表面に蒸着被膜を効率的に形成することができることを見出した。   As a result of intensive studies in view of the above points, the present inventors have found that when a deposited film is formed on the surface of an object to be processed using the deposited film forming apparatus shown in FIG. A large number of spring members can be accommodated, or a metal spring can be installed in the cylindrical barrel with tension applied to control the free movement of the workpiece in the cylindrical barrel. The present inventors have found that a deposition film can be efficiently formed on the surface of the film while suppressing the rate of occurrence of film peeling.

上記の知見に基づいてなされた本発明の蒸着被膜形成方法は、請求項１記載の通り、真空処理室内に、蒸着材料の蒸発部と、その表面に蒸着材料が蒸着される被処理物を収容するための多孔性周面を有する筒型バレルを備え、筒型バレルを横設して水平方向の回転軸線を中心に回転させながら被処理物の表面に蒸着材料を蒸着させる蒸着被膜形成装置を用いた蒸着被膜形成方法であって、被処理物と金属製スプリング部材を、筒型バレル内にそれぞれ多数収容し、被処理物の表面に蒸着材料を蒸着させることを特徴とする。
また、本発明の蒸着被膜形成方法は、請求項２記載の通り、真空処理室内に、蒸着材料の蒸発部と、その表面に蒸着材料が蒸着される被処理物を収容するための多孔性周面を有する筒型バレルを備え、筒型バレルを横設して水平方向の回転軸線を中心に回転させながら被処理物の表面に蒸着材料を蒸着させる蒸着被膜形成装置を用いた蒸着被膜形成方法であって、金属製スプリングをテンションを付加して架設した筒型バレル内に、被処理物を多数収容し、被処理物の表面に蒸着材料を蒸着させることを特徴とする。
また、請求項３記載の蒸着被膜形成方法は、請求項１または２記載の蒸着被膜形成方法において、蒸着材料がアルミニウムであることを特徴とする。
また、請求項４記載の蒸着被膜形成方法は、請求項１乃至３のいずれかに記載の蒸着被膜形成方法において、被処理物が板状体であることを特徴とする。
また、請求項５記載の蒸着被膜形成方法は、請求項１乃至４のいずれかに記載の蒸着被膜形成方法において、被処理物が希土類系永久磁石であることを特徴とする。 The vapor deposition film forming method of the present invention made on the basis of the above knowledge, according to claim 1, accommodates an evaporation portion of the vapor deposition material and an object to be vapor deposited on the surface thereof in the vacuum processing chamber. A vapor deposition film forming apparatus comprising a cylindrical barrel having a porous peripheral surface for performing vapor deposition on a surface of an object to be processed while horizontally rotating the cylindrical barrel and rotating around a horizontal rotation axis The vapor deposition film forming method used is characterized in that a large number of workpieces and metal spring members are accommodated in a cylindrical barrel, and a vapor deposition material is vapor deposited on the surface of the workpiece.
In addition, the vapor deposition film forming method of the present invention, as described in claim 2, is a porous peripheral chamber for accommodating a vapor deposition portion of a vapor deposition material and an object to be vapor deposited on the surface thereof in a vacuum processing chamber. A vapor deposition film forming method using a vapor deposition film forming apparatus comprising a cylindrical barrel having a surface, and depositing a vapor deposition material on a surface of an object while rotating the cylindrical barrel around a horizontal rotation axis In this case, a large number of objects to be processed are accommodated in a cylindrical barrel in which a metal spring is applied with tension, and a deposition material is deposited on the surface of the object to be processed.
The vapor deposition film forming method according to claim 3 is the vapor deposition film forming method according to claim 1 or 2, wherein the vapor deposition material is aluminum.
The vapor deposition film forming method according to claim 4 is the vapor deposition film forming method according to any one of claims 1 to 3, wherein the object to be processed is a plate-like body.
The vapor deposition film forming method according to claim 5 is the vapor deposition film forming method according to any one of claims 1 to 4, wherein the object to be processed is a rare earth permanent magnet.

本発明によれば、サイズの大きい被処理物に対しても、被処理物の欠けや被膜ハガレの発生率を抑えて、その表面に蒸着被膜を効率的に形成することができる、蒸着被膜形成方法を提供することができる。   According to the present invention, it is possible to efficiently form a vapor deposition film on the surface of a large size object to be processed while suppressing the occurrence of chipping of the object to be processed and film peeling. A method can be provided.

