JP2012172054A - Liquid epoxy resin composition and electronic component using the same - Google Patents
Liquid epoxy resin composition and electronic component using the same Download PDFInfo
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- JP2012172054A JP2012172054A JP2011035209A JP2011035209A JP2012172054A JP 2012172054 A JP2012172054 A JP 2012172054A JP 2011035209 A JP2011035209 A JP 2011035209A JP 2011035209 A JP2011035209 A JP 2011035209A JP 2012172054 A JP2012172054 A JP 2012172054A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L24/00—Arrangements for connecting or disconnecting semiconductor or solid-state bodies; Methods or apparatus related thereto
- H01L24/01—Means 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
- H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
- H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
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Abstract
Description
本発明は、液状エポキシ樹脂組成物とそれを用いた電子部品に関するものである。 The present invention relates to a liquid epoxy resin composition and an electronic component using the same.
従来より、電気・電子分野の接着剤や封止材等においてエポキシ樹脂組成物が広く使用されている。これらエポキシ樹脂組成物においては、その硬化物の低弾性化、高靱性化を図るための工夫が様々に行われている。 Conventionally, epoxy resin compositions have been widely used in adhesives and sealants in the electric / electronic field. In these epoxy resin compositions, various devices for reducing the elasticity and toughness of the cured product have been made.
例えば、高靱性化による耐クラック性や耐衝撃性の向上のために、シリコーンパウダーを添加することや、ポリビニルアセタール樹脂を配合することが知られている。（特許文献１〜６参照） For example, it is known to add silicone powder or blend polyvinyl acetal resin in order to improve crack resistance and impact resistance by increasing toughness. (See Patent Documents 1 to 6)
しかしながら、シリコーンパウダーの添加については、機械的強度の低下やガラス転移温度の低下により信頼性が低下しやすい点が懸念され、また、エポキシ樹脂組成物の流動性が低下しやすい点も問題である。
一方、ポリビニルアセタール樹脂の配合では、硬化物の低弾性、高靱性化とともに組成物の低粘度化、流動性の向上とのバランスが重要な課題である。
それというのも、精密な接着作業や緻密な封止成形を主用途とする常温液状のエポキシ樹脂組成物において、液状組成物の低粘度化、流動性の向上が、主要課題になっているからである。
However, regarding the addition of silicone powder, there is a concern that reliability is likely to decrease due to a decrease in mechanical strength and a decrease in glass transition temperature, and the fluidity of the epoxy resin composition is likely to decrease. .
On the other hand, in the blending of the polyvinyl acetal resin, the balance between the low elasticity and high toughness of the cured product and the low viscosity of the composition and the improvement of fluidity are important issues.
This is because, in a normal temperature liquid epoxy resin composition whose main application is precise bonding work and precise sealing molding, lowering the viscosity of the liquid composition and improving fluidity are the main issues. It is.
そこで、本発明は、液状エポキシ樹脂組成物に関して、低粘度化による所要の流動性と反応性を確保しつつ、硬化物の弾性率を抑え、かつ、硬化物の耐衝撃性、靭性を高めた液状エポキシ樹脂組成物とそれを用いた電子部品を提供することを課題としている。 Therefore, the present invention relates to the liquid epoxy resin composition, while ensuring the required fluidity and reactivity by reducing the viscosity, suppressing the elastic modulus of the cured product, and improving the impact resistance and toughness of the cured product. It is an object to provide a liquid epoxy resin composition and an electronic component using the same.
本発明は、上記の課題を解決するために、以下のことを特徴としている。
すなわち、本発明の液状エポキシ樹脂組成物は、組成成分として、
ａ）常温で液状であるエポキシ樹脂、
ｂ）ポリビニルアセタール系改質材、
ｃ）硬化剤及び硬化促進剤、
ｄ）フィラー
を含有する常温で液状の液状エポキシ樹脂組成物であり、かつ、ポリビニルアセタール系改質材の配合割合は、常温で液状であるエポキシ樹脂１００質量部に対して、０．５〜２０質量部の範囲内であり、かつ、液状エポキシ樹脂組成物の全体量に対して、０．５〜７質量％の範囲内であることを特徴とする。
The present invention is characterized by the following in order to solve the above problems.
