JPH01147065A - Formation of film on powder - Google Patents

Formation of film on powder

Info

Publication number
JPH01147065A
JPH01147065A JP30339387A JP30339387A JPH01147065A JP H01147065 A JPH01147065 A JP H01147065A JP 30339387 A JP30339387 A JP 30339387A JP 30339387 A JP30339387 A JP 30339387A JP H01147065 A JPH01147065 A JP H01147065A
Authority
JP
Japan
Prior art keywords
powder
film
vacuum chamber
sputtering
diaphragm
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
JP30339387A
Other languages
Japanese (ja)
Inventor
Hiroaki Kawamura
裕明 川村
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.)
Ulvac Inc
Original Assignee
Ulvac Inc
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 Ulvac Inc filed Critical Ulvac Inc
Priority to JP30339387A priority Critical patent/JPH01147065A/en
Publication of JPH01147065A publication Critical patent/JPH01147065A/en
Pending legal-status Critical Current

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Abstract

PURPOSE:To uniformly form a film of fine grains around powder by allowing the fine grains generated by means of sputtering to plunge into the powder while applying vibrations to the powder by means of a vibrating plate. CONSTITUTION:The inside of a vacuum chamber 1 is evacuated, and Ar gas, etc., are introduced through an inlet pipe 3. A vibrating plate 7 on which a powder 9 of Ni, etc., is placed is driven, and then, electric power is applied from an electric power source 6 to a target 5 in a state where the agitation of the powder 9 is sufficiently continued, by which the fine grains of Cr, etc., sputtered from the target 5 by means of magnetron sputtering are allowed to adhere in a film-like state to the peripheral surface of the powder 9 in the rolled and agitated state. When the surface 7a, loaded with powder, of the vibrating plate 7 is formed into a projecting shape, the powder 9 is moved toward the top of the projecting surface and, as a result, the conditions of dispersion and agitation of the powder 9 can be improved.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は粒径が例えば数μmの粉末への被膜形成方法に
関する。
DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for forming a film on powder having a particle size of, for example, several μm.

(従来の技術) 従来、粒径が数μmの粉末に被膜を形成する方法として
CVD法や液相メツキ法等が知られている。このCVD
法は、例えば第1図示のように、内部にフィルタaを設
けた反応管す内に粉末Cを収め、該反応管すの流入口d
からコーティング材料の原料となるガス及び該粉末Cを
流動層状態にするガスを流入させ、該反応管すの外周に
設けた加熱用ヒータeにより流動層状態の粉末Cを加熱
し、熱化学反応により該粉末Cにコーティング材料の成
分で被膜を形成する。
(Prior Art) Conventionally, CVD methods, liquid phase plating methods, and the like are known as methods for forming a film on powder having a particle size of several μm. This CVD
For example, as shown in the first diagram, powder C is placed in a reaction tube equipped with a filter a, and the inlet d of the reaction tube is
A gas that is a raw material for the coating material and a gas that turns the powder C into a fluidized bed state are introduced into the reactor tube, and the powder C in a fluidized bed state is heated by a heating heater e provided on the outer periphery of the reaction tube to initiate a thermochemical reaction. A film is formed on the powder C using the components of the coating material.

また、液相メツキ法は、メツキ被膜となる金属の塩を含
む水溶液中にメツキすべき材料を浸し、電気的又は化学
的にメツキ被膜金属を該材料表面に還元析出させる方法
である。
The liquid phase plating method is a method in which a material to be plated is immersed in an aqueous solution containing a salt of a metal to be plated, and the metal to be plated is electrically or chemically reduced and precipitated on the surface of the material.

尚、被膜形成法としてスパッタ法や真空蒸着法などのP
VD法(Physical VaporDeposlt
ion法)が知られているが、この方法により微小粉末
へ被膜を形成することは困難視されており、有効な被膜
形成の実施例は報告されていない。
In addition, as a film forming method, P such as sputtering method or vacuum evaporation method is used.
VD method (Physical VaporDeposlt
ion method) is known, but it is considered difficult to form a film on fine powder by this method, and no examples of effective film formation have been reported.

