JPH0456701A - Manufacture of flaky metal powder - Google Patents

Manufacture of flaky metal powder

Info

Publication number
JPH0456701A
JPH0456701A JP2167482A JP16748290A JPH0456701A JP H0456701 A JPH0456701 A JP H0456701A JP 2167482 A JP2167482 A JP 2167482A JP 16748290 A JP16748290 A JP 16748290A JP H0456701 A JPH0456701 A JP H0456701A
Authority
JP
Japan
Prior art keywords
metal powder
flaky
particle size
powder
beads
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
JP2167482A
Other languages
Japanese (ja)
Inventor
Kazumasa Morikawa
和政 森川
Masayoshi Yoshitake
正義 吉武
Hitoshi Wada
仁 和田
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.)
Fukuda Metal Foil and Powder Co Ltd
Original Assignee
Fukuda Metal Foil and Powder Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Fukuda Metal Foil and Powder Co Ltd filed Critical Fukuda Metal Foil and Powder Co Ltd
Priority to JP2167482A priority Critical patent/JPH0456701A/en
Publication of JPH0456701A publication Critical patent/JPH0456701A/en
Pending legal-status Critical Current

Links

Abstract

PURPOSE:To efficiently manufacture flaky metal powder containing little quantity of super fine powder by using the specific diameter of pulverizing medium to treat the specific primary particle diameter of metal powder under the specific slurry concn. and treating. CONSTITUTION:The metal powder is formed to flaky shape in the solvent with a medium stirring mill. At this time, the primary particle diameter of metal powder as the starting raw material is made to be <=10mum. Further, the slurry concn. is made in the range of 5-60% and as the pulverizing medium, beads having 0.5-3mm diameter are used. In this way, the flaky metal powder having narrow particle size distribution width is obtd.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は粒度分布の狭い片状金属粉の製造方法である。[Detailed description of the invention] [Industrial application field] The present invention is a method for producing flaky metal powder with a narrow particle size distribution.

利用分野として塗膜形成を目的とするペースト充てん用
金属粉、メタリック顔料あるいは新しい機能性片状金属
粉として利用できる。
It can be used as metal powder for filling pastes for the purpose of forming coatings, metallic pigments, or new functional flaky metal powders.

〔従来の技術〕[Conventional technology]

金属粉と合成樹脂、あるいはセラミックスとの複合化に
よる新しい機能性材料の研究が進められいる。すでに導
電材料、磁性材料などについては多くの実績であり、種
々の金属粉が使用されている。しかし、現在使用されて
いる金属粉は大部分が粒状粉で塗膜を形成する用途には
薄膜化や塗面の平滑性を得るため、片状粉が良いとされ
ている。
Research is underway into new functional materials by combining metal powder with synthetic resins or ceramics. There have already been many achievements with regard to conductive materials, magnetic materials, etc., and various metal powders have been used. However, most of the metal powders currently used are granular powders, and flaky powders are considered to be preferable for applications in which coatings are formed, in order to obtain thinner coatings and smooth coating surfaces.

しかし、従来の片状粉は粒度分布幅が広く超微粉を多く
含むため、分散性が悪くペーストの粘度調整が難しい。
However, since conventional flaky powder has a wide particle size distribution and contains a large amount of ultrafine powder, it has poor dispersibility and is difficult to adjust the viscosity of the paste.

粒度分布巾が広い片状粉を使用すると塗膜の初期導電性
が悪く、塗膜の平滑性も悪く経時変化劣化も早いもので
ある。
If flaky powder with a wide particle size distribution is used, the initial conductivity of the coating film will be poor, the smoothness of the coating film will also be poor, and deterioration over time will be rapid.