That is, the liquid epoxy resin composition of the present invention is a composition component,
a) an epoxy resin that is liquid at room temperature,
b) a polyvinyl acetal modifier,
c) curing agent and curing accelerator,
d) A liquid epoxy resin composition that is liquid at room temperature containing a filler, and the blending ratio of the polyvinyl acetal modifier is 0.5 to 20 with respect to 100 parts by mass of the epoxy resin that is liquid at room temperature. It is in the range of 0.5 parts by mass and within the range of 0.5 to 7% by mass with respect to the total amount of the liquid epoxy resin composition.
この液状エポキシ樹脂組成物では、常温で液状であるエポキシ樹脂は、常温での粘度が０．０１〜２０Ｐａ・ｓであることが好ましい。液状エポキシ樹脂組成物では、硬化剤はアミン系硬化剤を含み、硬化促進剤はイミダゾール系硬化促進剤を含むことが好ましい。
さらに、液状エポキシ樹脂組成物では、ポリビニルアセタール系改質材は、アルキルアセタール化ポリビニルアルコールであって、アセタール化度が６５モル％以上であって、数平均分子量が１〜１８万であることが好ましい。
In this liquid epoxy resin composition, the epoxy resin that is liquid at room temperature preferably has a viscosity at room temperature of 0.01 to 20 Pa · s. In the liquid epoxy resin composition, it is preferable that the curing agent includes an amine curing agent and the curing accelerator includes an imidazole curing accelerator.
Furthermore, in the liquid epoxy resin composition, the polyvinyl acetal-based modifier is an alkyl acetalized polyvinyl alcohol having an acetalization degree of 65 mol% or more and a number average molecular weight of 1 to 180,000. preferable.
また、本発明の電子部品は、以上のとおりの液状エポキシ樹脂組成物の硬化物により接着されていることを特徴とする。 The electronic component of the present invention is characterized in that it is bonded with a cured product of the liquid epoxy resin composition as described above.
本発明の液状エポキシ樹脂組成物によれば、低粘度化による所要の流動性と反応性を確保しつつ、硬化物の弾性率を抑え、かつ、硬化物の耐衝撃性、靭性を高めることが可能となる。 According to the liquid epoxy resin composition of the present invention, it is possible to suppress the elastic modulus of the cured product and to improve the impact resistance and toughness of the cured product while ensuring the required fluidity and reactivity by reducing the viscosity. It becomes possible.
以下、本発明の実施の形態を説明する。 Embodiments of the present invention will be described below.
本発明の液状エポキシ樹脂組成物には、常温で液状であるエポキシ樹脂に対して、前記のとおりポリビニルアセタール系改質材が配合される。ポリビニルアセタール系改質材の配合割合は、常温で液状であるエポキシ樹脂１００質量部に対して、０．５〜２０質量部の範囲内であり、かつ、液状エポキシ樹脂組成物の全体量に対して、０．５〜７質量％の範囲内である。
このようなポリビニルアセタール系改質材の配合割合の範囲内において本発明の所望の効果が得られることになる。より好適には、その配合割合は、常温で液状であるエポキシ樹脂１００質量部に対して、１〜１０質量部の範囲内であり、かつ、液状エポキシ樹脂組成物の全体量に対して、０．８〜５質量％の範囲内である。
In the liquid epoxy resin composition of the present invention, as described above, a polyvinyl acetal-based modifier is blended with an epoxy resin that is liquid at room temperature. The blending ratio of the polyvinyl acetal-based modifier is within a range of 0.5 to 20 parts by mass with respect to 100 parts by mass of the epoxy resin that is liquid at room temperature, and with respect to the total amount of the liquid epoxy resin composition. In the range of 0.5 to 7% by mass.
The desired effect of the present invention can be obtained within the range of the blending ratio of such a polyvinyl acetal-based modifier. More preferably, the blending ratio is within a range of 1 to 10 parts by mass with respect to 100 parts by mass of the epoxy resin that is liquid at normal temperature, and 0 with respect to the total amount of the liquid epoxy resin composition. Within the range of 8 to 5% by mass.
