JP3403274B2 - Conductive resin paste - Google Patents

Conductive resin paste

Info

Publication number
JP3403274B2
JP3403274B2 JP22322495A JP22322495A JP3403274B2 JP 3403274 B2 JP3403274 B2 JP 3403274B2 JP 22322495 A JP22322495 A JP 22322495A JP 22322495 A JP22322495 A JP 22322495A JP 3403274 B2 JP3403274 B2 JP 3403274B2
Authority
JP
Japan
Prior art keywords
conductive resin
resin paste
platinum
compound
component
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.)
Expired - Fee Related
Application number
JP22322495A
Other languages
Japanese (ja)
Other versions
JPH0967518A (en
Inventor
慎吾 伊藤
光 大久保
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.)
Sumitomo Bakelite Co Ltd
Original Assignee
Sumitomo Bakelite 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 Sumitomo Bakelite Co Ltd filed Critical Sumitomo Bakelite Co Ltd
Priority to JP22322495A priority Critical patent/JP3403274B2/en
Publication of JPH0967518A publication Critical patent/JPH0967518A/en
Application granted granted Critical
Publication of JP3403274B2 publication Critical patent/JP3403274B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L24/00Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
    • H01L24/01Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
    • H01L24/26Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/28Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L24/29Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/10Details of semiconductor or other solid state devices to be connected
    • H01L2924/102Material of the semiconductor or solid state bodies
    • H01L2924/1025Semiconducting materials
    • H01L2924/10251Elemental semiconductors, i.e. Group IV
    • H01L2924/10253Silicon [Si]
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01LSEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L2924/00Indexing scheme for arrangements or methods for connecting or disconnecting semiconductor or solid-state bodies as covered by H01L24/00
    • H01L2924/15Details of package parts other than the semiconductor or other solid state devices to be connected
    • H01L2924/151Die mounting substrate
    • H01L2924/156Material
    • H01L2924/15786Material with a principal constituent of the material being a non metallic, non metalloid inorganic material
    • H01L2924/15787Ceramics, e.g. crystalline carbides, nitrides or oxides

Landscapes

  • Engineering & Computer Science (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Die Bonding (AREA)
  • Conductive Materials (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a conductive resin paste having a small amount of ionic impurities and improved in curability and workability by using a silver powder, a specified cyclosiloxane, a compound having a specified boiling point and containing an alkenyl group and a platinum catalyst as the essential components. SOLUTION: This conductive resin paste is prepared by premixing 60-90wt.% silver powder containing 10ppm or below of ionic impurities (e.g. sodium ions) with 1-20wt.% cyclosiloxane represented by the formula (wherein R1 to R3 are CH3 or phenyl; (m) is 2 or greater; (n) is an integer; and m+n=3-6) and containing 500ppm or below ionic impurities (e.g. chloride ions and sodium ions), 5-25wt.% compound having two or more alkenyl groups in the molecule and having a boiling point of 100 deg.C or above, 0.1-100ppm (in terms of the platinum atoms) of a platinum catalyst and optionally additives such as a flexibilizer, antifoamer and a coupling agent, kneading the obtained premix and deaerating the mixture in vacuo.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、IC、LSI等の半導
体素子を金属フレーム等に接着する導電性樹脂ペースト
に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a conductive resin paste for adhering semiconductor elements such as IC and LSI to a metal frame or the like.

【0002】[0002]

