JPH05239502A - Treatment of metallic flake - Google Patents
Treatment of metallic flakeInfo
- Publication number
- JPH05239502A JPH05239502A JP4079196A JP7919692A JPH05239502A JP H05239502 A JPH05239502 A JP H05239502A JP 4079196 A JP4079196 A JP 4079196A JP 7919692 A JP7919692 A JP 7919692A JP H05239502 A JPH05239502 A JP H05239502A
- Authority
- JP
- Japan
- Prior art keywords
- lubricant
- metal flakes
- flakes
- depositing
- metallic flake
- 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.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
- C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は例えば導電ペーストに使
用される金属フレークの処理方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for treating metal flakes used in, for example, a conductive paste.
【０００２】[0002]
【従来の技術】金属フレークは相互接触性が良好なため
に例えば導電ペースト等に有用である。上記金属フレー
クは金属塊をスタンプミル、ボールミル等のミリング装
置で粉砕することによって製造されるが、その際に焼付
き防止のため潤滑剤の添加が必要になる。BACKGROUND OF THE INVENTION Metal flakes have good mutual contact properties and are useful, for example, as a conductive paste. The metal flakes are produced by crushing a metal lump with a milling device such as a stamp mill or a ball mill. At that time, it is necessary to add a lubricant to prevent seizure.
【０００３】[0003]
【発明が解決しようとする課題】上記潤滑剤は金属フレ
ーク表面に付着しており、そのまゝ該フレークを使用し
て製造した導電ペーストを使用して塗布、焼成、硬化せ
しめて導電層を形成すると、焼成の際に該潤滑剤が１５
０〜３００℃の範囲で熱分解して発熱反応が起こり、ペ
ースト層が局部的に加熱され、金属フレークとペースト
中のバインダーとの熱膨張係数の差によって形成される
導電層に亀裂が発生し、導電層の電導度が低下してしま
うと云う問題点があった。The above lubricant is adhered to the surface of the metal flakes, and the conductive paste produced by using the flakes is applied, baked and cured to form a conductive layer. Then, when firing, the lubricant is 15
In the range of 0 to 300 ° C., thermal decomposition occurs and an exothermic reaction occurs, the paste layer is locally heated, and cracks occur in the conductive layer formed due to the difference in thermal expansion coefficient between the metal flakes and the binder in the paste. However, there is a problem that the electric conductivity of the conductive layer is lowered.
【０００４】[0004]
【課題を解決するための手段】本発明は上記従来の課題
を解決するための手段として、金属フレークを１２０℃
以上の温度で加熱することによって表面に付着している
潤滑剤を除去することを特徴とする金属フレークの処理
方法を提供し、更に金属フレークをガス気流中で１２０
℃以上の温度で加熱することによって表面に付着してい
る潤滑剤を除去することを金属フレークの処理方法を提
供するものであり、また更に金属フレークを１２０℃以
上の温度で加熱した後有機溶剤中に分散せしめることに
よって表面に付着している潤滑剤を除去する金属フレー
クの処理方法を提供するものである。As a means for solving the above-mentioned conventional problems, the present invention uses metal flakes at 120.degree.
A method for treating metal flakes, which comprises removing the lubricant adhering to the surface by heating at the above temperature, and further providing the metal flakes in a gas stream.
The present invention provides a method for treating metal flakes, in which the lubricant adhering to the surface is removed by heating at a temperature of ℃ or more, and further an organic solvent after heating the metal flakes at a temperature of 120 ℃ or more. Disclosed is a method for treating metal flakes, which removes lubricant adhering to the surface by dispersing the flakes therein.
【０００５】本発明において特に導電ペーストに用いら
れる金属フレークの材質としては、Ａg ，Ｃu ，Ａg −
Ｐd 合金等の導電性に優れた金属又は合金がある。In the present invention, as the material of the metal flakes used particularly in the conductive paste, Ag, Cu, Ag-
There are metals or alloys having excellent conductivity such as Pd alloy.