本発明に用いられるポリビニルアセタール系改質材としては、例えば、アルキルアセタール化ポリビニルアルコールであって、アセタール化度が６５モル％以上のものが挙げられる。数平均分子量は１〜１８万のものを用いることができる。このアセタール化度と数平均分子量の範囲内において、液状エポキシ樹脂組成物の低粘度化、流動性の向上が図られ、また、硬化物の低弾性化、高靱性化が可能となる。これらのバランスは実際的に好ましいものとなる。より好適には、アセタール化度が７０〜８０モル％であって、数平均分子量が２〜１５万の範囲内であることが考慮される。
これらのポリビニルアセタール系改質材は、市販品を入手して利用しても良いし、合成したものを用いても良い。合成品については、たとえば、酢酸ビニルなどのビニルエステル系単量体を重合して得たビニルエステル系重合体をケン化してビニルアルコール系重合体とし、次いでアルデヒド類と反応させてアセタール化する方法などにより取得することが可能である。
Examples of the polyvinyl acetal-based modifier used in the present invention include alkyl acetalized polyvinyl alcohol having an acetalization degree of 65 mol% or more. A number average molecular weight of 1 to 180,000 can be used. Within the range of the degree of acetalization and the number average molecular weight, the liquid epoxy resin composition can be reduced in viscosity and fluidity, and the cured product can be reduced in elasticity and increased in toughness. These balances are actually preferable. More preferably, it is considered that the degree of acetalization is 70 to 80 mol% and the number average molecular weight is in the range of 2 to 150,000.
As these polyvinyl acetal-based modifiers, commercially available products may be used and synthesized ones may be used. For synthetic products, for example, a method of saponifying a vinyl ester polymer obtained by polymerizing a vinyl ester monomer such as vinyl acetate to form a vinyl alcohol polymer and then acetalizing it by reacting with an aldehyde It is possible to acquire by such as.
本発明の液状エポキシ樹脂組成物に配合される常温で液状であるエポキシ樹脂としては、例えば、１分子内に２以上のエポキシ基を有するもので、常温での粘度が０．０１〜２０Ｐａ・ｓであることが好ましい。
常温、すなわち、一般的に１５℃〜２５℃の温度下で液状であれば特に限定されないが、例えば、ビスフェノールＡ型エポキシ樹脂、ビスフェノールＦ型エポキシ樹脂等のビスフェノール型エポキシ樹脂、水添ビスフェノールＡ型エポキシ樹脂、水添ビスフェノールＦ型エポキシ樹脂等の水添ビスフェノール型エポキシ樹脂等が挙げられる。これらは１種単独で用いてもよく、２種以上を併用してもよい。
Examples of the epoxy resin that is liquid at room temperature to be blended in the liquid epoxy resin composition of the present invention include those having two or more epoxy groups in one molecule, and a viscosity at room temperature of 0.01 to 20 Pa · s. It is preferable that
Although it will not specifically limit if it is liquid at normal temperature, ie, the temperature of 15 to 25 degreeC generally, For example, bisphenol type epoxy resins, such as bisphenol A type epoxy resin and bisphenol F type epoxy resin, hydrogenated bisphenol A type Examples thereof include hydrogenated bisphenol type epoxy resins such as epoxy resins and hydrogenated bisphenol F type epoxy resins. These may be used alone or in combination of two or more.
本発明の液状エポキシ樹脂組成物には、硬化剤として、好ましくはアミン系硬化剤が配合される。アミン系硬化剤としては、たとえば、三井化学製「エポミックQ-640」を例示することができる。
また、本発明の液状エポキシ樹脂組成物には、硬化促進剤として、好ましくはイミダゾール系硬化促進剤が配合される。イミダゾール系硬化促進剤としては、たとえば、四国化成製「1M2PZ」を例示することができる。
The liquid epoxy resin composition of the present invention preferably contains an amine curing agent as a curing agent. Examples of the amine curing agent include “Epomic Q-640” manufactured by Mitsui Chemicals.
The liquid epoxy resin composition of the present invention preferably contains an imidazole curing accelerator as a curing accelerator. Examples of the imidazole curing accelerator include “1M2PZ” manufactured by Shikoku Kasei.