【従来の技術】半導体製造工程における半導体素子の接
着、所謂ダイボンド工程において生産性の向上を目的と
しダイボンダー、ワイヤボンダー等を同一ライン上にレ
イアウトしたインライン硬化方式が採用され、今後ます
ます増加する傾向にある。従って、従来から行われてき
たバッチ方式による導電性樹脂ペーストの硬化条件に比
較し、硬化に要する時間は著しく制限され、例えばバッ
チ硬化方式の場合には150〜200℃で、60〜90
分間で硬化を行っていたが、インライン硬化方式の場合
には15〜90秒間での硬化が要求されている。更に
は、チップサイズが大きく、銅フレームを使用する半導
体製品のインライン硬化に際して、チップとフレームの
熱膨張係数の差に基づくチップの反り量の最小限化及び
フレームの酸化防止のためにも低温硬化が要求され、ま
た硬化時間に関してもより短時間での硬化が要求されて
いる。従来より用いられてきたポリイミド系のペースト
の場合、N−メチル−2−ピロリドン、ジメチルホルム
アミド等の高沸点溶媒を使用しているため90秒以下の
短時間での硬化は難しく、短時間で硬化させるには硬化
温度を250℃以上にしなければならないので、硬化中
に著しくボイドが発生してしまい接着力の低下、導電
性、熱伝導性の悪化など半導体製品の特性の低下につな
がっていた。一方、現在主流のエポキシ系の導電性ペー
ストの場合は、例えばアミン系硬化剤等を用いることに
より60秒程度での硬化は可能であるが、15〜30秒
といった超短時間硬化への対応はなされていない。
2. Description of the Related Art In-line curing method in which die bonders, wire bonders, etc. are laid out on the same line is adopted for the purpose of improving the productivity in the so-called die-bonding process, which is the bonding of semiconductor elements in the semiconductor manufacturing process. It is in. Therefore, the time required for curing is significantly limited as compared with the conventional curing method of the conductive resin paste by the batch method. For example, in the case of the batch curing method, the temperature is 60 to 90 ° C. at 60 to 90 ° C.
Although the curing was carried out in a minute, in the case of the in-line curing method, curing in 15 to 90 seconds is required. In addition, when in-line curing of semiconductor products with large chip size and copper frame is used, low temperature curing is used to minimize chip warpage and prevent frame oxidation due to the difference in thermal expansion coefficient between chip and frame. Is required, and the curing time is required to be shorter. In the case of a polyimide paste that has been used conventionally, it is difficult to cure in a short time of 90 seconds or less because a high boiling point solvent such as N-methyl-2-pyrrolidone or dimethylformamide is used. In order to do so, the curing temperature must be 250 ° C. or higher, so that voids are remarkably generated during the curing, which leads to deterioration of characteristics of semiconductor products such as a decrease in adhesive strength, deterioration of electrical conductivity and thermal conductivity. On the other hand, in the case of the epoxy-based conductive paste, which is currently the mainstream, it is possible to cure in about 60 seconds by using, for example, an amine-based curing agent, but it is not possible to cure in an ultra short time of 15 to 30 seconds. Not done.

【0003】[0003]

【発明が解決しようとする課題】本発明は150℃以
下、30秒以下の硬化条件でも硬化可能で、かつ塩素イ
オン、ナトリウムイオン等のイオン性不純物の少ない高
信頼性の導電性樹脂ペーストを提供するものである。
DISCLOSURE OF THE INVENTION The present invention provides a highly reliable conductive resin paste which can be cured under curing conditions of 150 ° C. or less and 30 seconds or less, and has a small amount of ionic impurities such as chlorine ions and sodium ions. To do.

【0004】[0004]

【課題を解決するための手段】本発明は、(A)銀粉、
(B)式(1)で示されるシクロシロキサン、(C)沸
点が100℃以上で、かつ1分子内に2個以上のアルケ
ニル基を有する化合物、(D)白金系触媒を必須成分と
し、かつ全導電性樹脂ペースト中に(A)成分を60〜
90重量%、(B)成分を1〜20重量%、(C)成分
を5〜25重量%、(D)成分を白金換算で0.1〜1
00ppm含み、(C)成分が、2−ヒドロキシ−1,
3−ジメタクリロキシプロパン、2,2−ビス(4−
(メタクリロキシジエトキシ)フェニル)プロパン、
1,6−ヘキサンジオールジメタクリレート又は2,2
−ビス(4−(メタクリロキシエトキシ)フェノールプ
ロパンである導電性樹脂ペーストである。
The present invention provides (A) silver powder,
(B) a cyclosiloxane represented by the formula (1), (C) a compound having a boiling point of 100 ° C. or higher and having two or more alkenyl groups in one molecule, (D) a platinum-based catalyst as an essential component, and 60 to 60% of component (A) in all conductive resin paste
90% by weight, 1 to 20% by weight of the component (B), 5 to 25% by weight of the component (C), and 0.1 to 1 of the component (D) in terms of platinum.
00ppm seen including, component (C), 2-hydroxy-1,
3-dimethacryloxypropane, 2,2-bis (4-
(Methacryloxydiethoxy) phenyl) propane,
1,6-hexanediol dimethacrylate or 2,2
-Bis (4- (methacryloxyethoxy) phenol
It is a conductive resin paste that is lopain .