具体的には、0.1μm以下の超微粉をほとんど含まず
、かつ50μm以上の粗大粉のない、しかも粒度分布巾
の非常に狭い片状金属粉は、電子部品導電ペースト用と
して以上述べた欠点がなく、最適な金属粉である。さら
に導電材以外の用途においても新しい機能性片状金属粉
として利用することができる。
Specifically, the flaky metal powder, which contains almost no ultrafine powder of 0.1 μm or less and no coarse powder of 50 μm or more, and has a very narrow particle size distribution width, is suitable for use in electrically conductive pastes for electronic components without the above-mentioned drawbacks. It is the most suitable metal powder. Furthermore, it can be used as a new functional flaky metal powder in applications other than conductive materials.

機械的に片状粉を製造する方法として従来までは直径1
001111以上のスチールボールなどを用いボールミ
ル、アジテータミル、振動ミルなどで粉砕している。
Conventionally, the method of mechanically producing flaky powder was
It is ground using a ball mill, agitator mill, vibration mill, etc. using steel balls of 001111 or higher.

これらの方法は主に粉砕して粒度を細かくするのが目的
であり、粉砕するためにはボールの衝撃力を強くする必
要がありそのため0.1μm以下の超微粉が粉砕中に非
常に多く発生する。粗粉は篩分などの方法で除(ことが
できるが超微粉は他の金属粉に付着したりして、分級な
どの方法を用いても取り除くことができない。小さなボ
ールを用いて片状化することも検討されたが、全く生産
性のないものとなってしまい、良い方法が見出されてい
ない。
The main purpose of these methods is to reduce the particle size by grinding, and in order to grind, it is necessary to increase the impact force of the ball, and as a result, a large amount of ultrafine powder of 0.1 μm or less is generated during grinding. do. Coarse powder can be removed by methods such as sieving, but ultrafine powder adheres to other metal powders and cannot be removed even by methods such as classification. Although it was considered to do so, it became completely unproductive and no good method has been found.

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

粉砕媒体として小さなボール(直径5mmφ以下のもの
をビーズと以下称する)を使用して衝撃力を弱くすると
超微粉の発生も少ないが、片状化も進まない。本発明者
等はいままで顔料などの分散機として使用されていた媒
体攪拌ミルに着目し、金属粉の片状化の研究を行った。
If small balls (those with a diameter of 5 mm or less are hereinafter referred to as beads) are used as the grinding medium to weaken the impact force, the generation of ultrafine powder will be reduced, but flaking will not proceed. The present inventors focused on a media stirring mill, which has been used as a dispersing machine for pigments, and conducted research on flaking metal powder.

媒体攪拌ミルとはビーズを含む分散溶媒をディスクで高
速回転させるものである。高速で回転するための出発原
料である金属粉の粒径、スラリー濃度等を検討しなけれ
ば、ビーズやディスクの摩耗や発熱が激しく、粗大片状
金属粉も多く発生し、目的とする粒度分布巾の狭い片状
金属粉を得ることができない。
A media stirring mill is one in which a dispersion solvent containing beads is rotated at high speed using a disk. If we do not consider the particle size of the metal powder, which is the starting material for high-speed rotation, and the slurry concentration, etc., beads and disks will wear out and generate heat, and a large amount of coarse flaky metal powder will be generated. It is not possible to obtain flaky metal powder with a narrow cloth.

本発明者等は粉砕媒体と出発原料の粒径の関係ならびに
スラリー濃度の研究を行い、媒体攪拌ミルを用いて効率
よく超微粉の少ない片状金属粉を製造する方法を見出し
たものである。
The present inventors conducted research on the relationship between the particle size of the grinding medium and the starting material, as well as the slurry concentration, and discovered a method for efficiently producing flaky metal powder with a small amount of ultrafine powder using a media agitation mill.

