JPS63278987A - Two-pack low-temperature curable electroconductive epoxy adhesive - Google Patents
Two-pack low-temperature curable electroconductive epoxy adhesiveInfo
- Publication number
- JPS63278987A JPS63278987A JP11346987A JP11346987A JPS63278987A JP S63278987 A JPS63278987 A JP S63278987A JP 11346987 A JP11346987 A JP 11346987A JP 11346987 A JP11346987 A JP 11346987A JP S63278987 A JPS63278987 A JP S63278987A
- Authority
- JP
- Japan
- Prior art keywords
- adhesive
- curing
- epoxy resin
- silver
- filler
- 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.)
- Granted
Links
- 229920006332 epoxy adhesive Polymers 0.000 title claims description 11
- 239000000853 adhesive Substances 0.000 claims abstract description 28
- 230000001070 adhesive effect Effects 0.000 claims abstract description 28
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052709 silver Inorganic materials 0.000 claims abstract description 19
- 239000004332 silver Substances 0.000 claims abstract description 19
- 239000000945 filler Substances 0.000 claims abstract description 16
- 239000003822 epoxy resin Substances 0.000 claims abstract description 13
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 13
- 229920005989 resin Polymers 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims abstract description 11
- 229920000768 polyamine Polymers 0.000 claims abstract description 7
- 125000001931 aliphatic group Chemical group 0.000 claims abstract description 6
- 239000003085 diluting agent Substances 0.000 claims abstract description 6
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000011230 binding agent Substances 0.000 claims abstract description 5
- 238000004898 kneading Methods 0.000 claims abstract description 5
- 239000002245 particle Substances 0.000 claims abstract description 5
- 238000001723 curing Methods 0.000 claims description 40
- 238000010438 heat treatment Methods 0.000 claims description 10
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 9
- 238000013007 heat curing Methods 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 239000011231 conductive filler Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 10
- 239000004841 bisphenol A epoxy resin Substances 0.000 abstract 3
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000002075 main ingredient Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005538 encapsulation Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229930185605 Bisphenol Natural products 0.000 description 1
- 229910000906 Bronze Inorganic materials 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000005856 abnormality Effects 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000010974 bronze Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- -1 i.e. Substances 0.000 description 1
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010943 off-gassing Methods 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/30—Assembling printed circuits with electric components, e.g. with resistor
- H05K3/32—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits
- H05K3/321—Assembling printed circuits with electric components, e.g. with resistor electrically connecting electric components or wires to printed circuits by conductive adhesives
Landscapes
- Adhesives Or Adhesive Processes (AREA)
- Epoxy Resins (AREA)
Abstract
Description
【発明の詳細な説明】
（１）発明の目的
［産業上の利用分野］
本発明は、リードワイヤーの接点接着、磁気・セラミッ
クの充填封入、シルクスクリーン印刷、回路基板の補修
、成形カーボンと金属の接着、各種電子素子をリードフ
レームやアルミナ基板への接着、ＰＴＣと金属の面接着
、ネサガラス間の接着等多用途に供される二液式低温加
熱硬化型導電性エポキシ系接着剤に関する。Detailed Description of the Invention (1) Purpose of the Invention [Field of Industrial Application] The present invention is applicable to lead wire contact adhesion, magnetic/ceramic filling and encapsulation, silk screen printing, circuit board repair, molded carbon and metal The present invention relates to a two-component low-temperature heat-curing conductive epoxy adhesive that can be used for a variety of purposes, such as adhesion of various electronic devices to lead frames and alumina substrates, surface adhesion of PTC and metal, and adhesion between Nesa glass.