(発明が解決しようとする問題点) 前記CVD法は、基本的に熱化学反応を伴うため有機物
のような耐熱性に乏しい材料の粉末の被膜形成には使え
ない。また金属材料でも粉末は焼結し易いので高温を有
する熱化学反応は使えない。更にコーティング材料とな
る原料ガスは反応管eの流入口dから流出口fへと流れ
る間にガスの組成が変化し、被膜の厚さにムラが生じる
おそれがあり、しかもCVD法に於て使用される原料ガ
スは一般に腐蝕性が強く、反応管eやこれに連らなる配
管材料、排ガス処理設備に耐蝕性、安全性を考慮する必
要がある。
(Problems to be Solved by the Invention) Since the CVD method basically involves a thermochemical reaction, it cannot be used to form a film on powder of a material with poor heat resistance, such as an organic substance. Furthermore, powders of metallic materials are easily sintered, so thermochemical reactions involving high temperatures cannot be used. Furthermore, the composition of the raw material gas used as the coating material changes while flowing from the inlet d to the outlet f of the reaction tube e, which may cause unevenness in the thickness of the coating. The raw material gas used is generally highly corrosive, and it is necessary to consider the corrosion resistance and safety of the reaction tube e, the piping materials connected thereto, and the exhaust gas treatment equipment.

また液相メツキ法によるときは、被コーティング材が金
属に限られしかもその種類が限定さされる不都合があり
、メツキ工程も煩雑でメツキ浴の管理に細心の注意を必
要とし、メツキ液から不純物が被膜中に混入し易い欠点
がある。
Furthermore, when using the liquid phase plating method, there are disadvantages in that the materials to be coated are limited to metals and the types thereof are also limited, the plating process is complicated, and careful management of the plating bath is required, and impurities are removed from the plating liquid. It has the disadvantage of being easily mixed into the coating.

更に粉末表面にメツキを施す場合、その粒径が小さくな
るにつれメツキ浴への分散が困難になり、均一な被膜形
成が出来ない。
Furthermore, when plating the powder surface, as the particle size becomes smaller, it becomes difficult to disperse the powder into the plating bath, making it impossible to form a uniform film.

本発明は、上記のようなCVD法やメツキ法による欠点
を解決し、PVD法により微小粉末へ被膜を形成するこ
とを目的とするものである。
The present invention aims to solve the above-mentioned drawbacks of the CVD method and the plating method, and to form a film on fine powder by the PVD method.

(問題点を解決するための手段) 本発明では、前記問題点を解決すべく、スパッタリング
等のPVD法による被膜を生成する真空装置の真空室内
に、被コーティング材の粉末を載せた振動板を設け、該
振動板により該粉末へ振動を与え乍ら該粉末に該真空装
置で生成される微粒子の被膜を形成するようにし、好ま
しくは該振動板はその粉末載置面を凸面に形成したもの
が使用される。
(Means for Solving the Problems) In order to solve the above-mentioned problems, the present invention provides a diaphragm on which powder of a material to be coated is placed in the vacuum chamber of a vacuum device that generates a coating by a PVD method such as sputtering. and the vibrating plate is configured to apply vibration to the powder while forming a film of fine particles generated by the vacuum device on the powder, and preferably the vibrating plate has a powder mounting surface formed as a convex surface. is used.

(作 用) PVD法による真空装置として例えばスパッタリング装
置を使用した場合、その真空室内を例えば1O−4Pa
に排気したのちArガスを導入し、該真空室内に設けた
ターゲットに負電位を与えると共に該真空室をアース電
位とすることにより該ターゲットと真空室との間でプラ
ズマ放電を生じさせる。該プラズマ放電によりArガス
イオンが発生し、これがターゲットへ衝突するとターゲ
ットから原子サイズの微粒子が被膜材料として発生する
(Function) When a sputtering device, for example, is used as a vacuum device using the PVD method, the vacuum chamber is heated to, for example, 1O-4Pa.
After the vacuum chamber is evacuated, Ar gas is introduced, and a negative potential is applied to a target provided in the vacuum chamber, and the vacuum chamber is brought to earth potential, thereby generating plasma discharge between the target and the vacuum chamber. Ar gas ions are generated by the plasma discharge, and when they collide with the target, atomic-sized fine particles are generated from the target as coating material.