【０００６】[0006]
【作用】潤滑剤が付着した金属フレークを１２０℃以上
に加熱すると、該潤滑剤が分解もしくは燃焼して該金属
フレークから除去される。上記加熱は１分以上継続され
ることが望ましい。また上記加熱をガス気流中で行なう
と、該潤滑剤の分解ガスが該金属フレーク表面上に停滞
せず駆逐されるので、該潤滑剤の分解は一層容易とな
る。この際用いられるガスとしては大気、窒素ガス、ア
ルゴンガス、水素ガス等の不活性ガスまたは還元性ガス
がある。また加熱処理後に有機溶剤中に分散させると加
熱処理中に凝集したフレークが分散する。When the metal flakes to which the lubricant adheres are heated to 120 ° C. or higher, the lubricant is decomposed or burned and removed from the metal flakes. It is desirable that the heating be continued for 1 minute or more. Further, when the heating is carried out in a gas stream, the decomposition gas of the lubricant is expelled without stagnation on the surface of the metal flakes, so that the decomposition of the lubricant becomes easier. As the gas used at this time, there are an inert gas such as air, nitrogen gas, argon gas, hydrogen gas or a reducing gas. Further, when dispersed in an organic solvent after the heat treatment, aggregated flakes are dispersed during the heat treatment.
【０００７】[0007]
【実施例】平均粒径２μのＡg −２０Ｐd 合金のフレー
ク２０ｇを管状炉に入れて表１に示す方法によって夫々
処理したEXAMPLES 20 g of flakes of Ag-20Pd alloy having an average particle size of 2 μ were placed in a tube furnace and treated by the method shown in Table 1.
【０００８】[0008]
【表１】 [Table 1]
【０００９】〔示差熱分析〕表１に示す試料Ｎo.１，Ｎ
o.２，Ｎo.４，Ｎo.５について示差熱分析行なった結果
を図１に示す。大気中で加熱処理を行なった試料Ｎo.１
は付着潤滑剤が略完全に分解除去されており、示差熱分
析において発熱ピークは認められない。不活性ガスであ
るＡr中で加熱処理を行なった試料Ｎo.２においても、
気流を発生させた場合には付着潤滑剤が殆ど完全に分解
除去されており、示差熱分析において１９５℃付近に極
めて小さな発熱ピークが認められるにすぎない。一方無
処理のＮo.４では除去されていない付着潤滑剤の熱分解
により２７０℃付近で大きな発熱ピークが認められる。
またアセトン洗浄を行なった試料Ｎo.５は示差熱分析に
おいてＮo.４と全く同一挙動を示し、洗浄効果は全くな
いことがわかる。[Differential Thermal Analysis] Samples No. 1 and N shown in Table 1
The results of differential thermal analysis of o.2, No. 4 and No. 5 are shown in FIG. Sample No. 1 which was heat-treated in the atmosphere
The adhered lubricant was almost completely decomposed and removed, and no exothermic peak was observed in the differential thermal analysis. Also in the sample No. 2 which was heat-treated in Ar which is an inert gas,
When the air flow was generated, the adhered lubricant was almost completely decomposed and removed, and an extremely small exothermic peak was observed at around 195 ° C. in the differential thermal analysis. On the other hand, with untreated No. 4, a large exothermic peak is observed at around 270 ° C. due to thermal decomposition of the adhered lubricant that has not been removed.
In addition, the sample No. 5 that had been washed with acetone showed exactly the same behavior as the sample No. 4 in the differential thermal analysis, indicating that there was no cleaning effect.
【００１０】〔粒度〕試料Ｎo.１とＮo.３についてエポ
キシ樹脂を用いてペースト化し、粒ゲージにてペースト
中の試料Ｎo.１とＮo.３の粒度評価を行なった。その結
果試料Ｎo.１の平均粒度は１５μ、Ｎo.３の平均粒度は
２μであり、アセトン中の分散によって粉末凝集物が分
散せしめられることがわかる。[Particle Size] Sample No. 1 and No. 3 were made into a paste using an epoxy resin, and the particle size of Sample No. 1 and No. 3 in the paste was evaluated with a particle gauge. As a result, the average particle size of sample No. 1 was 15μ and the average particle size of No. 3 was 2μ, and it can be seen that the powder agglomerates are dispersed by the dispersion in acetone.