【0005】[0005]

【化3】 [Chemical 3]

【0006】本発明に用いる銀粉は、用いる分野が電子
・電気分野のため塩素イオン、ナトリウムイオン等のイ
オン性不純物量が10ppm以下であることが望まし
い。また形状としてはフレーク状、樹枝状あるいは球状
のものを単独あるいは混合して用いることができる。更
に粒径に関しては通常平均粒径が2〜10μm、最大粒
径は50μm程度のものが好ましく、比較的細かい銀粉
と粗い銀粉を混合して用いるのが好ましい。全導電性樹
脂ペースト中の銀粉量が60重量%未満だと硬化物の電
気導電性が低下し、90重量%を越えると樹脂ペースト
の粘度が高くなりすぎ塗布作業性の低下の原因となるの
で好ましくない。
Since the silver powder used in the present invention is used in the fields of electronics and electricity, it is desirable that the amount of ionic impurities such as chlorine ions and sodium ions be 10 ppm or less. As the shape, flaky, dendritic or spherical shapes can be used alone or in combination. Regarding the particle size, it is usually preferable that the average particle size is 2 to 10 μm and the maximum particle size is about 50 μm, and it is preferable to use a mixture of relatively fine silver powder and coarse silver powder. If the amount of silver powder in the total conductive resin paste is less than 60% by weight, the electrical conductivity of the cured product will decrease, and if it exceeds 90% by weight, the viscosity of the resin paste will be too high, which will cause a decrease in coating workability. Not preferable.

【0007】本発明で用いる式(1)のシクロシロキサ
ンは、R1、R2、R3がメチル基、又はフェニル基でm
は2以上の整数で、m+nは3〜6である。より好まし
いのは、式(2)で示される構造のものでmは2以上の
整数で、m+nは4である。
In the cyclosiloxane of the formula (1) used in the present invention, R 1 , R 2 and R 3 are methyl groups or phenyl groups and m
Is an integer of 2 or more, and m + n is 3 to 6. More preferred is a structure represented by the formula (2), m is an integer of 2 or more, and m + n is 4.

【0008】[0008]

【化4】 例えば、式(1)のシクロシロキサンと異なる構造の直
鎖状のシロキサンである1,1,3,3−テトラメチル
ジシロキサンでは、沸点が約70℃と低く硬化時に発泡
あるいは揮発してしまい、またシロキサン単位が2以上
のいわゆるHオイルの場合には、反応の相手となるアル
ケニル基を有する化合物との相溶性が悪くなり硬化前あ
るいは硬化時に分離する欠点があるのに対し、式(1)
のシクロシロキサンではこれらの欠点がない。式(1)
のシクロシロキサンは、塩素、ナトリウム等のイオン性
不純物が50ppm以下であることが好ましい。これら
の例としては、テトラメチルシクロテトラシロキサン、
ヘキサメチルシクロテトラシロキサン、ペンタメチルシ
クロテトラシロキサン等が挙げられる。式(1)のシク
ロシロキサンの配合量は、全導電性樹脂ペースト中に1
〜20重量%であり、1重量%未満だと期待する性能が
得られず、20重量%を越えると十分な架橋構造が得ら
れないので、導電性樹脂ペースト硬化物の凝集力が弱く
十分な接着力を発揮し得ない。
[Chemical 4] For example, 1,1,3,3-tetramethyldisiloxane, which is a linear siloxane having a structure different from that of the cyclosiloxane of the formula (1), has a low boiling point of about 70 ° C. and is foamed or volatilized during curing. Further, in the case of so-called H oil having 2 or more siloxane units, the compatibility with the compound having an alkenyl group as a reaction partner is deteriorated and there is a drawback that the compound is separated before or during curing, whereas in the formula (1)
Cyclosiloxane does not have these drawbacks. Formula (1)
It is preferable that the cyclosiloxane has ionic impurities such as chlorine and sodium of 50 ppm or less. Examples of these are tetramethylcyclotetrasiloxane,
Hexamethylcyclotetrasiloxane, pentamethylcyclotetrasiloxane and the like can be mentioned. The compounding amount of the cyclosiloxane of the formula (1) is 1 in the total conductive resin paste.
If it is less than 1% by weight, the expected performance cannot be obtained, and if it exceeds 20% by weight, a sufficient crosslinked structure cannot be obtained. It cannot exhibit adhesive strength.