こうした作用は一成約スバッタリングの場合と特に変わ
りがないが、本発明に於ては該真空室内に振動板を設け
てこれに被コーティング材の粉末を載せ、振動板で粉末
に振動を与え乍らスパッタリングで発生した微粒子を粉
末に突入させ、該粉末を微粒子でコーティングするもの
で、該粉末は振動板の振動により転勤撹拌されて新らた
な面が上方に現われ、そこに微粒子が突入するので粉末
の周面に均一に微粒子の被膜を形成することが出来る。
These effects are not particularly different from those of single-contract sputtering, but in the present invention, a diaphragm is provided in the vacuum chamber, powder of the material to be coated is placed on it, and the diaphragm vibrates the powder. However, the fine particles generated by sputtering are forced into the powder, and the powder is coated with fine particles.The powder is transferred and stirred by the vibration of the diaphragm, and a new surface appears above, into which the fine particles rush. Therefore, a film of fine particles can be uniformly formed on the circumferential surface of the powder.

(実施例) 本発明の実施例を図面第2図に示したようなスパッタリ
ング装置を使用して粒径的5μmのNIの粉末の被コー
ティング材にCrの被膜を形成する場合につき説明する
(Example) An example of the present invention will be described in which a sputtering apparatus as shown in FIG. 2 is used to form a Cr film on a material to be coated with NI powder having a particle size of 5 μm.

Ts2図に於て、符号(1)は真空排気口(2)、Ar
ガス導入管(3)、真空計(4)を備えたスパッタリン
グ装置のアース電位の真空室、(5)は該真空室(1)
内に設けたCr製のターゲット、(6)は該ターゲット
(5)に負電位を与える電源を示し、該真空室(1)内
ターゲット(5)と100m+wの間隔を存して凸面形
の振動板(7)とこれを振動するスピーカーからなる駆
動装置(8)とを設け、該振動板(7)の凸面形の粉末
載置面(7a)上に粒径的5μmの旧の被コーティング
材の粉末(9)をlOg載せるようにした。(′1Oa
tは駆動装置(8)を適当な振動数と振巾で作動させる
ための発振器と増巾器、(121は該ターゲット(5)
の背面に設けたマグネトロンスパッタ用の磁石である。
In the Ts2 diagram, code (1) is the vacuum exhaust port (2), Ar
A vacuum chamber at ground potential of the sputtering apparatus equipped with a gas introduction pipe (3) and a vacuum gauge (4), (5) is the vacuum chamber (1)
A Cr target (6) is provided in the vacuum chamber (1), and a convex vibrator is provided at a distance of 100m+w from the target (5) in the vacuum chamber (1). A drive device (8) consisting of a plate (7) and a speaker for vibrating the plate is provided, and an old material to be coated with a particle size of 5 μm is placed on the convex powder placement surface (7a) of the vibration plate (7). 10g of powder (9) was placed thereon. ('1 Oa
t is an oscillator and amplifier for operating the drive device (8) at an appropriate frequency and amplitude; (121 is the target (5))
This is a magnet for magnetron sputtering installed on the back of the

以上の装置を使用する場合、まず真空室(1)内を真空
排気口(2)からlO°’ Paに排気し、次いでAr
ガス導入管(3)からArガスを真空室(1)内が0.
4Paになるように導入する。次いで振動板(7)を駆
動し、旧粉末の撹拌が十分行なわれる状態としてから電
源(6)かラターゲット(5)ニ5001.2.OA電
力を投入し、Crのマグネトロンスパッタを行なうと、
ターゲット(5)からスパッタされたCrが転勤撹拌さ
れるN1粉末(9)の周面に被膜状に付着する。この場
合、振動板(7)には50〜IKIlzの範囲の振動数
を与えたが、振動数を変化させることで粉末(9)の分
散状態及び撹拌状態を変化させることが出来る。
When using the above apparatus, first the inside of the vacuum chamber (1) is evacuated to 10°' Pa through the vacuum exhaust port (2), and then Ar
Ar gas is introduced from the gas introduction pipe (3) until the inside of the vacuum chamber (1) reaches 0.
Introduce the pressure to 4Pa. Next, the diaphragm (7) is driven to ensure that the old powder is sufficiently stirred, and then the power source (6) or the target (5) is turned on. When OA power is applied and Cr magnetron sputtering is performed,
Cr sputtered from the target (5) adheres in the form of a film to the peripheral surface of the N1 powder (9) being transferred and stirred. In this case, the vibration plate (7) was given a vibration frequency in the range of 50 to IKIlz, but by changing the vibration frequency, the state of dispersion and stirring of the powder (9) can be changed.