まず、本発明の第一の蒸着被膜形成方法について説明する。この方法は、真空処理室内に、蒸着材料の蒸発部と、その表面に蒸着材料が蒸着される被処理物を収容するための多孔性周面を有する筒型バレルを備え、筒型バレルを横設して水平方向の回転軸線を中心に回転させながら被処理物の表面に蒸着材料を蒸着させる蒸着被膜形成装置を用いた蒸着被膜形成方法であって、被処理物と金属製スプリング部材を、筒型バレル内にそれぞれ多数収容し、被処理物の表面に蒸着材料を蒸着させることを特徴とする。以下に、この方法の一例を、図面を用いながら説明する。   First, the 1st vapor deposition film forming method of this invention is demonstrated. In this method, a vacuum barrel is provided with a cylindrical barrel having an evaporation portion for vapor deposition material and a porous peripheral surface for accommodating an object to be processed on which vapor deposition material is deposited. A vapor deposition film forming method using a vapor deposition film forming apparatus that deposits a vapor deposition material on the surface of the object to be processed while rotating around a horizontal rotation axis, the object to be processed and a metal spring member, A large number of each is accommodated in a cylindrical barrel, and a vapor deposition material is vapor-deposited on the surface of the workpiece. Hereinafter, an example of this method will be described with reference to the drawings.

図４は、被処理物とともに筒型バレル内に収容する、金属製スプリング部材の一例の模式的側面図である。筒型バレル内に収容する金属製スプリング部材は、被処理物と略同一大とすることが望ましい。筒型バレル内での被処理物の自由運動を適度に制御する緩衝部材としての機能を発揮させるのに好都合であり、被処理物の欠けや被膜ハガレの発生率を抑えて、その表面に蒸着被膜を効率的に形成することができるからである。例えば、被処理物の体積を１とした場合、金属製スプリング部材の体積（外接円筒の体積と見なすことができる）が０．５〜２．５であれば、金属製スプリング部材は被処理物と略同一大であるとすることができる。図５は、被処理物とともに筒型バレル内に収容する、金属製スプリング部材のその他の例の模式的側面図である。この金属製スプリング部材は、部材を構成する線状材の一部にスプリングを巻回したものである。   FIG. 4 is a schematic side view of an example of a metal spring member housed in a cylindrical barrel together with an object to be processed. It is desirable that the metal spring member accommodated in the cylindrical barrel is approximately the same size as the object to be processed. It is convenient for exhibiting the function as a buffering member that appropriately controls the free movement of the object to be processed in the cylindrical barrel, and suppresses the occurrence of chipping of the object to be processed and film peeling, and deposits on the surface. It is because a film can be formed efficiently. For example, if the volume of the object to be processed is 1, and the volume of the metal spring member (which can be regarded as the volume of the circumscribed cylinder) is 0.5 to 2.5, the metal spring member is the object to be processed. And approximately the same size. FIG. 5 is a schematic side view of another example of a metal spring member housed in a cylindrical barrel together with an object to be processed. This metal spring member is obtained by winding a spring around a part of a linear material constituting the member.

図６は、例えば、被処理物である板状の希土類系永久磁石３０と金属製スプリング部材３１を、それぞれ多数収容した円筒形バレル５内の模式的部分拡大斜視図である。円筒形バレル５内への磁石３０と金属製スプリング部材３１の収容個数は、磁石３０を１００個とした場合、金属製スプリング部材３１は９０個〜１１０個とすることが望ましい。両者をこのような比率で円筒形バレル５内に収容することで、円筒形バレル５内での磁石３０の自由運動が適度に制御され、磁石３０の欠けや被膜ハガレの発生率を抑えて、その表面に蒸着被膜を効率的に形成することができる。   FIG. 6 is a schematic partial enlarged perspective view of the cylindrical barrel 5 in which a large number of plate-like rare earth permanent magnets 30 and metal spring members 31 as objects to be processed are accommodated, for example. The number of magnets 30 and metal spring members 31 accommodated in the cylindrical barrel 5 is preferably 90 to 110 metal spring members 31 when the number of magnets 30 is 100. By accommodating both in the cylindrical barrel 5 at such a ratio, the free movement of the magnet 30 in the cylindrical barrel 5 is appropriately controlled, and the occurrence rate of chipping of the magnet 30 and film peeling is suppressed, A vapor deposition film can be efficiently formed on the surface.