本発明の液状エポキシ樹脂組成物には、硬化収縮や熱歪みを低減し、機械的強度を高めるためにフィラーが配合される。フィラーとしては、無機質のもの、たとえば、溶融球状シリカ等を好ましく用いることができる。フィラーの平均粒径としては、数μｍ〜十数μｍ程度のものを好ましく用いることができる。 In the liquid epoxy resin composition of the present invention, a filler is blended in order to reduce curing shrinkage and thermal distortion and increase mechanical strength. As the filler, an inorganic material such as fused spherical silica can be preferably used. As the average particle diameter of the filler, those having a particle size of about several μm to several tens of μm can be preferably used.
本発明の液状エポキシ樹脂組成物には、本発明の効果を損なわない範囲内において、さらに他の成分を配合することができる。このような他の成分の具体例としては、難燃剤、密着性付与剤、着色剤、消泡剤、カップリング剤等が挙げられる。 The liquid epoxy resin composition of the present invention can further contain other components within a range not impairing the effects of the present invention. Specific examples of such other components include flame retardants, adhesion promoters, colorants, antifoaming agents, coupling agents, and the like.
本発明の液状エポキシ樹脂組成物の粘度は、塗布時の作業性等を考慮すると、常温で液状であり、好ましくは室温（２５℃）で５０Ｐａ・ｓ以下、さらに好ましくは室温（２５℃）で５Ｐａ・ｓ未満である。粘度を下げるため、反応性希釈剤や有機溶媒を適宜添加することもできる。
本発明の液状エポキシ樹脂組成物は、常温で液状であるエポキシ樹脂を含む主剤と、硬化剤及び硬化促進剤を含む混合剤（副剤）との二液混合型として構成することもできる。両剤を混合して調合した直後のエポキシ樹脂組成物の粘度が５０Ｐａ・ｓ以下であるものとすることもできる。
The viscosity of the liquid epoxy resin composition of the present invention is liquid at room temperature, preferably 50 Pa · s or less at room temperature (25 ° C.), more preferably at room temperature (25 ° C.) in consideration of workability during coating. It is less than 5 Pa · s. In order to lower the viscosity, a reactive diluent or an organic solvent can be appropriately added.
The liquid epoxy resin composition of the present invention can also be configured as a two-component mixed type of a main agent containing an epoxy resin that is liquid at room temperature and a mixture (adjunct) containing a curing agent and a curing accelerator. The viscosity of the epoxy resin composition immediately after mixing and preparing both agents may be 50 Pa · s or less.
また、本発明の液状エポキシ樹脂組成物は、定法により、エポキシ樹脂、硬化剤、および必要に応じて他の成分を配合し、必要に応じて加熱処理や冷却処理を行いながら、撹拌、溶解、混合、粉砕を行い、トランスファー成形に好適な粉体状のエポキシ樹脂組成物に調製することもできる。 In addition, the liquid epoxy resin composition of the present invention is blended with an epoxy resin, a curing agent, and other components as necessary according to a conventional method, stirring and dissolving while performing heat treatment and cooling treatment as necessary. It can also be mixed and pulverized to prepare a powdery epoxy resin composition suitable for transfer molding.
本発明の液状エポキシ樹脂組成物を用いて半導体素子等の部材を封止する際には、例えば、電子部品の種類等に応じて、従来知られている方法や態様により行うことができる。例えば、ディスペンサーからの吐出によるポッティング封止、アンダーフィル封止、加圧と加熱を同時に行う圧接封止、マスクやスクリーンを用いた印刷による封止等が挙げられる。多層回路板や、銅貼り積層回路シート等では、印刷や塗工による接着や封止ができる。 When sealing a member such as a semiconductor element using the liquid epoxy resin composition of the present invention, it can be performed by a conventionally known method or mode depending on the type of electronic component, for example. For example, potting sealing by discharging from a dispenser, underfill sealing, pressure contact sealing in which pressurization and heating are performed simultaneously, sealing by printing using a mask or a screen, and the like can be given. In a multilayer circuit board, a copper-clad laminated circuit sheet, etc., adhesion or sealing by printing or coating can be performed.