［従来の技術］
この種二液式導電性エポキシ系接着剤は、従来ハンダづ
けができなかったプラスチック類（エポキシ・フェノー
ル樹脂等）の導電接着や液晶表示管に使うネサガラスの
接着、マイクロモーターに使うリン青銅とカーボンブラ
シの接着、水晶振動子、Ｓｄｃメーターなどのリード線
接着等に欠くことができない材料である。[Prior technology] This type of two-component conductive epoxy adhesive can be used for conductive bonding of plastics (epoxy, phenol resin, etc.) that could not be soldered in the past, for bonding Nesa glass used in liquid crystal display tubes, and for micro motors. It is an indispensable material for adhering phosphor bronze and carbon brushes, and for adhering lead wires for crystal resonators, SDC meters, etc.
特に、半導体工業における最近の発展はめざましく、次
々にＩＣやＬＳＩが開発され、量産化され続けているが
、これ等の半導体チップ（シリコンウェハー）のリード
フレームへの接着には従来Ａｕ−８ｉ共品による方法が
とられていたが、低コスト化・生産性向上を目的として
エポキシ樹脂に銀粉を混練した導電性接着剤が多用され
るようになり、現在ダイボンディング方式の中で最も有
力視されている。In particular, recent developments in the semiconductor industry have been remarkable, with ICs and LSIs being developed one after another and being mass-produced. However, in order to reduce costs and improve productivity, conductive adhesives made of epoxy resin mixed with silver powder have come into widespread use, and are now considered the most promising method among die bonding methods. ing.
しかしながらこの種従来の二液式高温加熱型導電性エポ
キシ系接着剤は銀含有ｍが７０〜９０重量％が一般的で
あり銀フィラーエポキシ樹脂と硬化剤の混合比を１＝１
又は１：２として希釈溶剤にＳＨシンナーを用いており
、粘度が１０万〜２０万ＣＰＳを示し硬化条件も１００
℃〜１３０℃Ｘ１Ｈ（時間）か１５０℃×０゜５日であ
り、粘度が高く混練性は悪く接着力に関係する濡れ性も
悪い。即ちエポキシ系導電性接着剤の配合設計をする際
、通常、原料エポキシ樹脂の粘度が高いため銀フィラー
と混練した場合さらに粘度が上昇し、マイクロディスペ
ンサー、シルクスクリーン印刷等による塗布作業性がい
ちじるしく悪くなる場合があるため溶剤を配合しなけれ
ばならず、その結果被塗物を面接着する場合、溶剤が含
まれていると加熱硬化した際、硬化剤が発砲しその結果
として特性劣化（導電性のバラツキ、接着強度の低下）
が起り易く、電子部品の組立接着に使われる導電性接着
剤には無溶剤が望ましいこと、また気密性の高い部品内
で用いる場合微ｍの揮発分がスイッチ接点部や金属部に
悪い影響を及ぼす場合があるため注意が必要であること
、特にＩＣやＬＳＩのダイボンディング用のものにはア
ウトガスがないものが要求されること等を知りながら粘
度低下のため溶剤を使用せざるを得ず、リード線の接着
のようにオーブン状態で接着する場合は溶剤の添加によ
る粘度調整で作業性が改善されると言えどもＩＣ関係の
接着や半導体素子の接着は面接着が多く、また接着後は
合成樹脂等で気密封止されるので残留溶剤による不良原
因となり、溶剤含有接着剤は好ましくない。However, this type of conventional two-component high-temperature heating conductive epoxy adhesive generally has a silver content of 70 to 90% by weight, and the mixing ratio of silver filler epoxy resin and curing agent is 1=1.
Or, SH thinner is used as the dilution solvent as 1:2, the viscosity is 100,000 to 200,000 CPS, and the curing conditions are also 100,000 to 200,000 CPS.