次に、本発明の第二の蒸着被膜形成方法について説明する。この方法は、真空処理室内に、蒸着材料の蒸発部と、その表面に蒸着材料が蒸着される被処理物を収容するための多孔性周面を有する筒型バレルを備え、筒型バレルを横設して水平方向の回転軸線を中心に回転させながら被処理物の表面に蒸着材料を蒸着させる蒸着被膜形成装置を用いた蒸着被膜形成方法であって、金属製スプリングをテンションを付加して架設した筒型バレル内に、被処理物を多数収容し、被処理物の表面に蒸着材料を蒸着させることを特徴とする。以下に、この方法の一例を、図面を用いながら説明する。   Next, the second deposited film forming method of the present invention will be described. In this method, a vacuum barrel is provided with a cylindrical barrel having an evaporation portion for vapor deposition material and a porous peripheral surface for accommodating an object to be processed on which vapor deposition material is deposited. A vapor deposition film forming method using a vapor deposition film forming apparatus that deposits a vapor deposition material on the surface of an object to be processed while rotating about a horizontal rotation axis. A large number of objects to be processed are accommodated in the cylindrical barrel, and a deposition material is deposited on the surface of the object to be processed. Hereinafter, an example of this method will be described with reference to the drawings.

図７は、例えば、４本の金属製スプリング３２を両端面間にテンションを付加して架設した円筒形バレル５の模式的斜視図であり、図８は、被処理物である板状の希土類系永久磁石３０を多数収容したこの円筒形バレル５内の模式的部分拡大斜視図である。このような構成とすることで、金属製スプリング３２の存在により、円筒形バレル５内での磁石３０の自由運動が適度に制御され、磁石３０の欠けや被膜ハガレの発生率を抑えて、その表面に蒸着被膜を効率的に形成することができる。   FIG. 7 is a schematic perspective view of a cylindrical barrel 5 in which, for example, four metal springs 32 are installed with tension applied between both end faces, and FIG. 8 is a plate-shaped rare earth that is an object to be processed. FIG. 3 is a schematic partial enlarged perspective view in the cylindrical barrel 5 in which a large number of system permanent magnets 30 are accommodated. By adopting such a configuration, the presence of the metal spring 32 appropriately controls the free movement of the magnet 30 in the cylindrical barrel 5, and suppresses the occurrence rate of chipping of the magnet 30 and film peeling, A vapor deposition film can be efficiently formed on the surface.

本発明の蒸着被膜形成方法を適用することができる被処理物は、特に限定されるものではなく、蒸着処理によって蒸着被膜の形成が可能なものであればどのようなものでも構わない。しかしながら、本発明の蒸着被膜形成方法は、縦４０ｍｍ×横１５ｍｍ×厚み５ｍｍを超えるような板状の希土類系永久磁石や、単重が２０ｇを超えるような弓形の希土類系永久磁石などの、サイズの大きい希土類系永久磁石の表面に、膜厚が１μｍ〜１５μｍの蒸着被膜を形成する際などに特に適している。   The to-be-processed object which can apply the vapor deposition film formation method of this invention is not specifically limited, What kind of thing may be used if a vapor deposition film can be formed by vapor deposition treatment. However, the vapor deposition film forming method of the present invention has a size such as a plate-like rare earth-based permanent magnet exceeding 40 mm in length, 15 mm in width, and 5 mm in thickness, or an arc-shaped rare earth-based permanent magnet having a unit weight exceeding 20 g. Particularly suitable for forming a deposited film having a film thickness of 1 μm to 15 μm on the surface of a rare earth permanent magnet having a large thickness.

また、本発明の蒸着被膜形成方法は、真空蒸着法のように蒸着材料を単に加熱によって蒸発させて蒸着被膜を形成する場合にも適用することができるし、例えば、イオンプレーティング法のように蒸発したものをイオン化させて蒸着被膜を形成する場合にも適用することができる。   The vapor deposition film forming method of the present invention can also be applied to a case where a vapor deposition material is formed by simply evaporating a vapor deposition material by heating, such as a vacuum vapor deposition method. For example, an ion plating method can be used. The present invention can also be applied to the case where the evaporated film is ionized to form a vapor deposition film.