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

本発明は、媒体攪拌ミルにて金属粉を溶媒中で片状化す
る方法において、出発原料である金属粉の一次粒子径が
10μm以下で、スラリー濃度が5〜60パーセントの
範囲内で、粉砕媒体として直径0.5〜3 n+mのビ
ーズを用いることを特徴とする粒度分布巾の狭い金属粉
の製造方法である。
The present invention is a method of flaking metal powder in a solvent using a media agitation mill. This is a method for producing metal powder with a narrow particle size distribution, characterized by using beads with a diameter of 0.5 to 3 n+m as a medium.

出発原料の金属粉は凝集した粉であっても、次粒子径が
10μ細以下であれば良い。ある程度凝集していても、
攪拌中に金属粉が一次粒子に分散され片状化が進む。−
次粒子径が10μm以上であると、片状化後の粒子径が
50uI11以上となったり、出発原料が大きすぎるた
め、片状化があまり進まず効率が非常に悪くなる。金属
粉の組成については、Al+Cu+N’t+Fe+Ag
+Pd+Au及びこれらの合金粉が適する。
Even if the starting material metal powder is agglomerated powder, it is sufficient if the secondary particle size is 10 μm or less. Even if there is some degree of agglomeration,
During stirring, metal powder is dispersed into primary particles and flaking progresses. −
If the secondary particle size is 10 μm or more, the particle size after flaking will be 50 uI11 or more, or the starting material will be too large, so flaking will not proceed much and the efficiency will be extremely poor. Regarding the composition of metal powder, Al+Cu+N't+Fe+Ag
+Pd+Au and alloy powders thereof are suitable.

その他、大部分の金属粉について展延性を有するものは
片状化ができるが、Si、Cr、稠などの硬い金属やM
g、Naなとの溶媒と反応するものは、好ましくない。
In addition, most metal powders that have malleability can be made into flakes, but hard metals such as Si, Cr, and
Those that react with solvents such as g and Na are not preferred.

溶媒への金属粉充填量はスラリー濃度で示されスラリー
濃度=金属粉重量/金属粉重量+溶媒重量のことである
The amount of metal powder charged into the solvent is indicated by the slurry concentration, which is slurry concentration=metal powder weight/metal powder weight+solvent weight.

粒度分布巾の狭い片状金属粉を製造するためのスラリー
濃度は5〜60パーセントが良い。スラリー濃度が5パ
ーセント以下であると超微粉が多く発生し、またビーズ
やディスクの摩耗が激しい。
The slurry concentration for producing flaky metal powder with a narrow particle size distribution range is preferably 5 to 60 percent. If the slurry concentration is less than 5%, a large amount of ultrafine powder will be generated, and beads and disks will be severely worn.

また、60パ一セント以上であると粒度分布巾が広いも
のとなる。
Moreover, if it is 60 percent or more, the particle size distribution width will be wide.

スラリー濃度は片状化する金属粉の組成によって変える
必要が有るが、AI、 A1合金粉では、10〜20パ
ーセント、Cu + N i + F e及びこれらの
合金粉は、30〜50パーセント、Ag+ Pd、Au
及びこれらの合金粉は30〜60パーセントが最適スラ
リー濃度である。
The slurry concentration needs to be changed depending on the composition of the metal powder to be flaked, but it is 10 to 20% for AI and A1 alloy powders, 30 to 50% for Cu + Ni + Fe and these alloy powders, and 30 to 50% for Ag + Pd, Au
The optimum slurry concentration of these alloy powders is 30 to 60%.

粉砕媒体としては、直径0.5〜3 mmのビースを使
用するが、それより小さいビーズは片状化が進まず、ま
たビーズの摩耗も激しく良くない。
Beads with a diameter of 0.5 to 3 mm are used as the grinding medium, but beads smaller than this do not cause flaking and are also severely abraded, which is not good.

3IIII11より大きい直径のビーズであると粗大な
片状粉が非常に多く発生し、粒度分布巾も広いものとな
り良くない。
If the beads have a diameter larger than 3III11, a large amount of coarse flaky powder will be generated and the particle size distribution will be wide, which is not good.