本発明の液状エポキシ樹脂組成物の硬化条件は、特に限定されるものではないが、例えば、８０〜１６０℃、０．１〜５時間で行うことができる。 Although the hardening conditions of the liquid epoxy resin composition of this invention are not specifically limited, For example, it can carry out at 80-160 degreeC and 0.1 to 5 hours.
本発明の液状エポキシ樹脂組成物によれば、このようにして封止した硬化物の弾性率を５ＧＰａ以下とすることができる。さらに好ましくは弾性率を１ＧＰａ以下とすることができる。
また、粘度については、１００Ｐａ・ｓ未満、さらには５０Ｐａ・ｓ以下に、耐衝撃試験では、１０ｋＪ／ｍ２以上にすることができる。
According to the liquid epoxy resin composition of the present invention, the cured product thus sealed can have an elastic modulus of 5 GPa or less. More preferably, the elastic modulus can be 1 GPa or less.
The viscosity can be less than 100 Pa · s, further 50 Pa · s or less, and 10 kJ / m 2 or more in the impact resistance test.
以下、実施例により本発明をさらに詳しく説明するが、本発明はこれらの実施例に何ら限定されるものではない。 EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this invention is not limited to these Examples at all.
表１に示す配合量（質量部）で各成分を配合し、液状エポキシ樹脂組成物を調製した。 Each component was mix | blended with the compounding quantity (mass part) shown in Table 1, and the liquid epoxy resin composition was prepared.
表１に示す配合成分として、以下のものを用いた。
〈主剤としての常温で液状であるエポキシ樹脂〉
・ビスフェノールＡ型エポキシ樹脂、ジャパン・エポキシレジン（株）製、エピコー
ト８２８、エポキシ当量 １８９
〈改質材〉
・ポリビニルアセタール系樹脂、積水化学工業（株）製、ＫＳ−１
〈硬化剤〉
・アミン系硬化剤、三井化学（株）製、エポミックＱ−６４０
〈硬化促進剤〉
・イミダゾール系硬化促進剤、四国化成（株）製、１Ｍ２ＰＺ
〈反応性希釈剤〉
・エチルヘキシルグリシジルエーテル系反応性希釈剤、ナガセケムテックス（株） 製、ＥＸ−１２１
〈フィラー〉
・溶融球状シリカ、平均粒径 ７μｍ
実施例および比較例に用いる各液状エポキシ樹脂組成物は、エポキシ樹脂を含む主剤と、硬化剤、硬化促進剤を含む混合剤（副剤）の二液型として調製した。使用直前に、その二液を混合して液状エポキシ樹脂組成物としたものを用いて次の評価を行った。
なお、改質剤、フィラー、反応性希釈剤、その他配合成分は、粘度や反応性に特段の不都合のない限り、主剤に配合しておいても、副剤に配合しておいても、両剤に分けて配合しておいてもよい。
As the blending components shown in Table 1, the following were used.
<Epoxy resin that is liquid at room temperature as the main agent>
-Bisphenol A type epoxy resin, manufactured by Japan Epoxy Resin Co., Ltd., Epicoat 828, Epoxy equivalent 189
<Modifier>
-Polyvinyl acetal resin, manufactured by Sekisui Chemical Co., Ltd., KS-1
<Curing agent>
Amine-based curing agent, manufactured by Mitsui Chemicals, Epomic Q-640
<Curing accelerator>
・ Imidazole-based curing accelerator, manufactured by Shikoku Kasei Co., Ltd., 1M2PZ
<Reactive diluent>
-Ethylhexyl glycidyl ether type reactive diluent, manufactured by Nagase ChemteX Corporation, EX-121
<Filler>
・ Fused spherical silica, average particle size 7μm
Each liquid epoxy resin composition used for an Example and a comparative example was prepared as a two-pack type of the main ingredient containing an epoxy resin, and the mixture (adjunct) containing a hardening agent and a hardening accelerator. Immediately before use, the following evaluation was performed using the liquid epoxy resin composition obtained by mixing the two liquids.