また、本発明の蒸着被膜形成方法は、金属やその合金などの蒸着材料を用いた蒸着被膜形成に適用することができるが、中でも、軟質金属や軟質金属成分を含む合金、例えば、アルミニウム、亜鉛、錫、マグネシウム、これらの金属成分の少なくとも１成分を含む合金などを使用した蒸着被膜形成に好適に適用することができる。   The vapor deposition film forming method of the present invention can be applied to vapor deposition film formation using a vapor deposition material such as a metal or an alloy thereof. Among them, a soft metal or an alloy containing a soft metal component, for example, aluminum or zinc , Tin, magnesium, and an alloy containing at least one of these metal components can be suitably applied to the formation of a deposited film.

また、本発明の蒸着被膜形成方法を実施するために使用される、真空処理室内に、蒸着材料の蒸発部と、その表面に蒸着材料が蒸着される被処理物を収容するための多孔性周面を有する筒型バレルを備え、筒型バレルを横設して水平方向の回転軸線を中心に回転させながら被処理物の表面に蒸着材料を蒸着させる蒸着被膜形成装置としては、図１に示した装置の他、例えば、米国特許４１１６１６１号公報やGraham Legge :"Ion VaporDeposited Coatings for Improved Corrosion Protection": Reprinted from Industrial Heating, September, 135-140, 1994に記載の装置が挙げられる。図９は、その一例の、図略の真空排気系に連なる真空処理室１０１の内部の模式的正面図（一部透視図）である。その室内上方には、例えば、ステンレス製のメッシュ金網で形成された円筒形バレル１０５が水平方向の回転軸線上の回転シャフト１０６を中心に回転自在に２個併設されている。また、その室内下方には、蒸着材料であるアルミニウムを蒸発させる蒸発部であるボート１０２が、支持テーブル１０３上に立設されたボート支持台１０４上に複数個配置されている。そして、この装置によれば、被処理物である希土類系永久磁石１３０を円筒形バレル１０５内に多数収容し、この円筒形バレルを矢示のごとく回転シャフト１０６を中心に回転させながら、図略の加熱手段によって所定温度に加熱されたボート１０２からアルミニウムを蒸発させることで、円筒形バレル１０５内の希土類永久磁石１３０の表面にアルミニウム被膜が形成される。   In addition, a porous surrounding for accommodating an evaporation portion of the vapor deposition material and an object to be vapor deposited on the surface thereof in a vacuum processing chamber used for carrying out the vapor deposition film forming method of the present invention. A vapor deposition film forming apparatus that includes a cylindrical barrel having a surface, and that deposits a vapor deposition material on the surface of an object to be processed while rotating the horizontal barrel about the horizontal barrel axis is shown in FIG. In addition to the above-mentioned apparatuses, for example, there are apparatuses described in US Pat. FIG. 9 is a schematic front view (partially perspective view) of the inside of the vacuum processing chamber 101 connected to an unillustrated evacuation system, as an example. Two cylindrical barrels 105 formed of, for example, a stainless steel mesh wire mesh are provided at the upper part of the room so as to be rotatable around a rotation shaft 106 on a horizontal rotation axis. A plurality of boats 102, which are evaporating portions for evaporating aluminum as a deposition material, are arranged on a boat support base 104 erected on a support table 103 below the room. According to this apparatus, a large number of rare earth permanent magnets 130, which are objects to be processed, are accommodated in the cylindrical barrel 105, and the cylindrical barrel is rotated around the rotary shaft 106 as indicated by an arrow, while not shown. By evaporating aluminum from the boat 102 heated to a predetermined temperature by the heating means, an aluminum film is formed on the surface of the rare earth permanent magnet 130 in the cylindrical barrel 105.

以下、本発明を実施例と比較例によってさらに詳細に説明するが、本発明はこれに限定して解釈されるものではない。なお、以下の実施例と比較例は、例えば、米国特許４７７０７２３号公報や米国特許４７９２３６８号公報に記載されているようにして、公知の鋳造インゴットを粉砕し、微粉砕後に成形、焼結、熱処理、表面加工を行うことによって得られた１４Ｎｄ−７９Ｆｅ−６Ｂ−１Ｃｏ組成（ａｔ％）の縦４２ｍｍ×横１８ｍｍ×厚み６ｍｍで単重３６ｇの板状焼結磁石（以下、磁石体試験片と称する）を用いて行った。   EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further in detail, this invention is limited to this and is not interpreted. In the following examples and comparative examples, for example, as described in US Pat. No. 4,770,723 and US Pat. No. 4,792,368, a known cast ingot is pulverized, and after pulverization, molding, sintering, and heat treatment are performed. A plate-like sintered magnet having a composition of 14Nd-79Fe-6B-1Co (at%) obtained by performing surface processing, 42 mm long x 18 mm wide x 6 mm thick and having a unit weight of 36 g (hereinafter referred to as a magnet test piece). ).

