JP2015091957A - Circuit connection material, connection structure using the same and temporal crimping method - Google Patents

Circuit connection material, connection structure using the same and temporal crimping method Download PDF

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JP2015091957A
JP2015091957A JP2014219103A JP2014219103A JP2015091957A JP 2015091957 A JP2015091957 A JP 2015091957A JP 2014219103 A JP2014219103 A JP 2014219103A JP 2014219103 A JP2014219103 A JP 2014219103A JP 2015091957 A JP2015091957 A JP 2015091957A
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circuit
mass
parts
resin
connection
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孝 中澤
Takashi Nakazawa
孝 中澤
小林　宏治
Koji Kobayashi
宏治 小林
隆伸 小林
Takanobu Kobayashi
隆伸 小林
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Showa Denko Materials Co Ltd
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Hitachi Chemical Co Ltd
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    • C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
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Abstract

PROBLEM TO BE SOLVED: To provide a circuit connection material sufficiently excellent in low temperature and short time temporal crimping properties to a connection member, a connection structure using the same, and a temporal crimping method.SOLUTION: Provided is a circuit connection material electrically connecting confronted circuit electrodes each other, comprising: (a) an epoxy resin; (b) a potential hardener; (c) a film forming material; and (d) a thermoplastic polymer including carboxylic vinyl ester as a monomer unit.

Description

本発明は、回路接続材料、それを用いた接続構造体及び仮圧着方法に関する。   The present invention relates to a circuit connection material, a connection structure using the same, and a temporary crimping method.

半導体素子や液晶表示素子用の接着剤としては、接着性に優れ、かつ高い信頼性を示すエポキシ樹脂等の熱硬化性樹脂が用いられている（例えば、特許文献１参照）。上記接着剤の構成成分としては、エポキシ樹脂、エポキシ樹脂と反応性を有するフェノール樹脂等の硬化剤、エポキシ樹脂と硬化剤との反応を促進する熱潜在性触媒が一般に用いられている。熱潜在性触媒は、接着剤の硬化温度及び硬化速度を決定する重要な因子となっており、室温での貯蔵安定性及び加熱時の硬化速度の観点から種々の化合物が用いられている。   As an adhesive for a semiconductor element or a liquid crystal display element, a thermosetting resin such as an epoxy resin having excellent adhesiveness and high reliability is used (for example, see Patent Document 1). As a constituent component of the adhesive, a curing agent such as an epoxy resin, a phenol resin having reactivity with the epoxy resin, and a thermal latent catalyst for promoting the reaction between the epoxy resin and the curing agent are generally used. The heat latent catalyst is an important factor for determining the curing temperature and curing rate of the adhesive, and various compounds are used from the viewpoint of storage stability at room temperature and curing rate during heating.

また、最近では、アクリレート誘導体やメタクリレート誘導体等のラジカル重合性化合物とラジカル重合開始剤である過酸化物とから構成されるラジカル硬化型接着剤が注目されている（例えば、特許文献２参照）。ラジカル硬化型接着剤は、低温かつ短時間での硬化が可能であるものの、接着性が接続部材の表面状態に左右される傾向がある。一方、比較的低温かつ短時間で接着可能な回路接続材料として、エポキシ樹脂を用いたカチオン重合系の接着剤が開発され実用化されている（例えば、特許文献３参照）。   Recently, attention has been focused on radical curable adhesives composed of radical polymerizable compounds such as acrylate derivatives and methacrylate derivatives and peroxides as radical polymerization initiators (see, for example, Patent Document 2). Although the radical curable adhesive can be cured at a low temperature in a short time, the adhesiveness tends to depend on the surface state of the connecting member. On the other hand, as a circuit connection material that can be bonded at a relatively low temperature in a short time, a cationic polymerization type adhesive using an epoxy resin has been developed and put into practical use (for example, see Patent Document 3).

特開平１−１１３４８０号公報Japanese Patent Laid-Open No. 1-113480 国際公開第９８／０４４０６７号パンフレットInternational Publication No. 98/044067 Pamphlet 特開平７−９０２３７号公報JP-A-7-90237

しかしながら、従来のエポキシ樹脂を用いた接着剤は、ラジカル硬化型接着剤に比べ、接続部材に仮接着する際の仮圧着性が劣る傾向があり、特に、低温かつ短時間における仮圧着性の向上が望まれている。   However, adhesives using conventional epoxy resins tend to be inferior in temporary crimping properties when temporarily bonded to connecting members as compared to radical curing adhesives, and in particular, improve temporary crimping properties at low temperatures and in a short time. Is desired.

そこで、本発明は、接続部材への低温かつ短時間での仮圧着性に十分に優れる回路接続材料、それを用いた接続構造体及び仮圧着方法を提供することを目的とする。   Then, an object of this invention is to provide the circuit connection material which is sufficiently excellent in the temporary crimping property to a connection member at low temperature for a short time, a connection structure using the same, and a temporary crimping method.