In addition, modifiers, fillers, reactive diluents, and other compounding components may be added to the main agent or the auxiliary agent, as long as there is no particular inconvenience in viscosity and reactivity. You may mix and divide.
[粘度]
液状エポキシ樹脂組成物の粘度を室温（２５℃）にてＢ型粘度計を用いて測定し、次の基準に基づき評価した。
○：粘度５０Ｐａ・ｓ未満
△：粘度５０Ｐａ・ｓ以上１００Ｐａ・ｓ未満
×：粘度１００Ｐａ・ｓ以上
[弾性率]
液状エポキシ樹脂組成物をガラス板で挟みこみ、１５０℃で２時間加熱して硬化させて、長さ５８ｍｍ×幅１４ｍｍ×厚さ７ｍｍの試験片を形成した。この試験片に関して引張圧縮試験機を用い、一般的な３点曲げ試験により室温（２５℃）で曲げ弾性率を測定し、次の基準に基づき評価した。
○：５ＧＰａ未満、
△：５ＧＰａ以上１０ＧＰａ未満、
×：１０ＧＰａ以上
［耐衝撃性］
液状エポキシ樹脂組成物をガラス板で挟みこみ、１５０℃で２時間加熱して硬化させて、長さ５８ｍｍ×幅１４ｍｍ×厚さ７ｍｍの試験片を形成した。この試験片にあらかじめクラックを入れ、シャルピー耐衝撃性試験を行い、耐衝撃性試験とした。判別基準は下記の通りに定めた。
○：１０ｋＪ／ｍ２以上
△：５ｋＪ／ｍ２以上１０ｋＪ／ｍ２未満
×：５ｋＪ／ｍ２未満
これらの評価結果を表１に示す。
[viscosity]
The viscosity of the liquid epoxy resin composition was measured using a B-type viscometer at room temperature (25 ° C.) and evaluated based on the following criteria.
○: Viscosity less than 50 Pa · s Δ: Viscosity of 50 Pa · s to less than 100 Pa · s
[Elastic modulus]
The liquid epoxy resin composition was sandwiched between glass plates and cured by heating at 150 ° C. for 2 hours to form a test piece having a length of 58 mm × width of 14 mm × thickness of 7 mm. With respect to this test piece, a bending elastic modulus was measured at room temperature (25 ° C.) by a general three-point bending test using a tensile and compression tester, and evaluated based on the following criteria.
○: Less than 5 GPa
Δ: 5 GPa or more and less than 10 GPa,
×: 10 GPa or more [impact resistance]
The liquid epoxy resin composition was sandwiched between glass plates and cured by heating at 150 ° C. for 2 hours to form a test piece having a length of 58 mm × width of 14 mm × thickness of 7 mm. This test piece was cracked in advance, and a Charpy impact resistance test was performed to obtain an impact resistance test. Discrimination criteria were determined as follows.
○: 10 kJ / m 2 or more
△: 5kJ / m 2 or more 10 kJ / m 2 less ×: 5kJ / m 2 less than these evaluation results are shown in Table 1.
表１より、ポリビニルアセタール系改質材を、常温で液状であるエポキシ樹脂１００質量部に対して１．７５〜１７．５質量部配合し、かつ、液状エポキシ樹脂組成物全量に対して約１〜５質量％配合した実施例１〜３の液状エポキシ樹脂組成物は、粘度５０Ｐａ・ｓ未満で所要の液状性と反応性を確保しつつ、硬化物の弾性率を５ＧＰａ以下の低いものとし、かつ、耐衝撃性、すなわち靱性を１０ｋＪ／ｍ２以上とすることができた。 From Table 1, 1.75-17.5 mass parts is mix | blended with respect to 100 mass parts of epoxy resins which are liquid at normal temperature from polyvinyl acetal type modifier, and about 1 with respect to the liquid epoxy resin composition whole quantity. The liquid epoxy resin composition of Examples 1 to 3 blended in an amount of ˜5% by mass has a viscosity of less than 50 Pa · s and ensures the required liquidity and reactivity, and the cured product has a low elastic modulus of 5 GPa or less, And impact resistance, ie, toughness, could be 10 kJ / m 2 or more.