°C to 130°C x 1 hour (hour) or 150°C x 0° for 5 days, the viscosity is high, the kneading properties are poor, and the wettability related to adhesive strength is also poor. In other words, when designing the formulation of epoxy conductive adhesives, the viscosity of the raw material epoxy resin is usually high, so when mixed with silver filler, the viscosity increases further, making application workability with microdispensers, silk screen printing, etc. extremely poor. As a result, when surface adhering the coated object, if a solvent is included, the curing agent will foam when heated and hardened, resulting in property deterioration (conductivity). variation, decrease in adhesive strength)
Solvent-free conductive adhesives are desirable for use in assembling electronic parts, and when used in highly airtight parts, minute amounts of volatile matter can have a negative effect on switch contacts and metal parts. Although I knew that I needed to be careful because it could cause harmful effects, and that products with no outgassing were required especially for die bonding of ICs and LSIs, I had no choice but to use a solvent to reduce the viscosity. When adhering in an oven, such as when adhering lead wires, workability can be improved by adjusting the viscosity by adding a solvent. Since the adhesive is hermetically sealed with a resin or the like, residual solvent may cause defects, so adhesives containing solvents are not preferred.
加えて硬化温度が高温加熱硬化型でしかも長時間加熱し
なければならないため接着剤自体の劣化変質のため引張
り剪断強度も２９〜６２ＫＷ／７の値しか示さず、さら
に致命的欠陥は接着対象やその周辺の電子部品群に熱的
悪影響を及ぼし電気的特性を悪化する欠点である。In addition, since the curing temperature is a high temperature heat curing type and it must be heated for a long time, the adhesive itself deteriorates and changes in quality, resulting in a tensile shear strength of only 29 to 62 KW/7. This is a drawback in that it has an adverse thermal effect on surrounding electronic components and deteriorates their electrical characteristics.
［発明が解決しようとする問題点］
本発明は従来の欠点に鑑み接着剤粘度を低めて混練性を
高め、接着力を増大する濡れ性および延展性を良好にし
て低硬化温度と短時間加熱の硬化条件に大幅に改善し接
着時の熱的悪影響を可及的に抑制した二液式低温加熱硬
化型導電性エポキシ系接着剤を提供せんとするものであ
る。[Problems to be Solved by the Invention] In view of the conventional drawbacks, the present invention lowers the adhesive viscosity to improve kneading properties, improves wettability and spreadability to increase adhesive strength, and achieves a low curing temperature and short heating time. The purpose of the present invention is to provide a two-component low temperature heat-curable conductive epoxy adhesive which has significantly improved curing conditions and suppresses as much as possible adverse thermal effects during adhesion.
（２）発明の構成
［問題点を解決するための手段］
本発明の二液式低湿加熱硬化型導電性エポキシ系接着剤
は、導電性フィラーとして粒径５〜３０μｍの銀フィラ
ーとこれを分散混練したバインダー樹脂との用旦比を９
０〜７５：１０〜２５としフェニグリシジルエーテル等
の適量の反応性希釈剤を加えたビスフェノールＡ系銀フ
ィラーエポキシ樹脂に、使用に当り添加するトリエチレ
ンテトラアミン笠の脂肪族ポリアミン系硬化剤とのＭ位
％を前記ビスフェノールΔ系銀フィラーエポキシ樹脂１
００部に対し２〜３部として、１万〜５万ＣＰＳに低粘
度化しかつ硬化温度を５０℃〜８０℃にすることにより
接着力を増強してなる。(2) Structure of the invention [Means for solving the problems] The two-component low-humidity heat-curable conductive epoxy adhesive of the present invention includes silver filler with a particle size of 5 to 30 μm as a conductive filler and a silver filler dispersed therein. The usage ratio with the kneaded binder resin is 9.
0-75: Bisphenol A-based silver filler epoxy resin with a ratio of 10-25 and an appropriate amount of reactive diluent such as pheniglycidyl ether, and an aliphatic polyamine-based curing agent of triethylenetetraamine caps added during use. M% of the bisphenol Δ-based silver filler epoxy resin 1
The adhesive strength is increased by reducing the viscosity to 10,000 to 50,000 CPS and setting the curing temperature to 50°C to 80°C.
［実 施 例］ 本発明の実施例を以下に説明する。[Example] Examples of the present invention will be described below.