本発明は、対向する回路電極同士を電気的に接続する回路接続材料であって、（ａ）エポキシ樹脂と、（ｂ）潜在性硬化剤と、（ｃ）フィルム形成材と、（ｄ）カルボン酸ビニルエステルをモノマー単位として含む熱可塑性ポリマーとを含有する回路接続材料を提供する。   The present invention is a circuit connection material for electrically connecting opposing circuit electrodes, and includes (a) an epoxy resin, (b) a latent curing agent, (c) a film forming material, and (d) a carvone. There is provided a circuit connecting material containing a thermoplastic polymer containing an acid vinyl ester as a monomer unit.

本発明の回路接続材料は、上記構成を備えることにより、接続部材への低温かつ短時間での仮圧着性に十分に優れるものとなる。ここで、仮圧着とは、支持フィルム上に形成された回路接続材料からなる接着剤層を、被着体である回路部材に転写する工程をいう。上記工程では、通常、加熱及び加圧により接着剤層を構成する樹脂成分が溶融して回路部材に接着した後、支持フィルムを剥離して接着剤層を回路部材上に転写する。しかしながら、エポキシ樹脂系の回路接続材料の場合、仮圧着時の熱により硬化が進行してしまうことがあるため、加熱温度が制限される。したがって、回路接続材料には、被着体に対する接着性と支持フィルムからの剥離性との両立が求められる。そこで、本発明の回路接続材料は、（ａ）成分であるエポキシ樹脂と共に、（ｂ）成分として潜在性硬化剤を含有することで仮圧着時にはエポキシ樹脂の硬化が進行せず、後の本接続において良好な接続性を示すことができる。その一方で、加熱することである程度樹脂成分を溶融させて回路部材に仮接着する必要があるため、（ｄ）成分としてカルボン酸ビニルエステルをモノマー単位として含む熱可塑性ポリマーを含有することで仮圧着時の加熱温度で（ｄ）成分が溶融して回路部材に仮接着することができる。   The circuit connection material of the present invention is sufficiently excellent in the provisional press-bonding property to the connection member at a low temperature and in a short time by having the above configuration. Here, temporary press bonding refers to a step of transferring an adhesive layer made of a circuit connecting material formed on a support film to a circuit member that is an adherend. In the above step, usually, after the resin component constituting the adhesive layer is melted and adhered to the circuit member by heating and pressurization, the support film is peeled off and the adhesive layer is transferred onto the circuit member. However, in the case of an epoxy resin-based circuit connection material, curing may proceed due to heat at the time of temporary pressure bonding, and thus the heating temperature is limited. Therefore, the circuit connection material is required to have both adhesion to the adherend and releasability from the support film. Therefore, the circuit connection material of the present invention contains the latent curing agent as the component (b) together with the epoxy resin as the component (a), so that the curing of the epoxy resin does not proceed at the time of temporary pressing, and the subsequent main connection Good connectivity can be exhibited. On the other hand, since it is necessary to melt the resin component to some extent by heating and temporarily bond it to the circuit member, it is temporarily crimped by containing a thermoplastic polymer containing a carboxylic acid vinyl ester as a monomer unit as the component (d). The component (d) can be melted and temporarily bonded to the circuit member at the heating temperature.

上記カルボン酸ビニルエステルは、酢酸ビニルであることが好ましい。これにより、回路接続材料は、接続部材への低温かつ短時間での仮圧着性をより一層向上することができる。   The carboxylic acid vinyl ester is preferably vinyl acetate. Thereby, the circuit connection material can further improve the temporary press-bonding property to the connection member at a low temperature in a short time.

また、本発明の回路接続材料において、本接続時の工程を低温化・短時間化できることから、潜在性硬化剤がカチオン重合型潜在性硬化剤であることが好ましく、カチオン重合型潜在性硬化剤が芳香族スルホニウム塩であることがより好ましい。   Further, in the circuit connection material of the present invention, the latent curing agent is preferably a cationic polymerization type latent curing agent because the process at the time of this connection can be reduced in temperature and time, and the cationic polymerization type latent curing agent is preferable. Is more preferably an aromatic sulfonium salt.

さらに、各種接続部材への接着性を向上する観点から、本発明の回路接続材料は、有機微粒子を更に含有することが好ましい。   Furthermore, from the viewpoint of improving adhesion to various connection members, the circuit connection material of the present invention preferably further contains organic fine particles.

本発明はまた、第一の基板及び該基板の主面上に形成された第一の回路電極を有する第一の回路部材と、第二の基板及び該基板の主面上に形成された第二の回路電極を有し、該第二の回路電極と第一の回路電極とが対向するように配置され、該第二の回路電極が上記第一の回路電極と電気的に接続されている第二の回路部材と、第一の回路部材及び第二の回路部材の間に介在する接続部とを備え、接続部が、上記本発明の回路接続材料の硬化物である接続構造体を提供する。   The present invention also provides a first circuit member having a first substrate and a first circuit electrode formed on the main surface of the substrate, a second substrate and a first circuit member formed on the main surface of the substrate. Two circuit electrodes, the second circuit electrode and the first circuit electrode are arranged to face each other, and the second circuit electrode is electrically connected to the first circuit electrode. Provided is a connection structure including a second circuit member and a connection portion interposed between the first circuit member and the second circuit member, wherein the connection portion is a cured product of the circuit connection material of the present invention. To do.