一方、表２のシリコーンパウダーを配合した比較例１の液状エポキシ樹脂組成物は、粘度５０Ｐａ・ｓ未満で液状性はあるものの、硬化物の弾性率は１０ＧＰａ以上で可とう性に欠け、耐衝撃性、すなわち靱性は５ｋＪ／ｍ２未満であった。比較例１の液状エポキシ樹脂組成物は、フィラーのシリカを添加していないので、かろうじて粘度５０Ｐａ・ｓ未満の液状性はあったが、硬化収縮は大きいことが目視で確認された。 On the other hand, the liquid epoxy resin composition of Comparative Example 1 in which the silicone powder of Table 2 was blended had a viscosity of less than 50 Pa · s and a liquid property, but the cured product had an elastic modulus of 10 GPa or more and lacked flexibility, impact resistance gender, namely toughness was less than 5 kJ / m 2. Since the liquid epoxy resin composition of Comparative Example 1 did not contain the filler silica, it was barely liquid with a viscosity of less than 50 Pa · s, but it was visually confirmed that the cure shrinkage was large.
主剤のビスフェノールＡ型エポキシ樹脂を全て反応性希釈剤にした比較例２の液状エポキシ樹脂組成物は、シリコーンパウダーを含んでおり、粘度５０Ｐａ・ｓ未満で所要の液状性はあるものの反応性が反応性が低下しており、硬化物の弾性率は１０ＧＰａ以上で低減せず、耐衝撃性、すなわち靱性は１０ｋＪ／ｍ２未満であった。 The liquid epoxy resin composition of Comparative Example 2 in which all of the main agent bisphenol A type epoxy resin is used as a reactive diluent contains silicone powder, has a viscosity of less than 50 Pa · s and has the required liquidity, but reacts. The elastic modulus of the cured product was not reduced at 10 GPa or more, and the impact resistance, that is, the toughness was less than 10 kJ / m 2 .
シリコーンパウダーの含有量が９質量％の比較例３の液状エポキシ樹脂組成物は、粘度１００Ｐａ・ｓ以上で液状性は無く、硬化物の弾性率は１０ＧＰａ以上で可とう性に欠け、耐衝撃性、すなわち靱性は１０ｋＪ／ｍ２未満であった。 The liquid epoxy resin composition of Comparative Example 3 having a silicone powder content of 9% by mass has a viscosity of 100 Pa · s or more and no liquidity, and the cured product has an elastic modulus of 10 GPa or more and lacks flexibility, impact resistance. That is, the toughness was less than 10 kJ / m 2 .
Claims (5)
ａ）常温で液状であるエポキシ樹脂、
ｂ）ポリビニルアセタール系改質材、
ｃ）硬化剤及び硬化促進剤、
ｄ）フィラー
を含有する常温で液状であるエポキシ樹脂組成物であって、
前記したポリビニルアセタール系改質材の配合割合は、常温で液状であるエポキシ樹脂１００質量部に対して、０．５〜２０質量部の範囲内であり、かつ、液状エポキシ樹脂組成物の全体量に対して、０．５〜７質量％の範囲内であることを特徴とする液状エポキシ樹脂組成物。 As a component,
a) an epoxy resin that is liquid at room temperature,
b) a polyvinyl acetal modifier,
c) curing agent and curing accelerator,
d) An epoxy resin composition that is liquid at room temperature and contains a filler,
The blending ratio of the polyvinyl acetal-based modifier described above is in the range of 0.5 to 20 parts by mass with respect to 100 parts by mass of the epoxy resin that is liquid at normal temperature, and the total amount of the liquid epoxy resin composition The liquid epoxy resin composition is characterized by being in the range of 0.5 to 7% by mass.
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| CN103923320A (en) * | 2014-04-02 | 2014-07-16 | 浙江大学 | Branched organosilicon epoxy resin curing agent and epoxy curing system |
| JP2017082022A (en) * | 2015-10-22 | 2017-05-18 | ナガセケムテックス株式会社 | Epoxy resin adhesive |
| JP7395979B2 (en) | 2019-11-15 | 2023-12-12 | 住友ベークライト株式会社 | Conductive paste and semiconductor devices |
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