本発明の二液式低温加熱硬化型導電性エポキシ系接着剤
は、銀フィラーのエポキシ樹脂（以下主剤とも言う）ポ
リアミン硬化型であって粘度１万〜５万ＣＰＳのクリー
ム状のペーストで作業性が良く、揮発性溶剤を全く含ま
ないため、硬化の際収縮がなく、硬化模の性能は高い導
電性と強い接着力を持ち、さらに充填、封入に対しても
適性を有する。The two-component low-temperature heat-curing conductive epoxy adhesive of the present invention is a silver-filler epoxy resin (hereinafter also referred to as the main ingredient) polyamine-curing type, and is a cream-like paste with a viscosity of 10,000 to 50,000 CPS and is easy to work with. Since it contains no volatile solvents, there is no shrinkage during curing, and the cured model has high conductivity and strong adhesive strength, and is also suitable for filling and encapsulation.
主剤となるバインダー役のエポキシ樹脂は１．粘度の調
整および硬化樹脂に可撓性を付与する反応性希釈剤によ
って調整された低粘度の液体である。The epoxy resin that serves as the main binder is 1. It is a low viscosity liquid prepared with reactive diluents that adjust the viscosity and add flexibility to the cured resin.
エポキシ樹脂はビスフェノールＡ系をベースとして、そ
の基本構造は次に示ず通りである。The epoxy resin is based on bisphenol A, and its basic structure is as shown below.
ＯＣ市 ０１１
主剤と混合される導電体、即ちエポキシ樹脂と精密に混
練り分散を行なう粒径５〜３０μｍ好ましくは５〜１０
μｍの銀粉には電解銀粉並びに還元銀粉を用いるが主剤
に対する銀フィラーの配分重量比は１０〜２５ ： ９
０〜７５．好ましくは１７：８３である。OC City 011 Particle size of 5-30 μm, preferably 5-10 μm, which is precisely kneaded and dispersed with the conductor mixed with the base material, i.e., epoxy resin.
Electrolytic silver powder and reduced silver powder are used for the μm silver powder, and the weight ratio of silver filler to the main ingredient is 10 to 25:9.
0-75. Preferably it is 17:83.
電解銀粉は、電気銀を再電解して樹枝状に析出させたも
ので、純度が高く成形性が良好な銀粉末である。Electrolytic silver powder is produced by re-electrolyzing electrolytic silver to precipitate it in a dendritic form, and is a silver powder with high purity and good moldability.
また還元銀粉は、銀塩水流液にホルマリン等の還元剤を
加えて還元析出させて、これを乾燥し粉粒状として得ら
れたものを用いる。Further, the reduced silver powder is obtained by adding a reducing agent such as formalin to a silver salt aqueous solution, reducing and precipitating it, and drying this to obtain a powder.
これ等の銀粉の性状としては、粒度がこまかく分散性に
すぐれ、凝集力がないこと等が要求される。The properties of these silver powders include fine particle size, excellent dispersibility, and no cohesion.
硬化剤は、一般的には混合物の粘度、可使時間（ポット
ライフ）、硬化条件、並びに接着力等を基準に選定され
ざらにカブレ等が生じにくく少量で硬化反応が行ない得
るトリエチレンテトラアミン等の脂肪族ポリアミン系硬
化剤が用いられる。The curing agent is generally selected based on the viscosity of the mixture, pot life, curing conditions, and adhesive strength, etc. Triethylenetetraamine, which is less likely to cause blistering and can carry out the curing reaction in a small amount. An aliphatic polyamine curing agent such as the following is used.
トリエチレンテトラアミン（Ｔ Ｔ Ａ −ｔｒｉｅｔ
ｈｙｌｅｎｅ ｔｅｔｒａｍｉｎｅ ）の化学構造式は
次に示す通りである。Triethylenetetraamine (TTA-triet
The chemical structural formula of hylene tetramine is as shown below.