上記接続構造体は、低温かつ短時間での仮圧着性に優れる回路接続材料を用いて接続部が形成されていることにより、安定した品質を有する接続構造体となる。   The connection structure is a connection structure having stable quality because the connection portion is formed using a circuit connection material that is excellent in temporary press bonding properties at a low temperature for a short time.

本発明はさらに、支持フィルムと、該支持フィルムの一方面上に設けられ、本発明の回路接続材料からなる接着剤層とを備えるフィルム状接着剤を、基板及び該基板の主面上に形成された回路電極を有する回路部材に、８０℃以下で仮接着する工程と、仮接着後、支持フィルムを剥離して接着剤層を基板の主面に転写する工程とを備える仮圧着方法を提供する。   The present invention further forms a film adhesive on a substrate and the main surface of the substrate, comprising a support film and an adhesive layer provided on one surface of the support film and made of the circuit connection material of the present invention. Provisional crimping method comprising a step of temporarily adhering to a circuit member having a circuit electrode formed at 80 ° C. or less, and a step of peeling a support film and transferring an adhesive layer to a main surface of a substrate after temporary adhesion To do.

上記仮圧着方法によれば、低温かつ短時間で接着剤層を回路部材へ転写することができるために、安定した接着力を有する接続構造体を作業効率よく作製することができる。   According to the temporary pressure bonding method, the adhesive layer can be transferred to the circuit member at a low temperature and in a short time, so that a connection structure having a stable adhesive force can be produced with high work efficiency.

本発明によれば、接続部材への低温かつ短時間での仮圧着性に十分に優れる回路接続材料、それを用いた接続構造体及び仮圧着方法を提供することができる。   ADVANTAGE OF THE INVENTION According to this invention, the circuit connection material which is fully excellent in the temporary crimping property to a connection member in low temperature for a short time, a connection structure using the same, and a temporary crimping method can be provided.

回路接続材料の一実施形態を示す断面図である。It is sectional drawing which shows one Embodiment of a circuit connection material. 接続構造体の一実施形態を示す断面図である。It is sectional drawing which shows one Embodiment of a connection structure. 回路接続材料を用いた仮圧着方法の一実施形態を概略断面図により示す工程図である。It is process drawing which shows one Embodiment of the temporary crimping | compression-bonding method using a circuit connection material with a schematic sectional drawing.

以下、必要に応じて図面を参照しつつ、本発明の好適な実施形態について詳細に説明する。ただし、本発明は以下の実施形態に限定されるものではない。なお、図面中、同一要素には同一符号を付すこととし、重複する説明は省略する。また、上下左右等の位置関係は、特に断らない限り、図面に示す位置関係に基づくものとする。更に、図面の寸法比率は図示の比率に限られるものではない。また、本明細書における「（メタ）アクリル」とは、「アクリル」及びそれに対応する「メタクリル」を意味する。   Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the drawings as necessary. However, the present invention is not limited to the following embodiments. In the drawings, the same elements are denoted by the same reference numerals, and redundant description is omitted. Further, the positional relationship such as up, down, left and right is based on the positional relationship shown in the drawings unless otherwise specified. Further, the dimensional ratios in the drawings are not limited to the illustrated ratios. In addition, “(meth) acryl” in the present specification means “acryl” and “methacryl” corresponding thereto.

本実施形態に係る回路接続材料は、回路電極同士を電気的に接続するために用いられる接着剤である。図１は、回路接続材料の一実施形態を示す断面図である。図１に示す回路接続材料１は、樹脂層３と、樹脂層３内に分散している複数の導電性粒子５とから構成され、フィルム状の形状を有する。樹脂層３は、（ａ）エポキシ樹脂と、（ｂ）潜在性硬化剤と、（ｃ）フィルム形成材と、（ｄ）カルボン酸ビニルエステルをモノマー単位として含む熱可塑性ポリマーとを含有する。言い換えると、回路接続材料１は、（ａ）エポキシ樹脂と、（ｂ）潜在性硬化剤と、（ｃ）フィルム形成材と、（ｄ）カルボン酸ビニルエステルをモノマー単位として含む熱可塑性ポリマーと、導電性粒子５とを含有する。回路接続材料１が加熱されたときにエポキシ樹脂の架橋により樹脂層３において架橋構造が形成され、回路接続材料１の硬化物が形成される。   The circuit connection material according to the present embodiment is an adhesive used to electrically connect circuit electrodes. FIG. 1 is a cross-sectional view showing an embodiment of a circuit connecting material. A circuit connecting material 1 shown in FIG. 1 is composed of a resin layer 3 and a plurality of conductive particles 5 dispersed in the resin layer 3 and has a film shape. The resin layer 3 contains (a) an epoxy resin, (b) a latent curing agent, (c) a film forming material, and (d) a thermoplastic polymer containing a carboxylic acid vinyl ester as a monomer unit. In other words, the circuit connecting material 1 includes (a) an epoxy resin, (b) a latent curing agent, (c) a film-forming material, and (d) a thermoplastic polymer containing a carboxylic acid vinyl ester as a monomer unit, And conductive particles 5. When the circuit connection material 1 is heated, a crosslinked structure is formed in the resin layer 3 by crosslinking of the epoxy resin, and a cured product of the circuit connection material 1 is formed.