ビーズの材質は、ガラス、セラミックス、スチール、ス
テンレスなどを用いることができ、特に制限はないが、
Feなとの不純物をきらう用途にはセラミックスビーズ
が適する。
The material of the beads can be glass, ceramics, steel, stainless steel, etc., and is not particularly limited.
Ceramic beads are suitable for applications where impurities such as Fe are avoided.

溶媒としては、水、アルコール、炭化水素、ケトン、エ
ステル、多価アルコールなどが使用できるが、イオウや
塩素を含むものや、金属を腐食する溶媒は、電子部品用
として使用する場合、好ましくない。なお、溶媒中に粉
砕助剤として脂肪酸を添加することもできる。
Water, alcohol, hydrocarbons, ketones, esters, polyhydric alcohols, etc. can be used as the solvent, but solvents containing sulfur or chlorine, or solvents that corrode metals are not preferred when used for electronic parts. In addition, a fatty acid can also be added to the solvent as a grinding aid.

媒体攪拌ミルのディスク回転数は周速で表すことができ
るが、9〜18 s/secが良い。
The disk rotation speed of the media stirring mill can be expressed in terms of circumferential speed, but preferably 9 to 18 s/sec.

9 va/sec以下の周速であると片状化に、非常に
時間が必要となり、18m/sec以上であると、均一
に片状化ができず、粒度分布巾も広くなる場合がある。
If the circumferential speed is less than 9 va/sec, it will take a very long time to flake, and if it is more than 18 m/sec, it may not be possible to flake uniformly and the particle size distribution may become wide.

なお、最初は低速で金属粉を溶媒中に均一に分散し、そ
の後、高速で運転する方法も可能である。
Note that it is also possible to uniformly disperse the metal powder in the solvent at low speed at first, and then operate at high speed.

〔作用] 片状金属粉を得るためには機械的な力を金属粉に与え、
片状加工を行う必要がある。
[Operation] To obtain flaky metal powder, mechanical force is applied to the metal powder,
It is necessary to perform flaky processing.

従来までの粉砕機は、粉砕が目的であるため、衝撃力が
強く、非常に細かい金属粉が多く発生したり再凝集によ
る粗大薄片になったりし、非常に粒度分布巾の広いもの
しか製造できなかった。
Conventional pulverizers are used for the purpose of pulverization, so the impact force is strong, producing a large amount of very fine metal powder or coarse flakes due to reaggregation, and they can only produce products with a very wide particle size distribution. There wasn't.

媒体攪拌ミルは、本来顔料などを溶媒に分散する分散機
として使用するものであるが、これを用いて金属粉の片
状化を行った結果、非常に粒度分布巾の狭い片状金属粉
が得られることが判明した。
A media stirring mill is originally used as a dispersion machine to disperse pigments etc. in a solvent, but as a result of using this to flake metal powder, flaky metal powder with a very narrow particle size distribution was created. It turns out that it can be obtained.

つまり、たとえ金属粉が凝集していても、金属粉の一次
粒子径が10μm以下の小さいものを出発原料として、
スラリー濃度5〜60パーセントの範囲で直径0.3〜
3IIl111のビーズを粉砕媒体として媒体撹拌ミル
にて高速回転で片状加工することにより、粒度分布巾の
狭い片状金属粉が得られるものである。
In other words, even if the metal powder is agglomerated, using small metal powder with a primary particle size of 10 μm or less as a starting material,
Diameter 0.3 to 60% slurry concentration range
By using beads of 3IIl111 as a grinding medium and processing them into flakes at high speed rotation in a media agitation mill, flaky metal powder with a narrow particle size distribution width can be obtained.

一般に10μm以下の金属粉は金属粉同志が弱く凝集し
ている場合が多く、大きいボールで機械加工を加えると
金属粉数個が、圧接され、大きい片状物となる。
Generally, metal powders with a diameter of 10 μm or less are often weakly aggregated together, and when machining is applied using a large ball, several pieces of metal powder are pressed together and become large flakes.