トドＮ （Ｊト ＣトｂＮ Ｃ）し Ｃト
ドＮ （Ｊト ＣトレＮ １−１？
所で混合される主剤と硬化剤は化学反応によって硬化が
行なわれるが、硬化反応に化学当量が必要となる。つま
りエポキシ樹脂のエポキシ基とポリアミンのアミン基が
過不足なく結合し三次元的な強い構造になるにはそれぞ
れの化学当量が篩用されなければならないが、主剤樹脂
１００部に対して硬化剤の量を変えた時の接着力の試験
結果である相関特性線図を第１図に示す。TODON (JTO CTObN C) CTODON (JTO CTREN 1-1? The main agent and curing agent that are mixed together are cured by a chemical reaction, but a chemical equivalent is required for the curing reaction. In other words, in order for the epoxy groups of the epoxy resin and the amine groups of the polyamine to bond in just the right amount and form a strong three-dimensional structure, chemical equivalents of each must be used. FIG. 1 shows a correlation characteristic diagram showing the test results of adhesion strength when the amount of .
当該第１図に基づき主剤１００部（重量）に対し硬化剤
２部（重量）を最適基準値として算出した。従って第１
図に示すよう、混合される主剤と硬化剤の配分比が基準
値より多過ぎても少な過ぎても接着力に影響が見られる
。Based on FIG. 1, 2 parts (by weight) of the curing agent was calculated as the optimum standard value for 100 parts (by weight) of the main agent. Therefore, the first
As shown in the figure, the adhesion strength is affected if the distribution ratio of the base agent and curing agent to be mixed is too much or too little than the standard value.
［発明の特性］
導電性接着剤に要求される基本特性は銀フィラーの形状
例えばウロコ状および粒径による導電性と樹脂による接
着強度である。この２つの特性が経時で劣化せずに長期
の信頼性を保つことが重要である。[Characteristics of the Invention] The basic characteristics required of a conductive adhesive are conductivity due to the shape of the silver filler, such as scale-like shape and particle size, and adhesive strength due to the resin. It is important that these two characteristics do not deteriorate over time and maintain long-term reliability.
本発明の特性の試験例を以下に説明する。Test examples of the characteristics of the present invention will be explained below.
■一般的性状 次の第１表に示す通りである。■General properties As shown in Table 1 below.
■硬化条件
加熱温度と時間の組合せによって決定され、例えば常温
（２５℃）でも硬化は進むが時間は４８時間以、トを要
し、しかも８Ｉ電度は満足する結果を得られない。(2) Curing conditions It is determined by the combination of heating temperature and time. For example, although curing proceeds at room temperature (25° C.), it takes more than 48 hours, and 8I electric power does not give satisfactory results.
従って最低でも５０℃以上の加熱を必要とする。Therefore, heating to at least 50°C is required.
主剤：硬化剤−１００：２で混合した場合の試験結果を
次の第２表に示す。The following Table 2 shows the test results when the base resin: curing agent was mixed at a ratio of 100:2.
第２表 る。Table 2 Ru.
さらに主剤：硬化剤＝１００：２の配合比で混合した場
合の硬化温度と体積固有抵抗の関係を第２図に、また低
湿加熱５０’Ｃにおいて加熱時間を変えた場合の導電度
の関係を第３図にそれぞれ示す。Furthermore, Figure 2 shows the relationship between curing temperature and volume resistivity when mixing base resin: curing agent at a blending ratio of 100:2, and the relationship between conductivity when heating time is varied in low humidity heating at 50'C. Each is shown in Figure 3.
■接着強度
主剤：硬化剤−１００：２の配合比で混合し硬化条件と
して８０’ＣＸ１５分、常温２４時間放１！４１に測定
した場合の試験結果を次の第３表に示す。(2) Adhesive Strength The following Table 3 shows the test results when the adhesive strength was measured at a ratio of 100:2 of main ingredient: curing agent and curing conditions were 80'C x 15 minutes and 1.41 hours left at room temperature.