以下、回路接続材料１の各構成材料について説明する。   Hereinafter, each constituent material of the circuit connection material 1 will be described.

（ａ）エポキシ樹脂
（ａ）エポキシ樹脂としては、ビスフェノールＡ、Ｆ、ＡＤ等のビスフェノールのグリシジルエーテルであるビスフェノール型エポキシ樹脂及びフェノールノボラック又はクレゾールノボラックから誘導されるエポキシノボラック樹脂が代表的なエポキシ樹脂である。その他の例として、ナフタレン骨格を有するナフタレン型エポキシ樹脂、グリシジルアミン型エポキシ樹脂、グリシジルエステル型エポキシ樹脂、脂環式エポキシ樹脂及び複素環式エポキシ樹脂が挙げられる。これらは単独又は２種以上混合して用いられる。 (A) Epoxy resin (a) Epoxy resin is typically a bisphenol type epoxy resin that is a glycidyl ether of bisphenol such as bisphenol A, F, or AD, and an epoxy novolac resin derived from phenol novolac or cresol novolac. It is. Other examples include naphthalene type epoxy resins having a naphthalene skeleton, glycidylamine type epoxy resins, glycidyl ester type epoxy resins, alicyclic epoxy resins and heterocyclic epoxy resins. These are used individually or in mixture of 2 or more types.

上記エポキシ樹脂の中でも、ビスフェノール型エポキシ樹脂が分子量の異なるグレードが広く入手可能で、接着性や反応性等を任意に設定できることから好ましい。ビスフェノール型エポキシ樹脂の中でも、ビスフェノールＦ型エポキシ樹脂が特に好ましい。ビスフェノールＦ型エポキシ樹脂の粘度は低く、フェノキシ樹脂との組み合わせて用いることにより、回路接続材料の流動性を容易に広範囲に設定できる。また、ビスフェノールＦ型エポキシ樹脂は、回路接続材料に良好な粘着性を付与し易いという利点も有する。   Among the above epoxy resins, bisphenol type epoxy resins are preferable because grades with different molecular weights are widely available, and adhesiveness, reactivity, and the like can be arbitrarily set. Among bisphenol type epoxy resins, bisphenol F type epoxy resins are particularly preferable. The viscosity of the bisphenol F type epoxy resin is low, and the fluidity of the circuit connecting material can be easily set in a wide range by using it in combination with the phenoxy resin. Further, the bisphenol F type epoxy resin has an advantage that it is easy to impart good adhesiveness to the circuit connecting material.

不純物イオン（Ｎａ＋、Ｃｌ−等）濃度又は加水分解性塩素が３００ｐｐｍ以下であるエポキシ樹脂を用いることが、エレクトロンマイグレーション防止のために好ましい。 It is preferable to use an epoxy resin having an impurity ion (Na + , Cl − etc.) concentration or hydrolyzable chlorine of 300 ppm or less to prevent electron migration.

（ｂ）潜在性硬化剤
（ｂ）潜在性硬化剤としては、エポキシ樹脂を硬化させることができるものであればよい。また、潜在性硬化剤は、エポキシ樹脂と反応して架橋構造中に取り込まれる化合物であってもよいし、エポキシ樹脂の硬化反応を促進する触媒型硬化剤であってもよい。両者を併用することも可能である。 (B) Latent curing agent (b) Any latent curing agent may be used as long as it can cure the epoxy resin. The latent curing agent may be a compound that reacts with the epoxy resin and is incorporated into the crosslinked structure, or may be a catalytic curing agent that accelerates the curing reaction of the epoxy resin. Both can be used in combination.

触媒型硬化剤としては、例えば、エポキシ樹脂のアニオン重合を促進するアニオン重合型潜在性硬化剤、及びエポキシ樹脂のカチオン重合を促進するカチオン重合型潜在性硬化剤が挙げられる。   Examples of the catalytic curing agent include an anionic polymerization latent curing agent that promotes anionic polymerization of an epoxy resin and a cationic polymerization latent curing agent that promotes cationic polymerization of an epoxy resin.

アニオン重合型潜在性硬化剤としては、例えば、イミダゾール系、ヒドラジド系、三フッ素ホウ素−アミン錯体、アミンイミド、ポリアミンの塩、ジシアンジアミド及びこれらの変性物が挙げられる。イミダゾール系のアニオン重合型潜在性硬化剤は、例えば、イミダゾール又はその誘導体をエポキシ樹脂に付加して形成される。   Examples of the anionic polymerization type latent curing agent include imidazole series, hydrazide series, trifluoroboron-amine complex, amine imide, polyamine salt, dicyandiamide, and modified products thereof. The imidazole-based anionic polymerization latent curing agent is formed, for example, by adding imidazole or a derivative thereof to an epoxy resin.

