JP2013214508A5

JP2013214508A5 -

Info

Publication number: JP2013214508A5
Application number: JP2013043132A
Authority: JP
Filing date: 2013-03-05
Publication date: 2015-12-17
Anticipated expiration: 2033-03-05

Description

導電性微粒子を製造するときに、導電性微粒子に添加するものとして、増粘剤、分散剤、重金属不活性化剤等を使用できる。増粘剤を使用することで微粒子が過度に沈降することを抑制できる。増粘剤は、例えばシリカ系化合物、ポリカルボン酸系化合物、ポリウレタン系化合物、ウレア系化合物およびポリアマイド系等が挙げられる。分散剤を使用することで導電性微粒子の分散性をより向上できる。分散剤は、例えばカルボン酸やリン酸基から成る酸性分散剤、又はアミン基を含む塩基性分散剤、酸塩基で中和されている塩タイプの分散剤が挙げられる。
A thickener, a dispersing agent, a heavy metal deactivator, etc. can be used as what is added to electroconductive fine particles when manufacturing electroconductive fine particles. By using a thickener, it is possible to prevent the fine particles from precipitating excessively. Examples of the thickener include silica-based compounds, polycarboxylic acid-based compounds, polyurethane-based compounds, urea-based compounds, and polyamide-based compounds. Dispersibility of conductive fine particles by using a dispersant can be further improved. Examples of the dispersant include an acidic dispersant composed of a carboxylic acid or a phosphate group, a basic dispersant containing an amine group, and a salt type dispersant neutralized with an acid base.

導電性樹脂組成物の製造は、上記のように導電性微粒子を製造する前に樹枝状銀コート粉と樹脂とを同時に仕込み、固体媒体を衝突させて得ることができる。また、導電性微粒子の製造後に樹脂と混合して得ることもできる。樹脂を分散体に混合する際は、ディスパーマットで分散体を攪拌しながら樹脂を添加する方法が例示できる。
Producing the conductive resin composition can be obtained by the dendritic silver-coated powder and the resin was charged at the same time, to collide with the solid medium before producing the conductive fine particles as described above. It can also be obtained by mixing with a resin after the production of conductive fine particles. When the resin is mixed with the dispersion, a method of adding the resin while stirring the dispersion with a disperse mat can be exemplified.

＜円径度係数と円形係数＞測定サンプルとして、後述する電磁波シールドシートの作製方法により、対応する導電性微粒子を用いたサンプルを用意した。そして、ＳＥＭ用の円柱形の試料台に導電粘着剤を介して、１ｃｍ²のサンプルを固定した。具体的には、電磁波シールドシートの導電層側のセパレーターを剥離し、導電層が上層、絶縁層が下層になるように試料台に固定した。そして、電磁波シールドシートの導電層上に、白金蒸着を施した。蒸着後、１０００倍、加速電圧１５ｋＶの条件下で導電性粒子のＳＥＭ画像を取得し、上述の方法により解析した。
<Circularity coefficient and circular coefficient> As a measurement sample, a sample using corresponding conductive fine particles was prepared by a method for producing an electromagnetic wave shielding sheet described later. And the sample of 1 cm < ² > was fixed to the cylindrical sample stand for SEM through the electrically conductive adhesive. Specifically, the separator on the conductive layer side of the electromagnetic wave shield sheet was peeled off and fixed to the sample stage so that the conductive layer was the upper layer and the insulating layer was the lower layer. Then, the electromagnetic shielding sheet of the conductive layer was subjected to platinum deposition. After vapor deposition, SEM images of the conductive particles were obtained under the conditions of 1000 times and acceleration voltage of 15 kV, and analyzed by the method described above.

＜実施例２〜２０、比較例１〜４、参考例１の電磁波シールドシートの製造＞
導電性シートＣ１に代えて表４に記載した導電性シートを使用した以外は、実施例１と同様に行うことで電磁波シールドシートＥ２〜Ｅ２５を得た。
実施例１の導電性樹脂組成物に代えて実施例２〜２０の導電性樹脂組成物を用いた以外は、実施例１と同様の方法により電磁波シールドシートＥ２〜Ｅ２０を得た。また、実施例１の導電性樹脂組成物に代えて比較例１〜４、参考例１の導電性樹脂組成物を用いた以外は、実施例１と同様の方法により電磁波シールドシートＥ２１〜Ｅ２５を得た。

<Manufacture of electromagnetic wave shield sheets of Examples 2 to 20, Comparative Examples 1 to 4 and Reference Example 1>
Instead of the conductive sheet C 1 except for using the conductive sheet as described in Table 4, to obtain an electromagnetic wave shielding sheet E2~E25 by performing in the same manner as in Example 1.
Electromagnetic wave shield sheets E2 to E20 were obtained in the same manner as in Example 1, except that the conductive resin composition of Examples 2 to 20 was used instead of the conductive resin composition of Example 1. Moreover, it replaced with the electroconductive resin composition of Example 1, and except using the electroconductive resin composition of Comparative Examples 1-4 and the reference example 1 by the method similar to Example 1, electromagnetic shielding sheet E21-E25 was carried out. Obtained.