実施例１：
図２に示したような、直径１１０ｍｍ×長さ５７５ｍｍのステンレス製のメッシュ金網で形成された円筒形バレル内に、磁石体試験片８０個と、直径１５ｍｍ×長さ２０ｍｍのステンレス製スプリング部材（磁石体試験片の体積を１とした場合の体積は０．８）８０個を収容し、図１に示した蒸着被膜形成装置により、磁石体試験片の表面にアルミニウム被膜を形成した（円筒形バレルの装置への装着方法は図３に示した方法を採用したことから、装置全体では２４個の円筒形バレルを装着したので、一度に処理した磁石体試験片の総数は１９２０個である）。なお、蒸着条件は、蒸着時間３５分、円筒形バレル回転数４．７ｒｐｍとした。 Example 1:
As shown in FIG. 2, in a cylindrical barrel formed of a stainless steel mesh wire net having a diameter of 110 mm × a length of 575 mm, 80 magnet specimens and a stainless spring member having a diameter of 15 mm × a length of 20 mm ( The volume of the magnetic test piece is 0.8, and the volume is 0.8), and 80 pieces are accommodated, and an aluminum film is formed on the surface of the magnetic test piece by the vapor deposition film forming apparatus shown in FIG. Since the method shown in FIG. 3 was adopted for mounting the barrel to the apparatus, 24 cylindrical barrels were mounted in the entire apparatus, so the total number of magnetic test pieces processed at one time was 1920) . The vapor deposition conditions were a vapor deposition time of 35 minutes and a cylindrical barrel rotation speed of 4.7 rpm.

実施例２：
図７に示したような、４本の直径１５ｍｍのステンレス製スプリングを、両端面間にテンションを付加して架設した、直径１１０ｍｍ×長さ５７５ｍｍのステンレス製のメッシュ金網で形成された円筒形バレル内に、磁石体試験片８０個を収容し、図１に示した蒸着被膜形成装置により、磁石体試験片の表面にアルミニウム被膜を形成した（円筒形バレルの装置への装着方法は図３に示した方法を採用したことから、装置全体では２４個の円筒形バレルを装着したので、一度に処理した磁石体試験片の総数は１９２０個である）。なお、蒸着条件は、実施例１と同様の条件とした。 Example 2:
Cylindrical barrel made of stainless steel mesh wire with a diameter of 110 mm and a length of 575 mm, with four stainless steel springs with a diameter of 15 mm as shown in FIG. Inside, 80 magnet body test pieces were accommodated, and an aluminum film was formed on the surface of the magnet body test piece by the vapor deposition film forming apparatus shown in FIG. 1 (the mounting method of the cylindrical barrel in the apparatus is shown in FIG. 3). Since the entire apparatus was equipped with 24 cylindrical barrels because the method shown was adopted, the total number of magnet specimens processed at one time was 1920). The vapor deposition conditions were the same as those in Example 1.

比較例：
図２に示したような、直径１１０ｍｍ×長さ５７５ｍｍのステンレス製のメッシュ金網で形成された円筒形バレル内に、磁石体試験片８０個を収容し、図１に示した蒸着被膜形成装置により、磁石体試験片の表面にアルミニウム被膜を形成した（円筒形バレルの装置への装着方法は図３に示した方法を採用したことから、装置全体では２４個の円筒形バレルを装着したので、一度に処理した磁石体試験片の総数は１９２０個である）。なお、蒸着条件は、実施例１と同様の条件とした。 Comparative example:
In a cylindrical barrel formed of a stainless steel mesh wire net having a diameter of 110 mm and a length of 575 mm as shown in FIG. 2, 80 magnet body test pieces are accommodated, and the vapor deposition film forming apparatus shown in FIG. An aluminum coating was formed on the surface of the magnet test piece (since the method shown in FIG. 3 was used for mounting the cylindrical barrel on the apparatus, 24 cylindrical barrels were mounted on the entire apparatus. The total number of magnet specimens processed at one time is 1920). The vapor deposition conditions were the same as those in Example 1.