カチオン重合型潜在性硬化剤としては、例えば、エネルギー線照射によりエポキシ樹脂を硬化させる感光性オニウム塩（芳香族ジアゾニウム塩、芳香族スルホニウム塩等が主として用いられる）が好ましい。また、エネルギー線照射以外に加熱によって活性化しエポキシ樹脂を硬化させるものとして、脂肪族スルホニウム塩がある。この種の硬化剤は、速硬化性という特徴を有することから好ましい。   As the cationic polymerization type latent curing agent, for example, a photosensitive onium salt (mainly used is an aromatic diazonium salt, an aromatic sulfonium salt, or the like) that cures an epoxy resin by irradiation with energy rays. In addition to irradiation with energy rays, there is an aliphatic sulfonium salt that is activated by heating to cure the epoxy resin. This type of curing agent is preferable because it has a feature of fast curing.

これらの潜在性硬化剤を、ポリウレタン系、ポリエステル系等の高分子物質、ニッケル、銅等の金属薄膜及びケイ酸カルシウム等の無機物で被覆してマイクロカプセル化したものは、可使時間が延長できるため好ましい。   When these latent curing agents are coated with a polymer material such as polyurethane or polyester, a metal thin film such as nickel or copper, and an inorganic material such as calcium silicate, the pot life can be extended. Therefore, it is preferable.

アニオン重合型潜在性硬化剤の配合量は、（ａ）エポキシ樹脂１００質量部に対して３０〜６０質量部であることが好ましく、４０〜５５質量部であることがより好ましい。３０質量部未満であると回路接続材料の硬化収縮による被着体に対する締め付け力が低下する。その結果、導電性粒子５と回路電極との接触が保持されず、信頼性試験後の接続抵抗が上昇しやすくなる傾向がある。６０質量部を超えると締め付け力が強くなりすぎるため、回路接続材料の硬化物における内部応力が大きくなり、接着強度の低下を招き易くなる傾向がある。   It is preferable that the compounding quantity of an anionic polymerization type | mold latent hardening | curing agent is 30-60 mass parts with respect to 100 mass parts of (a) epoxy resins, and it is more preferable that it is 40-55 mass parts. If it is less than 30 parts by mass, the clamping force on the adherend due to the curing shrinkage of the circuit connecting material is reduced. As a result, the contact between the conductive particles 5 and the circuit electrode is not maintained, and the connection resistance after the reliability test tends to increase. If it exceeds 60 parts by mass, the tightening force becomes too strong, so that the internal stress in the cured product of the circuit connecting material tends to increase, and the adhesive strength tends to decrease.

カチオン重合型潜在性硬化剤の配合量は、（ａ）エポキシ樹脂１００質量部に対して３〜１５質量部であることが好ましく、５〜１０質量部であることがより好ましい。３質量部未満であると回路接続材料の硬化収縮による被着体に対する締め付け力が低下する。その結果、導電性粒子５と回路電極との接触が保持されず、信頼性試験後の接続抵抗が上昇しやすくなる傾向がある。１５質量部を超えると締め付け力が強くなりすぎるため、回路接続材料の硬化物における内部応力が大きくなり、接着強度の低下を招き易くなる傾向がある。   The blending amount of the cationic polymerization type latent curing agent is preferably 3 to 15 parts by mass and more preferably 5 to 10 parts by mass with respect to 100 parts by mass of the (a) epoxy resin. If it is less than 3 parts by mass, the clamping force on the adherend due to the curing shrinkage of the circuit connecting material is reduced. As a result, the contact between the conductive particles 5 and the circuit electrode is not maintained, and the connection resistance after the reliability test tends to increase. If it exceeds 15 parts by mass, the tightening force becomes too strong, so that the internal stress in the cured product of the circuit connecting material tends to increase, and the adhesive strength tends to decrease.

（ｃ）フィルム形成材
フィルム形成材とは、液状物を固形化し構成組成物をフィルム形状とした場合に、そのフィルムの取扱いを容易とし、容易に裂けたり、割れたり、べたついたりしない機械的特性等を付与するものであり、通常の状態（常温常圧）でフィルムとしての取扱いができるものである。 (C) Film-forming material Film-forming material means that when a liquid is solidified and the constituent composition is made into a film shape, the film is easy to handle and mechanical properties that do not easily tear, break, or stick. Etc., and can be handled as a film in a normal state (normal temperature and normal pressure).

（ｃ）フィルム形成材としては、例えば、フェノキシ樹脂、ポリビニルホルマール樹脂、ポリスチレン樹脂、ポリビニルブチラール樹脂、ポリエステル樹脂、ポリアミド樹脂、キシレン樹脂及びポリウレタン樹脂が挙げられる。これらの中でも、接着性、相溶性、耐熱性及び機械的強度に優れることからフェノキシ樹脂が好ましい。   (C) Examples of the film forming material include phenoxy resin, polyvinyl formal resin, polystyrene resin, polyvinyl butyral resin, polyester resin, polyamide resin, xylene resin, and polyurethane resin. Among these, a phenoxy resin is preferable because of excellent adhesiveness, compatibility, heat resistance, and mechanical strength.