小さいビーズを媒体とすると、金属粉の凝集を分離する
作用が働き、個々の金属粉に対して均一に片状加工を加
えることができる。
When small beads are used as a medium, they have the effect of separating agglomerated metal powders, and each individual metal powder can be uniformly processed into flakes.

媒体攪拌ミルでは、ボールミルなどと異なり、溶媒中で
のビーズの動きが均一であるためにより、均一に片状加
工を加えることができるのであろう。
Unlike a ball mill, etc., a media stirring mill allows the beads to move uniformly in the solvent, making it possible to process the beads more uniformly into flakes.

スラリー濃度は、均一に片状加工をする上で重要であり
、あまり低いとビーズの摩耗が激しく、また高くなると
ビーズが金属粉に均一に接触することができず、金属粉
の再凝集が生じ、粒度分布巾も広くなる。
Slurry concentration is important for uniform flaking; if it is too low, the beads will be severely worn, and if it is too high, the beads will not be able to come into uniform contact with the metal powder, causing re-agglomeration of the metal powder. , the particle size distribution width also becomes wider.

以下、実施例により本発明を具体的に説明する。Hereinafter, the present invention will be specifically explained with reference to Examples.

〔実施例〕〔Example〕

実施例■ 出発原料として、Ag粉を用い水、メタノールアセトン
、酢酸エチル、エチレングリコールを溶媒として、スラ
リー濃度5〜60パーセントにおいて直径0.5〜3 
mmのジルコン、ガラス、スチールのビーズを粉砕媒体
とし、媒体攪拌ミルにて片状物を製造した。
Example ■ Using Ag powder as a starting material and using water, methanol acetone, ethyl acetate, and ethylene glycol as solvents, a slurry with a diameter of 0.5 to 3 mm was prepared at a slurry concentration of 5 to 60 percent.
Pieces were produced using a media agitation mill using beads of zircon, glass, and steel of mm size as the grinding media.

製造条件ならびに結果を表1の試料Nα1〜23に示す
The manufacturing conditions and results are shown in samples Nα1 to 23 in Table 1.

表1に示すように粒度分布巾の狭い片状物が出来た。As shown in Table 1, pieces with a narrow particle size distribution were formed.

実施例■ 出発原料として、Cu、Ni、Fe、Pd、AI粉を用
い、メタノールを溶媒として、スラリー濃度15〜50
パーセントにおいて直径1.On+wのガラスのビーズ
を粉砕媒体とし、媒体攪拌ミルにて片状物を製造した。
Example ■ Using Cu, Ni, Fe, Pd, and AI powders as starting materials and using methanol as a solvent, slurry concentration was 15 to 50.
Diameter in percent 1. On+w glass beads were used as a grinding medium to produce flakes in a media stirring mill.

製造条件ならびに結果を表1の試料陥、24〜32に示
す。
The manufacturing conditions and results are shown in Samples 24 to 32 in Table 1.

比較例■ 出発原料として、平均粒径1.0μmのAg粉を用いて
、メタノールを溶媒として、スラリー濃度30パーセン
トにおいて直径101のスチールボールを粉砕媒体とし
、ボールミルにて60分間粉砕を行ない、片状物を製造
した。
Comparative Example■ Using Ag powder with an average particle size of 1.0 μm as a starting material, grinding was carried out in a ball mill for 60 minutes using methanol as a solvent and steel balls with a diameter of 101 mm as a grinding medium at a slurry concentration of 30%. A similar product was produced.

この片状物は、平均粒径30μmであるが粒度分布は0
.1μIIl〜200μmと非常に巾が広く、又超微粉
を含みかつ粗大粉も多く発生した。
This flaky material has an average particle size of 30 μm, but the particle size distribution is 0.
.. The width was very wide, ranging from 1μIIl to 200μm, and contained ultrafine powder and a large amount of coarse powder.