評価項目とその結果：
実施例１、実施例２、比較例それぞれについて、磁石体試験片の表面に形成されたアルミニウム被膜の膜厚（ｎ＝１０：断面観察による）を表１に示す。また、アルミニウム被膜が表面に形成された磁石体試験片１００００個について調べた、磁石体試験片の欠けと被膜ハガレの発生率と、磁石体試験片の欠けと被膜ハガレが認められず良品と判断されたアルミニウム被膜が表面に形成された磁石体試験片に対するプレッシャークッカ試験（ＰＣＴ試験：条件は温度１２５℃×相対湿度８５％×２ａｔｍの環境下に６０時間放置）の結果（ｎ＝５）を表１に示す。 Evaluation items and results:
Table 1 shows the film thickness (n = 10: by cross-sectional observation) of the aluminum coating formed on the surface of the magnet specimen for each of Example 1, Example 2, and Comparative Example. Further, 10,000 magnet test pieces having an aluminum film formed on the surface thereof were examined, and the occurrence rate of chipping and film peeling of the magnetic body test pieces, and the determination of non-defective products without chipping and film peeling of the magnet test piece. Pressure cooker test (PCT test: conditions are left for 60 hours in an environment of temperature 125 ° C. × relative humidity 85% × 2 atm) (n = 5) with respect to a magnet specimen having an aluminum coating formed thereon. Table 1 shows.

Figure 2006183098
Figure 2006183098

表１から明らかなように、実施例１と実施例２で得られたアルミニウム被膜が表面に形成された磁石体試験片は、比較例で得られたアルミニウム被膜が表面に形成された磁石体試験片よりも、磁石体試験片の欠けと被膜ハガレの発生率が大幅に減少しており、実施例１と実施例２の蒸着被膜形成方法は、優れた方法であることがわかった。   As is apparent from Table 1, the magnet body test piece on which the aluminum coating obtained in Example 1 and Example 2 was formed was the magnet body test in which the aluminum coating obtained in the comparative example was formed on the surface. The occurrence rate of chipping of the magnetic body test piece and film peeling was significantly reduced as compared with the piece, and it was found that the deposited film forming methods of Example 1 and Example 2 were excellent methods.

本発明は、サイズの大きい被処理物に対しても、被処理物の欠けや被膜ハガレの発生率を抑えて、その表面に蒸着被膜を効率的に形成することができる、蒸着被膜形成方法を提供することができる点において産業上の利用可能性を有する。   The present invention provides a vapor deposition film forming method capable of efficiently forming a vapor deposition film on the surface of a large size object to be processed while suppressing the occurrence of chipping or film peeling. It has industrial applicability in that it can be provided.

本発明の蒸着被膜形成方法を実施するための蒸着被膜形成装置の一例の真空処理室の内部の模式的正面図（一部透視図）である。It is a typical front view (partial perspective view) inside the vacuum processing chamber of an example of the vapor deposition film formation apparatus for enforcing the vapor deposition film formation method of this invention. 円筒形バレルの一例を示す模式的斜視図である。It is a typical perspective view which shows an example of a cylindrical barrel. 支持部材に支持された円筒形バレルの一例を示す模式的斜視図である。It is a typical perspective view which shows an example of the cylindrical barrel supported by the supporting member. 被処理物とともに筒型バレル内に収容する金属製スプリング部材の一例の模式的側面図である。It is a typical side view of an example of the metal spring member accommodated in a cylindrical barrel with a to-be-processed object. 同、その他の例の模式的側面図である。It is a typical side view of the other example. 被処理物である板状の希土類系永久磁石と金属製スプリング部材を、それぞれ多数収容した円筒形バレル内の模式的部分拡大斜視図である。It is a typical partial enlarged perspective view in the cylindrical barrel which accommodated many plate-shaped rare earth system permanent magnets and metal spring members which are processed objects, respectively. ４本の金属製スプリングを両端面間にテンションを付加して架設した円筒形バレルの模式的斜視図である。FIG. 4 is a schematic perspective view of a cylindrical barrel in which four metal springs are installed with tension applied between both end faces. 被処理物である板状の希土類系永久磁石を多数収容した図７の円筒形バレル内の模式的部分拡大斜視図である。FIG. 8 is a schematic partial enlarged perspective view in the cylindrical barrel of FIG. 7 in which a large number of plate-like rare earth permanent magnets to be processed are accommodated. 本発明の蒸着被膜形成方法を実施するための蒸着被膜形成装置のその他の例の真空処理室の内部の模式的正面図（一部透視図）である。It is a typical front view (partial perspective view) inside the vacuum processing chamber of the other example of the vapor deposition film forming apparatus for enforcing the vapor deposition film formation method of this invention.