フェノキシ樹脂は、２官能性フェノール類とエピハロヒドリンとを高分子化するまで反応させるか、又は２官能性エポキシ樹脂と２官能性フェノール類とを重付加させることにより得られる樹脂である。フェノキシ樹脂は、例えば、２官能性フェノール類１モルとエピハロヒドリン０．９８５〜１．０１５モルとをアルカリ金属水酸化物等の触媒の存在下、非反応性溶媒中で４０〜１２０℃の温度で反応させることにより得ることができる。   The phenoxy resin is a resin obtained by reacting a bifunctional phenol and epihalohydrin until they are polymerized or by polyaddition of a bifunctional epoxy resin and a bifunctional phenol. For example, the phenoxy resin contains 1 mol of a bifunctional phenol and 0.985 to 1.015 mol of epihalohydrin in the presence of a catalyst such as an alkali metal hydroxide at a temperature of 40 to 120 ° C. in a non-reactive solvent. It can be obtained by reacting.

また、フェノキシ樹脂としては、樹脂の機械的特性や熱的特性の観点からは、特に２官能性エポキシ樹脂と２官能性フェノール類との配合当量比をエポキシ基／フェノール水酸基＝１／０．９〜１／１．１とし、アルカリ金属化合物、有機リン系化合物、環状アミン系化合物等の触媒の存在下、沸点が１２０℃以上のアミド系、エーテル系、ケトン系、ラクトン系、アルコール系等の有機溶剤中で、反応固形分が５０質量％以下の条件で５０〜２００℃に加熱して重付加反応させて得たものが好ましい。   Further, as the phenoxy resin, from the viewpoint of the mechanical properties and thermal properties of the resin, the blending equivalent ratio of the bifunctional epoxy resin and the bifunctional phenols is particularly preferably epoxy group / phenol hydroxyl group = 1 / 0.9. To 1 / 1.1, in the presence of a catalyst such as an alkali metal compound, an organophosphorus compound, or a cyclic amine compound, such as an amide, ether, ketone, lactone, alcohol or the like having a boiling point of 120 ° C. or higher. What was obtained by heating to 50-200 degreeC on the conditions whose reaction solid content is 50 mass% or less in the organic solvent was obtained.

２官能性エポキシ樹脂としては、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、ビスフェノールＡＤ型エポキシ樹脂、ビスフェノールＳ型エポキシ樹脂を用いることができる。２官能性フェノール類は２個のフェノール性水酸基を有するものであり、例えば、ハイドロキノン類、ビスフェノールＡ、ビスフェノールＦ、ビスフェノールＡＤ、ビスフェノールＳ等のビスフェノール化合物が挙げられる。   As the bifunctional epoxy resin, bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol AD type epoxy resin, or bisphenol S type epoxy resin can be used. Bifunctional phenols have two phenolic hydroxyl groups, and examples thereof include bisphenol compounds such as hydroquinones, bisphenol A, bisphenol F, bisphenol AD, and bisphenol S.

フェノキシ樹脂は、ラジカル重合性の官能基により変性されていてもよい。フェノキシ樹脂は、１種を単独で又は２種以上を混合して用いることができる。   The phenoxy resin may be modified with a radical polymerizable functional group. A phenoxy resin can be used individually by 1 type or in mixture of 2 or more types.

上記（ｃ）成分の重量平均分子量は１００００以上であることが、製膜性などの観点から好ましい。ただし、熱可塑性樹脂の重量平均分子量が１００００００以上になると他の成分との混合が困難になる傾向がある。なお、本願で規定する重量平均分子量とは、以下の条件のゲルパーミエイションクロマトグラフィー法（ＧＰＣ）により、標準ポリスチレンによる検量線に基づいて決定される値をいう。
ＧＰＣ条件
使用機器：日立Ｌ−６０００ 型（（株）日立製作所）
カラム：ゲルパックＧＬ−Ｒ４２０＋ゲルパックＧＬ−Ｒ４３０＋ゲルパックＧＬ−Ｒ４４０（計３本）（日立化成工業（株）製商品名）
溶離液：テトラヒドロフラン
測定温度：４０℃
流量：１．７５ｍＬ／分
検出器：Ｌ−３３００ＲＩ（（株）日立製作所） The weight average molecular weight of the component (c) is preferably 10,000 or more from the viewpoint of film forming properties. However, when the weight average molecular weight of the thermoplastic resin is 1000000 or more, mixing with other components tends to be difficult. In addition, the weight average molecular weight prescribed | regulated by this application means the value determined based on the calibration curve by a standard polystyrene by the gel permeation chromatography method (GPC) of the following conditions.
Equipment using GPC conditions: Hitachi L-6000 type (Hitachi, Ltd.)
Column: Gel pack GL-R420 + Gel pack GL-R430 + Gel pack GL-R440 (3 in total) (trade name, manufactured by Hitachi Chemical Co., Ltd.)
Eluent: Tetrahydrofuran Measurement temperature: 40 ° C
Flow rate: 1.75 mL / min Detector: L-3300RI (Hitachi, Ltd.)

（ｃ）成分の配合量は、（ａ）及び（ｂ）成分の合計１００質量部に対して５０〜１４０質量部であることが好ましく、７０〜１２０質量部であることがより好ましい。   Component (c) is preferably blended in an amount of 50 to 140 parts by weight, more preferably 70 to 120 parts by weight, based on a total of 100 parts by weight of components (a) and (b).