第３表 但し＊印は接着剤層内部の破壊をいう。Table 3 However, *mark indicates damage inside the adhesive layer.
■耐熱性 １９０℃の耐熱試験では接着強度はほとんど変らない。■Heat resistance In the heat resistance test at 190°C, the adhesive strength hardly changes.
主剤：硬化剤−１００：２の配合比で混合し硬化条件と
して８０℃×１５分、常温２４時間放置後に耐熱性試験
をおこなった結果を次の第４表に示す。Table 4 below shows the results of a heat resistance test after mixing the base resin: curing agent at a blending ratio of 100:2, curing at 80° C. for 15 minutes, and leaving it at room temperature for 24 hours.
第４表 但し試料はスチール／スチールを接着した。Table 4 However, the sample was steel/steel bonded.
■温度と強度の関係
主剤：硬化剤−１００：２の配合比で混合し硬化条件と
して８０℃×１５分、常温２４時間放置後に測定した場
合における各温度と１時間３０分常温放置後の強度試験
結果を第４図に示す。■Relationship between temperature and strength Main ingredient: Curing agent - Mixed at a blending ratio of 100:2, curing conditions were 80℃ x 15 minutes, and strength after being left at room temperature for 24 hours and at each temperature and strength after being left at room temperature for 1 hour and 30 minutes. The test results are shown in Figure 4.
■塗厚・幅と体積固有抵抗の関係
主剤：硬化剤−１００：２の配合比で混合し硬化条件と
して８０℃×１５分、常温２４時間放置後の測定試験結
果を次の第５表に示す。■Relationship between coating thickness/width and volume resistivity Main agent: Curing agent - Mixed at a blending ratio of 100:2, curing conditions were 80℃ x 15 minutes, and measurement test results after being left at room temperature for 24 hours are shown in Table 5 below. show.
第５表 但し試料は基板ＰＭＭＡ （アクリル板）に塗る。Table 5 However, the sample is applied to the substrate PMMA (acrylic board).
［発明の使用法］ 本発明接着剤の使用例を以下に説明する。[How to use the invention] Examples of use of the adhesive of the present invention will be explained below.
良い性能を発揮させるためには主剤と硬化剤を正しく計
ａし、良く撹拌混合することが肝要である。In order to exhibit good performance, it is important to accurately measure the base agent and curing agent and to mix and stir well.
■混合比 主剤：硬化剤＝１００：２（１−ｍ％）■混合の目安 主剤 ・・・１ｇ 硬化剤・・・１滴（約０．０２９＞ 両者を良く混ぜる。■Mixing ratio Main agent: hardening agent = 100:2 (1-m%) ■ Mixing guideline Main ingredient...1g Hardening agent...1 drop (approx. 0.029> Mix both well.
■硬化条件（基準［）
５０℃×２時間・１ 、５ ＸＩＯ”Ω−ｃｒｓ８０℃
Ｘ１５分−５ Ｘ １０’Ω−α■ポットライフの持続
新らしく所定量の主剤：硬化剤を混合し、すみやかに冷
凍を行なう。例えば−２０℃の冷凍庫へ１２０時間（５
日間）放置して、のち取り出し撹拌しながら常温に戻し
通常の硬化手続に従って使用した結果性能に異常は認め
られなかった。■Curing conditions (standard [) 50℃×2 hours・1,5 XIO”Ω-crs80℃
x 15 minutes -5 For example, store it in a -20℃ freezer for 120 hours (5
After leaving it for several days), it was taken out and returned to room temperature with stirring, and used according to the normal curing procedure. No abnormality was observed in the performance.
■溶剤による粘度の調整
デイマベンシングの都合上、止む無くさらに粘度の調整
を必要とするときは本発明の混合物へ５％（重量）まで
トルエン、または酢酸エチルで希釈することができる。(2) Adjustment of viscosity using a solvent When further adjustment of the viscosity is unavoidably necessary due to dimmervencing, the mixture of the present invention can be diluted to 5% (by weight) with toluene or ethyl acetate.