符号の説明Explanation of symbols

１，１０１ 真空処理室
２，１０２ ボート
３，１０３ 支持テーブル
４，１０４ ボート支持台
５，１０５ 円筒形バレル
６，１０６ 回転シャフト
７ 支持部材
８ 支持軸
９ アルミニウムワイヤー
１０ 繰り出しリール
１１ 保護チューブ
１２ 切り欠き窓
１３ ギア
３０，１３０ 希土類系永久磁石
３１ 金属製スプリング部材
３２ 金属製スプリング DESCRIPTION OF SYMBOLS 1,101 Vacuum processing chamber 2,102 Boat 3,103 Support table 4,104 Boat support stand 5,105 Cylindrical barrel 6,106 Rotating shaft 7 Support member 8 Support shaft 9 Aluminum wire 10 Feeding reel 11 Protective tube 12 Notch Window 13 Gear 30, 130 Rare earth permanent magnet 31 Metal spring member 32 Metal spring

Claims (5)

真空処理室内に、蒸着材料の蒸発部と、その表面に蒸着材料が蒸着される被処理物を収容するための多孔性周面を有する筒型バレルを備え、筒型バレルを横設して水平方向の回転軸線を中心に回転させながら被処理物の表面に蒸着材料を蒸着させる蒸着被膜形成装置を用いた蒸着被膜形成方法であって、被処理物と金属製スプリング部材を、筒型バレル内にそれぞれ多数収容し、被処理物の表面に蒸着材料を蒸着させることを特徴とする蒸着被膜形成方法。   A vacuum processing chamber is provided with a cylindrical barrel having a vapor deposition material evaporation section and a porous peripheral surface for accommodating an object to be processed on which vapor deposition material is deposited. A deposition film forming method using a deposition film forming apparatus for depositing a deposition material on a surface of an object to be processed while rotating about a rotation axis of a direction, wherein the object to be processed and a metal spring member are placed in a cylindrical barrel A method for forming a vapor-deposited coating, comprising: depositing a plurality of vapor-deposited materials on the surface of an object to be treated. 真空処理室内に、蒸着材料の蒸発部と、その表面に蒸着材料が蒸着される被処理物を収容するための多孔性周面を有する筒型バレルを備え、筒型バレルを横設して水平方向の回転軸線を中心に回転させながら被処理物の表面に蒸着材料を蒸着させる蒸着被膜形成装置を用いた蒸着被膜形成方法であって、金属製スプリングをテンションを付加して架設した筒型バレル内に、被処理物を多数収容し、被処理物の表面に蒸着材料を蒸着させることを特徴とする蒸着被膜形成方法。   A vacuum processing chamber is provided with a cylindrical barrel having a vapor deposition material evaporation section and a porous peripheral surface for accommodating an object to be processed on which vapor deposition material is deposited. A vapor-deposited film forming method using a vapor-deposited film forming apparatus for depositing a vapor-deposited material on the surface of a workpiece while rotating around a rotation axis of a direction, and a cylindrical barrel constructed by attaching a metal spring with a tension A vapor deposition film forming method characterized in that a large number of objects to be processed are accommodated therein, and a vapor deposition material is deposited on the surface of the object to be processed. 蒸着材料がアルミニウムであることを特徴とする請求項１または２記載の蒸着被膜形成方法。   The vapor deposition material is aluminum, The vapor deposition film formation method of Claim 1 or 2 characterized by the above-mentioned. 被処理物が板状体であることを特徴とする請求項１乃至３のいずれかに記載の蒸着被膜形成方法。   4. The method for forming a deposited film according to claim 1, wherein the object to be processed is a plate-like body. 被処理物が希土類系永久磁石であることを特徴とする請求項１乃至４のいずれかに記載の蒸着被膜形成方法。   The vapor-deposited film forming method according to claim 1, wherein the object to be processed is a rare earth permanent magnet.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008045197A (en) * 2006-08-21 2008-02-28 Sony Corp Production method for composite powder, and production device for composite powder

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