（ｄ）カルボン酸ビニルエステルをモノマー単位として含む熱可塑性ポリマー
（ｄ）成分である熱可塑性ポリマーとしては、カルボン酸ビニルエステルをモノマー単位として含むものであれば特に限定されない。本発明の回路接続材料は、仮圧着工程における所定の加熱温度において（ｄ）成分が溶融（又は軟化）することで粘着性を示し、被着体へ容易に仮接着することができる。また、後述する（ｅ）有機微粒子を接着性向上の目的で回路接続材料に添加する場合、粘着性がやや低下して仮圧着性が低下することがある。特にこの場合、（ｄ）成分は、回路接続材料の粘着性と接着性とを両立するために有効に機能することができる。 (D) Thermoplastic polymer containing carboxylic acid vinyl ester as monomer unit The thermoplastic polymer as the component (d) is not particularly limited as long as it contains carboxylic acid vinyl ester as a monomer unit. The circuit connecting material of the present invention exhibits tackiness by melting (or softening) the component (d) at a predetermined heating temperature in the temporary press-bonding step, and can be easily temporarily bonded to the adherend. In addition, when (e) organic fine particles to be described later are added to the circuit connecting material for the purpose of improving adhesion, the tackiness may be slightly lowered and the temporary press bonding property may be lowered. Particularly in this case, the component (d) can function effectively in order to achieve both the tackiness and adhesiveness of the circuit connecting material.

カルボン酸ビニルエステルとしては、例えば、酢酸ビニル、プロピオン酸ビニル、酪酸ビニル、カプロン酸ビニル、カプリル酸ビニル、ラウリン酸ビニル、ミリスチン酸ビニル、バルミチン酸ビニル、ステアリン酸ビニル、シクロヘキシルカルボン酸ビニル、ピバリン酸ビニル、オクチル酸ビニル及び安息香酸ビニルが挙げられる。中でも、他のモノマーとの共重合性の観点から、酢酸ビニル、プロピオン酸ビニル、酪酸ビニル、カプロン酸ビニル、カプリル酸ビニル及びラウリン酸ビニルが好ましく、酢酸ビニルがより好ましい。   Examples of the vinyl carboxylate include vinyl acetate, vinyl propionate, vinyl butyrate, vinyl caproate, vinyl caprylate, vinyl laurate, vinyl myristate, vinyl valmitate, vinyl stearate, vinyl cyclohexylcarboxylate, and pivalic acid. Examples include vinyl, vinyl octylate and vinyl benzoate. Among these, from the viewpoint of copolymerizability with other monomers, vinyl acetate, vinyl propionate, vinyl butyrate, vinyl caproate, vinyl caprylate and vinyl laurate are preferable, and vinyl acetate is more preferable.

（ｄ）熱可塑性ポリマーは、極性モノマー単位であるカルボン酸ビニルエステルと共に、非極性モノマー単位であるオレフィンをモノマー単位として含むことで仮圧着性に優れるという本発明の効果をより一層有効かつ確実に発現することができる。オレフィンとしては、エチレン及びプロピレンが例示される。   (D) The thermoplastic polymer further effectively and reliably provides the effect of the present invention in that it has excellent temporary press-bonding properties by including, as a monomer unit, an olefin that is a nonpolar monomer unit together with a carboxylic acid vinyl ester that is a polar monomer unit. Can be expressed. Examples of olefins include ethylene and propylene.

また、上記熱可塑性ポリマーは、本発明の低温での仮圧着性に優れるという効果を逸脱しない範囲で、カルボン酸ビニルエステルと共重合可能なモノマーをモノマー単位として含んでいてもよい。このようなモノマーとしては、例えば、カルボン酸アリルエステル、（メタ）アクリル酸アルキルエステルが挙げられ、具体的には、酢酸アリル、（メタ）アクリル酸メチル及び（メタ）アクリル酸エチルが例示される。   The thermoplastic polymer may contain a monomer copolymerizable with a carboxylic acid vinyl ester as long as it does not deviate from the effect of excellent temporary press bonding at low temperatures of the present invention. Examples of such monomers include carboxylic acid allyl esters and (meth) acrylic acid alkyl esters, and specific examples include allyl acetate, methyl (meth) acrylate, and ethyl (meth) acrylate. .

カルボン酸ビニルエステルの割合は、（ｄ）成分を構成する全モノマー１００質量％を基準として、２０質量％以上６０質量％未満であることが好ましく、２５質量％以上５５質量％未満であることがより好ましく、３０質量％以上５０質量％未満であることがさらに好ましい。６０質量％以上では、室温において樹脂が粘着性を発現し、回路接続材料の巻重体を形成する際に、支持フィルムの背面へ転写してしまい、作業性が劣る傾向がある。２０質量％未満では、樹脂自体の融点が上昇し、仮圧着工程において十分に溶融せず、粘着力向上の効果が得られ難い傾向がある。   The proportion of the carboxylic acid vinyl ester is preferably 20% by mass or more and less than 60% by mass, and preferably 25% by mass or more and less than 55% by mass, based on 100% by mass of all monomers constituting the component (d). More preferably, it is more preferably 30% by mass or more and less than 50% by mass. When the amount is 60% by mass or more, the resin exhibits adhesiveness at room temperature, and when forming a wound body of the circuit connection material, the resin is transferred to the back surface of the support film, and the workability tends to be inferior. If it is less than 20% by mass, the melting point of the resin itself increases, and the resin does not melt sufficiently in the temporary press-bonding step, and the effect of improving the adhesive strength tends to be difficult to obtain.