マグネトロンスパッタの終了後、Nlの粉末(9)を取
出し、化学分析及び電子線マイクロプローブX線分析法
によりCrの付着量、付着状態をそれぞれ測定した。O
rの付着量は第3図示のようにスパッタ時間の経過と共
に増大することが化学分析の結果判明し、また電子線マ
イクロプローブx1分析法による分析の結果、Crが均
一にコーティングされていることが確認された。
After the magnetron sputtering was completed, the Nl powder (9) was taken out, and the amount and state of Cr deposited were measured by chemical analysis and electron beam microprobe X-ray analysis. O
Chemical analysis revealed that the amount of Cr deposited increased with the elapse of sputtering time, as shown in Figure 3, and analysis using electron beam microprobe x1 analysis revealed that Cr was coated uniformly. confirmed.

前記Nlの粉末(9)の代わりにAjh03(アルミナ
)の粉末を載せ、前記Nlの場合と同様の方法でCrを
コーティングすることも試みたが、この場合もAI!2
03の粉末の表面にはCrが均一にコーティングされて
いることがX線像及び電子顕微鏡により観察された。
An attempt was also made to place Ajh03 (alumina) powder in place of the Nl powder (9) and coat it with Cr in the same manner as in the case of Nl, but in this case as well, AI! 2
It was observed by an X-ray image and an electron microscope that the surface of the No. 03 powder was uniformly coated with Cr.

尚、振動板(7)を第2図示のように凸面形の粉末載置
面(7a)とすることにより振動を与えたとき粉末(9
)は凸面の頂部の方へ移動し、粉末載置面(7a)に於
ける粉末(9)の分散状態と撹拌状態が良好になるが、
粉末載置面(7a)を凹面形成は平面形に形成すると粉
末(9)は振動により粉末載置面(7a)の周辺部分に
片寄って堆積するようになり、粉末(9)に均一に被膜
を形成することが難しくなる。
In addition, by making the diaphragm (7) a convex powder placement surface (7a) as shown in the second figure, when vibration is applied, the powder (9
) moves toward the top of the convex surface, and the dispersion and agitation state of the powder (9) on the powder placement surface (7a) become better.
If the powder placement surface (7a) is formed into a concave or planar shape, the powder (9) will be deposited on the periphery of the powder placement surface (7a) due to vibration, and the powder (9) will be coated uniformly. becomes difficult to form.

以上はスパッタリングにより粉末に被膜を形成したが、
第4図示のように振動板(7)に栽せた粉末(9)を直
視出来る真空室(1)内の位置に蒸発源(13を設け、
該蒸発源a3からの蒸発物を振動板(n上の粉末(9)
に被膜状に付着させることも可能であり、真空アーク放
電蒸着、抵抗加熱法による蒸着等の蒸着源を使用出来る
In the above, a film was formed on the powder by sputtering, but
As shown in Figure 4, an evaporation source (13) is provided at a position within the vacuum chamber (1) where the powder (9) grown on the diaphragm (7) can be directly viewed;
The evaporated material from the evaporation source a3 is transferred to the diaphragm (powder (9) on n)
It is also possible to deposit it in the form of a film, and vapor deposition sources such as vacuum arc discharge vapor deposition and resistance heating vapor deposition can be used.

また粉末(9)及びこれへの被膜の材料は金属に限らず
有機物やセラミックス等であってもよい。
Further, the material of the powder (9) and the coating thereon are not limited to metals, but may be organic substances, ceramics, or the like.

(発明の効果) 以上のように本発明によるときは、PVD法により被膜
を形成する真空装置の真空室内に設けた振動板上に粉末
を載せ、該真空装置で生成される微粒子を該振動板によ
り振動する粉末に付着させて被膜を形成するようにした
ので、粉末を加熱することなくこれに均一に被膜を形成
することが出来、耐熱性の乏しい有機物等の粉末に被膜
を形成することが可能になり、腐蝕性の強い有害なガス
は使用しないので管理も容易で安全性も高く、金属以外
の粉末に金属以外の被膜を形成することが出来、豊富な
種類の被膜粉末を製造出来る等の効果がある。
(Effects of the Invention) As described above, according to the present invention, powder is placed on a diaphragm provided in the vacuum chamber of a vacuum device that forms a film by the PVD method, and fine particles generated in the vacuum device are transferred to the diaphragm. Since the film is formed by adhering it to the vibrating powder, it is possible to form a film uniformly on the powder without heating it, and it is possible to form a film on powders such as organic substances that have poor heat resistance. Since no highly corrosive and harmful gases are used, it is easy to manage and highly safe. It is also possible to form non-metallic coatings on non-metallic powders, making it possible to produce a wide variety of coated powders. There is an effect.