〔発明の効果〕〔Effect of the invention〕

本発明は超微粉が少なく、粒度分布巾の狭い片状金属粉
を工業的に製造できる方法である。
The present invention is a method for industrially producing flaky metal powder with a small amount of ultrafine powder and a narrow particle size distribution.

いままで粒度分布巾の狭い片状金属粉を工業的に製造す
る方法がなく、片状金属粉を充填した機能性塗膜(電気
、磁気、熱伝導性など)を開発することが難しかったが
、本発明により新しい機能性塗膜の開発が可能となった
Until now, there was no way to industrially produce flaky metal powder with a narrow particle size distribution, and it was difficult to develop functional coatings (electrical, magnetic, thermal conductive, etc.) filled with flaky metal powder. The present invention has made it possible to develop a new functional coating film.

Claims (1)

【特許請求の範囲】[Claims] 媒体攪拌ミルにて金属粉を溶媒中で片状化する方法にお
いて、出発原料である金属粉の一次粒子径が10μm以
下で、スラリー濃度が5〜60パーセントの範囲内で、
粉砕媒体として直径0.5〜3mmのビースを用いるこ
とを特徴とする、粒度分布巾の狭い片状金属粉の製造方
法。
In the method of flaking metal powder in a solvent with a media stirring mill, the primary particle diameter of the metal powder as a starting material is 10 μm or less, and the slurry concentration is within the range of 5 to 60%.
A method for producing flaky metal powder with a narrow particle size distribution, characterized by using beads with a diameter of 0.5 to 3 mm as a grinding medium.
JP2167482A 1990-06-26 1990-06-26 Manufacture of flaky metal powder Pending JPH0456701A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2167482A JPH0456701A (en) 1990-06-26 1990-06-26 Manufacture of flaky metal powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2167482A JPH0456701A (en) 1990-06-26 1990-06-26 Manufacture of flaky metal powder

Publications (1)

Publication Number Publication Date
JPH0456701A true JPH0456701A (en) 1992-02-24

Family

ID=15850501

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2167482A Pending JPH0456701A (en) 1990-06-26 1990-06-26 Manufacture of flaky metal powder

Country Status (1)

Country Link
JP (1) JPH0456701A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2004048017A1 (en) * 2002-11-22 2004-06-10 Mitsui Mining & Smelting Co.,Ltd. Copper flake powder, method for producing copper flake powder, and conductive paste using copper flake powder
JP2009242914A (en) * 2008-03-31 2009-10-22 Mitsui Mining & Smelting Co Ltd Flake silver powder, and method for producing the same
JP2010236039A (en) * 2009-03-31 2010-10-21 Dowa Electronics Materials Co Ltd Flaky silver powder, its production method and conductive paste
JPWO2014157177A1 (en) * 2013-03-29 2017-02-16 東洋アルミニウム株式会社 Flaked stainless steel pigment, resin composition comprising the same, and coated product having a coating film formed from the resin composition

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WO2004048017A1 (en) * 2002-11-22 2004-06-10 Mitsui Mining & Smelting Co.,Ltd. Copper flake powder, method for producing copper flake powder, and conductive paste using copper flake powder
CN1292861C (en) * 2002-11-22 2007-01-03 三井金属矿业株式会社 Copper flake powder, method for producing copper flake powder, and conductive paste using copper flake powder
JP2009242914A (en) * 2008-03-31 2009-10-22 Mitsui Mining & Smelting Co Ltd Flake silver powder, and method for producing the same
JP2010236039A (en) * 2009-03-31 2010-10-21 Dowa Electronics Materials Co Ltd Flaky silver powder, its production method and conductive paste
JPWO2014157177A1 (en) * 2013-03-29 2017-02-16 東洋アルミニウム株式会社 Flaked stainless steel pigment, resin composition comprising the same, and coated product having a coating film formed from the resin composition

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