【0009】本発明に用いる1分子内に2個以上のアル
ケニル基を有する化合物は、沸点が100℃以上である
が、沸点が100℃未満だと硬化時に発泡あるいは揮発
するため使用できない。またアニケニル基はシクロシロ
キサンとハイドロシリル化反応をするのに必要であり、
1分子内にアルケニル基が1個のみの場合には反応後も
高分子量化しないため実用的ではない。本発明では、沸
点が100℃以上であればよく、高分子量の化合物は沸
点に達する前に分解するため100℃以上と表現した。
この配合量は、全導電性樹脂ペースト中に5重量%未満
だと導電性樹脂ペーストの硬化物の架橋密度が高くなら
ず、導電性樹脂ペーストに必要とされる性能が得られ
ず、また25重量%を越えると硬化後も未反応のアルケ
ニル基が残存してしまうため好ましくない。1分子内に
2個以上のアルケニル基を有する化合物としては、2−
ヒドロキシ−1,3−ジメタクリロキシプロパン、2,
2−ビス(4−(メタクリロキシジエトキシ)フェニ
ル)プロパン、1,6−ヘキサンジオールジメタクリレ
ート、2,2−ビス(4−(メタクリロキシエトキシ)
フェノールプロパン等が挙げられる。
The compound having two or more alkenyl groups in one molecule used in the present invention has a boiling point of 100 ° C. or more, but if the boiling point is less than 100 ° C., it cannot be used because it foams or volatilizes during curing. The anikenyl group is necessary for hydrosilylation reaction with cyclosiloxane,
When the number of alkenyl groups in one molecule is only one, it is not practical because the molecular weight does not increase even after the reaction. In the present invention, the boiling point may be 100 ° C. or higher, and a compound having a high molecular weight is decomposed before reaching the boiling point, and is therefore expressed as 100 ° C. or higher.
If this content is less than 5% by weight in the total conductive resin paste, the crosslink density of the cured product of the conductive resin paste will not be high, and the performance required for the conductive resin paste will not be obtained. If it exceeds 5% by weight, unreacted alkenyl groups remain after curing, which is not preferable. Examples of the compound having two or more alkenyl groups in one molecule include 2-
Hydroxy-1,3-dimethacryloxypropane, 2,
2-bis (4- (methacryloxydiethoxy) phenyl) propane, 1,6-hexanediol dimethacrylate, 2,2-bis (4- (methacryloxyethoxy)
Examples include phenol propane.

【0010】更に本発明では白金系触媒として、ハイド
ロシリル化反応で一般に使用される6塩化白金酸を用い
てもよいが、使用する分野が電気・電子分野であること
から腐食性のイオンが極力少なく、また触媒活性の点か
ら白金と有機化合物あるいは有機シリコーン化合物との
錯体を用いるのが好ましい。具体的には白金とシクロ
(ビニルメチルシロキサン)錯体、白金とジビニルテト
ラメチルジシロキサン錯体、白金とオクチルアルコール
錯体等があるが錯体自体が硬化時に反応するという点
で、白金とシクロ(ビニルメチルシロキサン)との錯
体、白金とジビニルテトラメチルジシロキサンとの錯体
を用いるのが好ましい。白金系触媒の配合量は、全導電
性樹脂ペースト中に白金換算で0.1〜100ppmで
あるが、0.1ppm未満だと導電性樹脂ペーストが十
分に硬化しなかったり、あるいは硬化時間が長くなる。
100ppmを越えると導電性樹脂ペーストの硬化時の
反応に伴う発熱量が多くなりすぎ、硬化物中にボイドが
発生し易く接着強度の低下、電気伝導率、熱伝導率の悪
化の原因となる。本発明においては必要に応じ、可撓性
付与剤、消泡剤、カップリング剤等を用いることもでき
る。導電性樹脂ペーストの製造方法は、例えば各成分を
予備混合した後、3本ロールを用いて混練し、混練後真
空下脱泡し樹脂ペーストを得るなどがある。
Further, in the present invention, hexachloroplatinic acid, which is generally used in hydrosilylation reaction, may be used as the platinum-based catalyst, but since the field of use is the electric / electronic field, corrosive ions are as much as possible. It is preferable to use a complex of platinum with an organic compound or an organic silicone compound from the viewpoint of a small amount and catalytic activity. Specifically, there are platinum and cyclo (vinylmethylsiloxane) complex, platinum and divinyltetramethyldisiloxane complex, platinum and octyl alcohol complex, etc. However, platinum and cyclo (vinylmethylsiloxane) are complex in that they react during curing. ) And a complex of platinum and divinyltetramethyldisiloxane. The compounding amount of the platinum-based catalyst is 0.1 to 100 ppm in terms of platinum in the total conductive resin paste, but if it is less than 0.1 ppm, the conductive resin paste will not be sufficiently cured or the curing time will be long. Become.
If it exceeds 100 ppm, the amount of heat generated by the reaction during the curing of the conductive resin paste becomes too large, and voids are likely to occur in the cured product, resulting in a decrease in adhesive strength, deterioration in electrical conductivity and thermal conductivity. In the present invention, a flexibility-imparting agent, a defoaming agent, a coupling agent, etc. can be used if necessary. The method for producing the conductive resin paste includes, for example, premixing the respective components, kneading using a three-roll mill, and degassing under vacuum after the kneading to obtain a resin paste.