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

第1図は従来の粉末への被膜形成方法の説明図、第2図
は本発明の方法の実施例の説明図、第3図は本発明の実
施例に於ける被膜の付着量と時間の関係を示す線図、第
4図は本発明の他の実施例の説明図である。 (1)・・・真空室    (7)・・・振動板(9)
・・・粉 末 第30 第4図
Fig. 1 is an explanatory diagram of a conventional method for forming a film on powder, Fig. 2 is an explanatory diagram of an embodiment of the method of the present invention, and Fig. 3 is an explanatory diagram of the coating amount and time in an embodiment of the present invention. A diagram showing the relationship, FIG. 4 is an explanatory diagram of another embodiment of the present invention. (1)...Vacuum chamber (7)...Vibration plate (9)
...Powder No. 30 Figure 4

Claims (1)

【特許請求の範囲】 1、スパッタリング等のPVD法による被膜を形成する
真空装置の真空室内に、被コーティング材の粉末を載せ
た振動板を設け、該振動板により該粉末へ振動を与え乍
ら該粉末に該真空装置で生成される微粒子の被膜を形成
することを特徴とする粉末への被膜形成方法。 2、前記振動板として粉末載置面を凸面に形成したもの
を使用することを特徴とする特許請求の範囲第1項記載
の粉末への被膜形成方法。
[Scope of Claims] 1. A diaphragm on which powder of a material to be coated is placed is provided in a vacuum chamber of a vacuum device for forming a coating by a PVD method such as sputtering, and the diaphragm applies vibration to the powder. A method for forming a film on powder, the method comprising forming a film of fine particles produced in the vacuum device on the powder. 2. The method for forming a film on powder as set forth in claim 1, wherein the diaphragm is a diaphragm having a convex powder placement surface.
JP30339387A 1987-12-02 1987-12-02 Formation of film on powder Pending JPH01147065A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP30339387A JPH01147065A (en) 1987-12-02 1987-12-02 Formation of film on powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP30339387A JPH01147065A (en) 1987-12-02 1987-12-02 Formation of film on powder

Publications (1)

Publication Number Publication Date
JPH01147065A true JPH01147065A (en) 1989-06-08

Family

ID=17920481

Family Applications (1)

Application Number Title Priority Date Filing Date
JP30339387A Pending JPH01147065A (en) 1987-12-02 1987-12-02 Formation of film on powder

Country Status (1)

Country Link
JP (1) JPH01147065A (en)

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US6524381B1 (en) 2000-03-31 2003-02-25 Flex Products, Inc. Methods for producing enhanced interference pigments
US6586098B1 (en) 2000-07-27 2003-07-01 Flex Products, Inc. Composite reflective flake based pigments comprising reflector layers on bothside of a support layer
US6838166B2 (en) 2001-04-27 2005-01-04 Flex Products, Inc. Multi-layered magnetic pigments and foils
US6933048B2 (en) 2000-10-10 2005-08-23 Jds Uniphase Corporation Titanium-containing interference pigments and foils with color shifting properties
US7169472B2 (en) 2003-02-13 2007-01-30 Jds Uniphase Corporation Robust multilayer magnetic pigments and foils
JP2007204785A (en) * 2006-01-31 2007-08-16 Bridgestone Corp Particle coating method and particle coating apparatus
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CN103046012A (en) * 2012-11-16 2013-04-17 中国船舶重工集团公司第七二五研究所 Method for preparing covering type compound powder for thermal spraying by vacuum magnetron sputtering
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Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6241858B1 (en) * 1999-09-03 2001-06-05 Flex Products, Inc. Methods and apparatus for producing enhanced interference pigments
US6524381B1 (en) 2000-03-31 2003-02-25 Flex Products, Inc. Methods for producing enhanced interference pigments
US6676741B2 (en) 2000-03-31 2004-01-13 Flex Products, Inc. Methods for producing enhanced interference pigments
US6586098B1 (en) 2000-07-27 2003-07-01 Flex Products, Inc. Composite reflective flake based pigments comprising reflector layers on bothside of a support layer
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