＜接続抵抗値の測定＞
縦２５ｍｍ、横２５ｍｍにカットした導電性シート１０を用意し、横２５ｍｍ、縦１００ｍｍ、厚み０．５ｍｍのステンレス板１１の端部に固定し８０℃、２ＭＰａの条件で熱圧着することで仮接着した。その後、剥離性シートを剥がし、同じ大きさのステンレス板１２を上記同様に重ねた上で、再度８０℃、２ＭＰａの条件で熱圧着することで仮接着した。これを１５０℃、２ＭＰａの条件で３０分間熱圧着を行うことで図４に示す接続抵抗値測定用のテストピースを得た。このテストピースを使用して三菱化学アナリテック社製「ロレスターＧＰ」のＢＳＰプローブを図４のように、ステンレス板１１のＢ側およびステンレス板１２のＡ側に接触させることにより接続抵抗値を測定した。評価基準は以下の通りである。
Ａ：１．０×１０^-3未満
Ｂ：１．０×１０^-3以上、１．０×１０^-2未満
Ｃ：１．０×１０^-2以上、１．０×１０^-1未満
Ｄ：１．０×１０^-1以上
<Measurement of connection resistance>
Prepare conductive sheet 10 cut to 25mm length and 25mm width, and fix it to the end of stainless steel plate 11 with width 25mm, length 100mm, thickness 0.5mm, and temporarily press bonded under conditions of 80 ° C and 2MPa. did. Thereafter, the peelable sheet was peeled off and the same size stainless steel plate 12 was stacked in the same manner as described above, and then temporarily bonded by thermocompression bonding under the conditions of 80 ° C. and 2 MPa. This was thermocompression bonded for 30 minutes under the conditions of 150 ° C. and 2 MPa to obtain a test piece for connection resistance measurement shown in FIG. Using this test piece, the connection resistance value is measured by bringing the BSP probe of “Lorester GP” manufactured by Mitsubishi Chemical Analytech into contact with the B side of the stainless steel plate 11 and the A side of the stainless steel plate 12 as shown in FIG. did. The evaluation criteria are as follows.
A: Less than 1.0 × 10 ⁻³ B: 1.0 × 10 ⁻³ or more, less than 1.0 × 10 ⁻² C: 1.0 × 10 ⁻² or more, less than 1.0 × 10 ⁻¹ D: 1.0 × 10 ^-1 or more

Claims

A nucleus containing a conductive material;
Covering the core body, comprising a conductive material different from the core body, comprising at least a coating layer constituting an outermost layer,
Conductive fine particles having a circularity coefficient determined from the following mathematical formula (1) of 0.15 or more and 0.4 or less, and at least one of notches and branched leaves is formed in the outer edge shape.

The conductive fine particle according to claim 1, wherein the coating layer is 1 part by weight or more and 40 parts by weight or less with respect to 100 parts by weight of the core.

The conductive fine particles according to claim 1 or 2, wherein the thickness is 0.1 µm or more and 2 µm or less.

The conductive fine particles according to claim 1, wherein the coating layer is silver.

The electroconductive resin composition containing the electroconductive fine particles of any one of Claims 1-4, and resin.

Under Symbol Formula conductive resin composition according to claims 1 to 5 any one of compounds having the unit represented is blended with (1).

The conductive resin composition according to claim 6 , wherein the compound having a unit represented by the chemical formula (1) includes at least one of the following chemical formula (2) and the following chemical formula (3).

Conductive sheet having a conductive layer obtained by forming a conductive resin composition according to any one of claims 5-7.

A conductive layer obtained by forming a conductive resin composition according to any one of claims 5-7, electromagnetic shield sheet provided with an insulating layer.

A nucleus containing a conductive material;
A method for producing conductive fine particles, comprising a coating layer that coats the core and is made of a conductive material different from the core, and at least a part of which forms a coating layer.
Preparing a dendritic particle having conductivity and a solid medium for deforming the dendritic particle by colliding with the dendritic particle;
By causing the dendritic microparticles and the solid medium to collide in a closed container, the circularity coefficient obtained from the following mathematical formula (1) is 0.15 or more and 0.4 or less, and And a step of deforming the outer edge so that at least one of notches and branched leaves is formed in plural.

The method for producing conductive fine particles according to claim 10, wherein the dendritic fine particles are obtained by covering the dendritic core with the coating layer.

11. The method for producing conductive fine particles according to claim 10, wherein the dendritic fine particles comprise the dendritic core, and the dendritic fine particles are coated with the coating layer after the dendritic fine particles are deformed.