【0011】以下実施例を用いて本発明を具体的に説明
する。配合割合は重量部で示す。 実施例1〜4 粒径1〜30μmで、平均粒径3μmのフレーク状銀
粉、テトラメチルシクロテトラシロキサン(東芝シリコ
ーン(株)・製TSL8249)(以下シリコーン化合物
A)、ヘキサメチルシクロテトラシロキサン(東芝シリ
コーン(株)・製TSL8234)(以下シリコーン化合
物B)、2−ヒドロキシ−1,3−ジメタクリロキシプ
ロパン(沸点100℃以上)(以下メタクリル化合物
A)、白金とシクロ(ビニルメチルシロキサン)との錯
体のシクロ(ビニルメチルシロキサン)溶液(白金濃度
1重量%)(以下白金触媒A)及びカップリング剤(信
越化学工業(株)・製、KBM−503)を表1に示す割
合で配合し、3本ロールで混練して導電性樹脂ペースト
を得た。この導電性樹脂ペーストを真空チャンバーに
て、2mmHgで30分間脱泡した後以下の方法により
各種性能を評価した。
The present invention will be specifically described below with reference to examples. The blending ratio is shown in parts by weight. Examples 1 to 4 Flake silver powder having a particle size of 1 to 30 μm and an average particle size of 3 μm, tetramethylcyclotetrasiloxane (TSL8249 manufactured by Toshiba Silicone Co., Ltd.) (hereinafter Silicone Compound A), hexamethylcyclotetrasiloxane (Toshiba Silicone Co., Ltd. TSL8234) (hereinafter silicone compound B), 2-hydroxy-1,3-dimethacryloxypropane (boiling point 100 ° C. or higher) (hereinafter methacrylic compound A), platinum and cyclo (vinylmethylsiloxane) A cyclo (vinylmethylsiloxane) solution of the complex (platinum concentration 1% by weight) (hereinafter platinum catalyst A) and a coupling agent (Shin-Etsu Chemical Co., Ltd., KBM-503) were mixed in the proportions shown in Table 1, The mixture was kneaded with three rolls to obtain a conductive resin paste. The conductive resin paste was degassed in a vacuum chamber at 2 mmHg for 30 minutes, and then various performances were evaluated by the following methods.