【００１１】〔導電性テスト〕試料Ｎo.１とＮo.４につ
いてエポキシ樹脂を用いてペースト化し、図２に示すよ
うにＡu 電極(1) とＩＴＯ端子(2) との間に該ペースト
を充填し、１２０℃、６０分の硬化を行なって導電層
(3) を形成せしめる。この場合該導電層(3) の全体厚み
ｄ2 は２５μ、電極(1) とＩＴＯ端子(2) との間隔ｄ1
は４μであった。[Conductivity Test] Samples No. 1 and No. 4 were made into a paste using epoxy resin, and the paste was filled between the Au electrode (1) and the ITO terminal (2) as shown in FIG. Then, the conductive layer is cured by curing at 120 ° C. for 60 minutes.
(3) is formed. In this case, the total thickness d 2 of the conductive layer (3) is 25 μ, and the distance d 1 between the electrode (1) and the ITO terminal (2) is
Was 4μ.
【００１２】上記導電層の電気抵抗を測定すると、試料
Ｎo.１では３×１０-4Ωcmであったが、試料Ｎo.４では
６×１０-4Ωcmとなり、試料Ｎo.４では導電層(3) の内
部に亀裂が発生して電導度が半分程度に低下することが
わかる。When the electric resistance of the conductive layer was measured, it was 3 × 10 -4 Ωcm for sample No. 1, but was 6 × 10 -4 Ωcm for sample No. 4, and the conductive layer ( It can be seen that cracks occur inside 3) and the electrical conductivity drops to about half.
【００１３】[0013]
【発明の効果】したがって、本発明においては簡単な処
理で金属フレークに付着した潤滑剤を略完全に除去する
ことが出来る。Therefore, in the present invention, the lubricant adhering to the metal flakes can be almost completely removed by a simple treatment.
【００１４】[0014]
【図１】示差熱分析グラフ1] Differential thermal analysis graph
【図２】導電性テストの説明図FIG. 2 is an explanatory diagram of a conductivity test.
─────────────────────────────────────────────────────
─────────────────────────────────────────────────── ───
【手続補正書】[Procedure amendment]
【提出日】平成４年７月２４日[Submission date] July 24, 1992
【手続補正１】[Procedure Amendment 1]
【補正対象書類名】明細書[Document name to be amended] Statement
【補正対象項目名】００１４[Correction target item name] 0014
【補正方法】削除[Correction method] Delete
Claims (3)
することによって表面に付着している潤滑剤を除去する
ことを特徴とする金属フレークの処理方法1. A method for treating metal flakes, which comprises removing the lubricant adhering to the surface by heating the metal flakes at a temperature of 120 ° C. or higher.
の温度で加熱することによって表面に付着している潤滑
剤を除去することを特徴とする金属フレークの処理方法2. A method for treating metal flakes, which comprises removing the lubricant adhering to the surface by heating the metal flakes at a temperature of 120 ° C. or higher in a gas stream.
した後有機溶剤中に分散せしめることによって表面に付
着している潤滑剤を除去することを特徴とする金属フレ
ークの処理方法3. A method for treating metal flakes, which comprises heating the metal flakes at a temperature of 120 ° C. or higher and then dispersing them in an organic solvent to remove the lubricant adhering to the surface.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4079196A JPH05239502A (en) | 1992-02-28 | 1992-02-28 | Treatment of metallic flake |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4079196A JPH05239502A (en) | 1992-02-28 | 1992-02-28 | Treatment of metallic flake |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05239502A true JPH05239502A (en) | 1993-09-17 |
Family
ID=13683222
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4079196A Withdrawn JPH05239502A (en) | 1992-02-28 | 1992-02-28 | Treatment of metallic flake |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05239502A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006152327A (en) * | 2004-11-25 | 2006-06-15 | Dowa Mining Co Ltd | Silver powder and production method therefor |
| JP2012153979A (en) * | 2012-04-02 | 2012-08-16 | Dowa Holdings Co Ltd | Silver powder and method for production thereof |
-
1992
- 1992-02-28 JP JP4079196A patent/JPH05239502A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006152327A (en) * | 2004-11-25 | 2006-06-15 | Dowa Mining Co Ltd | Silver powder and production method therefor |
| KR101141839B1 (en) * | 2004-11-25 | 2012-05-07 | 도와 홀딩스 가부시키가이샤 | Silver Powder and Method for Producing Same |
| JP2012153979A (en) * | 2012-04-02 | 2012-08-16 | Dowa Holdings Co Ltd | Silver powder and method for production thereof |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Application deemed to be withdrawn because no request for examination was validly filed |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 19990518 |