（３）発明の効果
かくして本発明の接着剤は、■低温加熱５０〜８０℃で
硬化が行なわれる。■クリーム状ペーストで混合し易く
、ダレがない。■硬化後の収縮がな（充填・封入に適す
る。■安定した高い導電性が得られる。■接着力が強く
多くの新素材に適合する。■耐熱・耐湿性にすぐれてい
る。■溶剤により粘度の調整ができる。■ディスペンス
性が良い。■肉盛り隠蔽力に優れている。■棚寿命が長
く常温で約１カ年間有効である等の従来品に比べて種々
の特徴を有する。(3) Effects of the Invention Thus, the adhesive of the present invention is cured at low temperature heating of 50 to 80°C. ■It is a creamy paste that is easy to mix and does not drip. ■ No shrinkage after curing (suitable for filling and encapsulation. ■ Stable and high conductivity is obtained. ■ Strong adhesion and compatible with many new materials. ■ Excellent heat and moisture resistance. ■ Can be used with solvents The viscosity can be adjusted.■Good dispensing properties.■Excellent overlay hiding power.■It has a variety of features compared to conventional products, such as long shelf life and is effective for approximately one year at room temperature.
本発明は、低温硬化かつ短時間加熱であるため、接着剤
自体および接着対象部品や周辺の部品に熱的悪彰胃を及
ぼすことなく品質保持と信頼性を高め概して従来品に比
べ接着強度を２０％以上向上ししかも作業性を改善して
省エネ、省コストを果しご産体制を確立し得る等電子工
業界等に優れた技術革新インパクト効果を与える。Since the present invention cures at a low temperature and heats for a short time, it does not cause thermal damage to the adhesive itself, the parts to be bonded, or surrounding parts, maintains quality and reliability, and generally has higher adhesive strength than conventional products. It has an excellent technological innovation impact effect on the electronic industry, such as improving workability by more than 20%, saving energy and cost, and establishing a production system.
第１図は、本発明の実施例において樹脂１００部に対し
て硬化剤の量を変えたときの接着力相関特性線図、第２
図は同・硬化温度と体積固有抵抗の相関特性線図、第３
図は同・低温加熱５０℃において加熱時間を変えた場合
の導電度の相関特性線図、第４図は同・各温度と１時間
３０分常温放置後の引張り剪断強度との相関特性線図で
ある。
第１図
第２図
第３図
ｈｏ飴峙間（ｈｒｓ）
第４図
加８彊崖（６ｃ）FIG. 1 is an adhesive force correlation characteristic diagram when the amount of curing agent is varied with respect to 100 parts of resin in the example of the present invention, and FIG.
The figure is the same correlation characteristic diagram of curing temperature and volume resistivity, 3rd
The figure is a correlation characteristic diagram of conductivity when heating time is changed at the same low temperature heating at 50℃, and Figure 4 is a correlation characteristic diagram of the same temperature and tensile shear strength after being left at room temperature for 1 hour and 30 minutes. It is. Fig. 1 Fig. 2 Fig. 3 Ho Amechi interval (hrs) Fig. 4 Ka8jiang cliff (6c)
Claims (1)
ーとこれを分散混練したバインダー樹脂との重量比を９
０〜７５：１０〜２５とし適量の反応性希釈剤を加えた
ビスフェノールＡ系銀フィラーエポキシ樹脂に、使用に
当り添加する脂肪族ポリアミン系硬化剤との重量％を前
記ビスフェノールＡ系銀フィラーエポキシ樹脂１００部
に対し２〜３部として、低粘度化しかつ硬化温度を５０
℃〜８０℃にすることにより接着力を増強してなる二液
式低温加熱硬化型導電性エポキシ系接着剤 ２、反応性希釈剤としては、フェニグリシジルエーテル
を採用してなる特許請求の範囲第１項記載の二液式低温
加熱硬化型導電性エポキシ系接着剤 ３、脂肪族ポリアミン系硬化剤としては、トリエチレン
テトラアミンを採用してなる特許請求の範囲第１項又は
第２項記載の二液式低温加熱硬化型導電性エポキシ系接
着剤 ４、低粘度化は、混練性が高くかつ接着力増大の濡れ性
が良好な１万〜５万ＣＰＳとしてなる特許請求の範囲１
項、第２項又は第３項記載の二液式低温加熱硬化型導電
性エポキシ系接着剤[Claims] 1. The weight ratio of silver filler with a particle size of 5 to 30 μm as a conductive filler and a binder resin in which this is dispersed and kneaded is 9.