【0012】ゲルタイム:ペースト1ccを150℃の
熱板上に置き、スパチュラでかきまぜペーストが流動性
を示さなくなるまでの時間を測定した。 粘 度:E型粘度計(3°コーン)を用い25℃、
2.5rpmでの値を測定し粘度とした。 糸引き性 :導電性樹脂ペーストの中へ直径1mmΦの
ピンを深さ5mmまで入れ、ピンを300mm/分の速
度で引き上げ、ペーストが切れたときの高さを測定し
た。 体積抵抗率:スライドガラス上にペーストを幅4mm、
厚さ30μmに塗布し、150℃熱板上30秒間硬化し
た後硬化物の体積抵抗率を測定した。 接着強度 :5×5mmのシリコンチップをペーストを
用いて、銅フレームにマウントし150℃熱板上30秒
間硬化した。硬化後プッシュプルゲージを用い240℃
での熱時ダイシェア強度を測定した。 ボイド :接着強度測定前のサンプルを軟X線透過法
によりボイドの観察を行った。 不純物 :硬化・粉砕したペースト2gおよび純水4
0mlを125℃、20時間抽出して得られた抽出液の
ナトリウムおよび塩素イオン濃度をイオンクロマトグラ
フィーにて測定した。
Gel time: 1 cc of paste was placed on a hot plate at 150 ° C., and the time until the paste was agitated with a spatula until it showed no fluidity was measured. Viscosity: E type viscometer (3 ° cone) at 25 ° C,
The value at 2.5 rpm was measured and used as the viscosity. String pullability: A pin having a diameter of 1 mmΦ was inserted into a conductive resin paste to a depth of 5 mm, the pin was pulled up at a speed of 300 mm / min, and the height when the paste was broken was measured. Volume resistivity: paste 4 mm wide on glass slide,
After being applied to a thickness of 30 μm and cured on a hot plate at 150 ° C. for 30 seconds, the volume resistivity of the cured product was measured. Adhesive strength: A 5 × 5 mm silicon chip was mounted on a copper frame using a paste and cured on a hot plate at 150 ° C. for 30 seconds. After curing 240 ° C using push-pull gauge
The die shear strength during heating was measured. Void: The sample before adhesive strength measurement was observed for voids by the soft X-ray transmission method. Impurities: 2 g of hardened and ground paste and 4 pure water
The sodium and chloride ion concentrations of the extract obtained by extracting 0 ml at 125 ° C. for 20 hours were measured by ion chromatography.

【0013】実施例5 用いるアルケニル基を有する化合物として、2,2−ビ
ス(4−(メタクリロキシジエトキシ)フェニル)プロ
パン(沸点100℃以上)(以下メタクリル化合物B)
を併用した他は、実施例1〜4と全く同様にして導電性
樹脂ペーストを作製し評価を行った。 実施例6 用いる白金系触媒としては、白金とジビニルテトラメチ
ルジシロキサン錯体のキシレン溶液(白金濃度3重量
%)(以下白金触媒B)を用いた他は実施例1〜4と全
く同様にして導電性樹脂ペーストを作製し評価を行っ
た。 比較例1〜6 表2に示す配合割合で実施例と全く同様にして導電性樹
脂ペーストを作製した。なお比較例5ではシクロシロキ
サンの替わりに、1,1,3,3−テトラメチルジシロ
キサン(以下シリコーン化合物C)用い、比較例6では
アルケニル基を有する化合物としてメトキシジエチレン
グリコールメタクリレート(沸点100℃以上)(以下
メタクリル化合物C)を使用した。比較例1〜3は、硬
化しなかったので特性の評価は不可能だった。評価結果
を表2に示す。
Example 5 As a compound having an alkenyl group to be used, 2,2-bis (4- (methacryloxydiethoxy) phenyl) propane (boiling point: 100 ° C. or higher) (hereinafter, methacrylic compound B)
Conductive resin paste was prepared and evaluated in exactly the same manner as in Examples 1 to 4 except that was also used. Example 6 As the platinum-based catalyst to be used, conduction was conducted in the same manner as in Examples 1 to 4 except that a xylene solution of platinum and a divinyltetramethyldisiloxane complex (platinum concentration 3% by weight) (hereinafter platinum catalyst B) was used. A resinous paste was prepared and evaluated. Comparative Examples 1 to 6 Conductive resin pastes were prepared with the compounding ratios shown in Table 2 in exactly the same manner as in the examples. In Comparative Example 5, 1,1,3,3-tetramethyldisiloxane (hereinafter referred to as silicone compound C) was used instead of cyclosiloxane, and in Comparative Example 6, methoxydiethylene glycol methacrylate (boiling point 100 ° C. or higher) as a compound having an alkenyl group. (Hereinafter, methacrylic compound C) was used. Comparative Examples 1 to 3 did not cure, and therefore the evaluation of characteristics was impossible. The evaluation results are shown in Table 2.

【0014】[0014]

【表1】 [Table 1]

【0015】[0015]

【表2】 [Table 2]

【0016】[0016]

【発明の効果】本発明の導電性樹脂ペーストは、硬化性
に優れており150℃、30秒以下での硬化が可能であ
る。またディスペンス塗布時の作業性が良好で、イオン
性不純物が少く、42合金等の金属フレーム、セラミッ
ク基板、ガラスエポキシ等の有機基板へのIC、LSI
等の半導体素子の接着に用いることができる。
The conductive resin paste of the present invention has excellent curability and can be cured at 150 ° C. for 30 seconds or less. In addition, the workability at the time of dispensing is good, the amount of ionic impurities is small, and the IC, LSI to the metal frame such as 42 alloy, the ceramic substrate, the organic substrate such as glass epoxy, etc.
It can be used for bonding semiconductor elements such as.

Claims (4)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 (A)銀粉、(B)式(1)で示される
シクロシロキサン、(C)沸点が100℃以上で、かつ
1分子内に2個以上のアルケニル基を有する化合物、
(D)白金系触媒を必須成分とし、かつ全導電性樹脂ペ
ースト中に(A)成分を60〜90重量%、(B)成分
を1〜20重量%、(C)成分を5〜25重量%、
(D)成分を白金換算で0.1〜100ppm含み、
(C)成分が、2−ヒドロキシ−1,3−ジメタクリロ
キシプロパン、2,2−ビス(4−(メタクリロキシジ
エトキシ)フェニル)プロパン、1,6−ヘキサンジオ
ールジメタクリレート又は2,2−ビス(4−(メタク
リロキシエトキシ)フェノールプロパンであることを特
徴とする導電性樹脂ペースト。 【化1】
1. (A) silver powder, (B) cyclosiloxane represented by the formula (1), (C) a compound having a boiling point of 100 ° C. or higher and having two or more alkenyl groups in one molecule,
(D) Platinum-based catalyst is an essential component, and (A) component is 60 to 90% by weight, (B) component is 1 to 20% by weight, and (C) component is 5 to 25% by weight in the total conductive resin paste. %,
The component (D) 0.1~100ppm seen including in terms of platinum,
Component (C) is 2-hydroxy-1,3-dimethacryloyl
Xypropane, 2,2-bis (4- (methacryloxydiene
Ethoxy) phenyl) propane, 1,6-hexanedio
Dimethacrylate or 2,2-bis (4- (methacryl
A conductive resin paste which is riloxyethoxy) phenolpropane . [Chemical 1]
【請求項2】 式(1)が式(2)である請求項1記載
の導電性樹脂ペースト。 【化2】
2. The conductive resin paste according to claim 1, wherein formula (1) is formula (2). [Chemical 2]
【請求項3】 白金系触媒が、白金とシクロ(ビニルメ
チルシロキサン)との錯体である請求項1、又は請求項
2記載の導電性樹脂ペースト。
3. The conductive resin paste according to claim 1, wherein the platinum-based catalyst is a complex of platinum and cyclo (vinylmethylsiloxane).
【請求項4】 白金系触媒が、白金とジビニルテトラメ
チルジシロキサンとの錯体である請求項1、又は請求項
2記載の導電性樹脂ペースト。
4. The conductive resin paste according to claim 1, wherein the platinum-based catalyst is a complex of platinum and divinyltetramethyldisiloxane.
JP22322495A 1995-08-31 1995-08-31 Conductive resin paste Expired - Fee Related JP3403274B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP22322495A JP3403274B2 (en) 1995-08-31 1995-08-31 Conductive resin paste

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP22322495A JP3403274B2 (en) 1995-08-31 1995-08-31 Conductive resin paste

Publications (2)

Publication Number Publication Date
JPH0967518A JPH0967518A (en) 1997-03-11
JP3403274B2 true JP3403274B2 (en) 2003-05-06

Family

ID=16794745

Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
JP (1) JP3403274B2 (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4238384B2 (en) * 1998-07-31 2009-03-18 東レ株式会社 Photosensitive conductive paste and method for producing electrode for plasma display
US6706219B2 (en) * 1999-09-17 2004-03-16 Honeywell International Inc. Interface materials and methods of production and use thereof
JP2006143978A (en) * 2004-11-25 2006-06-08 Ge Toshiba Silicones Co Ltd Heat conductive silicone composition
JP2011208278A (en) * 2010-03-10 2011-10-20 Dowa Holdings Co Ltd Flaky silver powder and method for producing the same

Also Published As

Publication number Publication date
JPH0967518A (en) 1997-03-11

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