0-75: Bisphenol A-based silver filler epoxy resin with an appropriate amount of reactive diluent added at 10-25, and the weight percentage of the aliphatic polyamine-based curing agent added upon use of the bisphenol A-based silver filler epoxy resin. 2 to 3 parts per 100 parts to lower the viscosity and increase the curing temperature to 50%.
A two-component low-temperature heat-curing conductive epoxy adhesive 2 whose adhesive strength is enhanced by heating the adhesive at a temperature between ℃ and 80℃, and a phenylcidyl ether as a reactive diluent. The two-component low-temperature heat-curable conductive epoxy adhesive 3 according to claim 1, wherein triethylenetetraamine is used as the aliphatic polyamine curing agent. A two-component low-temperature heat-curable conductive epoxy adhesive 4, whose viscosity is reduced to 10,000 to 50,000 CPS, which has high kneading properties and good wettability to increase adhesive strength.Claim 1
Two-component low-temperature heat-curing conductive epoxy adhesive according to item 2, item 2, or item 3.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11346987A JPS63278987A (en) | 1987-05-12 | 1987-05-12 | Two-pack low-temperature curable electroconductive epoxy adhesive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11346987A JPS63278987A (en) | 1987-05-12 | 1987-05-12 | Two-pack low-temperature curable electroconductive epoxy adhesive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63278987A true JPS63278987A (en) | 1988-11-16 |
| JPH0567672B2 JPH0567672B2 (en) | 1993-09-27 |
Family
ID=14613040
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11346987A Granted JPS63278987A (en) | 1987-05-12 | 1987-05-12 | Two-pack low-temperature curable electroconductive epoxy adhesive |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63278987A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041104C (en) * | 1994-04-27 | 1998-12-09 | 丁秀福 | Binder of glass wool and face decoration material |
| JPH1143643A (en) * | 1997-04-11 | 1999-02-16 | Shimizu Corp | Low out-gas paint |
| EP1306148A1 (en) * | 2001-10-29 | 2003-05-02 | CERAMETAL S.a.r.l. | Method for slip casting bodies from ceramic glass or metal powder |
| WO2022188504A1 (en) * | 2021-03-11 | 2022-09-15 | 无锡帝科电子材料股份有限公司 | Heat-cured conductive adhesive and preparation method therefor |
-
1987
- 1987-05-12 JP JP11346987A patent/JPS63278987A/en active Granted
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1041104C (en) * | 1994-04-27 | 1998-12-09 | 丁秀福 | Binder of glass wool and face decoration material |
| JPH1143643A (en) * | 1997-04-11 | 1999-02-16 | Shimizu Corp | Low out-gas paint |
| EP1306148A1 (en) * | 2001-10-29 | 2003-05-02 | CERAMETAL S.a.r.l. | Method for slip casting bodies from ceramic glass or metal powder |
| WO2022188504A1 (en) * | 2021-03-11 | 2022-09-15 | 无锡帝科电子材料股份有限公司 | Heat-cured conductive adhesive and preparation method therefor |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0567672B2 (en) | 1993-09-27 |
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