仮圧着時の被着体への接着性に優れると共に、支持フィルムの剥離性に優れることから、（ｄ）熱可塑性ポリマーとして、オレフィン−カルボン酸ビニルエステル共重合体を含むことが好ましく、回路接続材料を構成する他の樹脂成分との相溶性の観点から、エチレン−酢酸ビニルエステル共重合体を含むことがより好ましい。   Since it is excellent in adhesion to the adherend during temporary pressure bonding and excellent in releasability of the support film, it is preferable that (d) a thermoplastic polymer contains an olefin-carboxylic acid vinyl ester copolymer, and circuit connection From the viewpoint of compatibility with other resin components constituting the material, it is more preferable to include an ethylene-vinyl acetate ester copolymer.

（ｄ）成分は、重量平均分子量（以下、「Ｍｗ」という）が４００００〜１５００００であることが好ましく、６００００〜１３００００であることがより好ましく、７００００〜１２００００であることがさらに好ましい。１５００００を超えると、汎用溶剤であるトルエン、酢酸エチル又はメチルエチルケトン等への溶解性が低下する傾向があり、４００００未満では、樹脂層３の凝集力が低下して接着力が低下する傾向にある。   The component (d) preferably has a weight average molecular weight (hereinafter referred to as “Mw”) of 40000 to 150,000, more preferably 60000 to 130,000, and still more preferably 70000 to 120,000. If it exceeds 150,000, the solubility in general-purpose solvents such as toluene, ethyl acetate, or methyl ethyl ketone tends to decrease, and if it is less than 40000, the cohesive force of the resin layer 3 tends to decrease and the adhesive strength tends to decrease.

（ｄ）成分は、融点が３０℃以上８０℃未満であることが好ましく、３０〜７０℃であることがより好ましい。融点が３０℃未満では、仮圧着時に樹脂染み出しを誘発しやすくなるため、作業性が低下する傾向がある。一方、融点が８０℃以上では、低温での仮圧着性に優れるという本発明の効果を奏し難くなる。   The component (d) preferably has a melting point of 30 ° C. or higher and lower than 80 ° C., more preferably 30 to 70 ° C. If the melting point is less than 30 ° C., it is easy to induce resin seepage during temporary pressure bonding, and workability tends to be reduced. On the other hand, when the melting point is 80 ° C. or higher, it is difficult to achieve the effect of the present invention that the temporary press bonding property at low temperature is excellent.

（ｄ）成分の配合量は、（ａ）及び（ｃ）成分の合計１００質量部に対して、０．５〜５質量部であることが好ましく、１〜３質量部であることがより好ましい。（ｄ）成分の配合量が０．５質量部未満では低温での仮圧着時に優れるという本発明の効果を奏し難くなる傾向にあり、５質量部を超えると接続信頼性や接続外観が低下する傾向にある。   The blending amount of the component (d) is preferably 0.5 to 5 parts by mass, more preferably 1 to 3 parts by mass with respect to 100 parts by mass in total of the components (a) and (c). . When the blending amount of the component (d) is less than 0.5 parts by mass, it tends to be difficult to achieve the effect of the present invention, which is excellent at the time of temporary pressure bonding at a low temperature. There is a tendency.

（ｅ）有機微粒子
本発明に係る回路接続材料には、必要に応じ有機微粒子を配合してもよい。有機微粒子は、応力緩和性を有する耐衝撃緩和剤としての機能を有するものである。回路接続材料が（Ｅ）成分として有機微粒子を含むことで、仮圧着後の本接続における各種接続部材との接着性をより一層向上することができる。特に、（ｂ）成分としてカチオン重合型潜在性硬化剤を用いた回路接続材料の場合、被着体に対する接着強度がアニオン重合型潜在性硬化剤を用いた場合よりもやや劣る傾向があるため、（ｅ）成分を添加することで接着性を改善することができる。 (E) Organic fine particles Organic fine particles may be blended in the circuit connecting material according to the present invention as necessary. The organic fine particles have a function as an impact relaxation agent having stress relaxation properties. By including the organic fine particles as the component (E) in the circuit connection material, it is possible to further improve the adhesiveness with various connection members in the main connection after the temporary pressure bonding. In particular, in the case of a circuit connection material using a cationic polymerization type latent curing agent as the component (b), the adhesive strength to the adherend tends to be slightly inferior to the case where an anion polymerization type latent curing agent is used, (E) Adhesiveness can be improved by adding a component.

有機微粒子としては、例えば、アクリル樹脂、シリコーン樹脂、ブタジエンゴム、ポリエステル、ポリウレタン、ポリビニルブチラール、ポリアリレート、ポリメチルメタクリレート、アクリルゴム、ポリスチレン、ＮＢＲ、ＳＢＲ、シリコーン変性樹脂等を成分として含む共重合体が挙げられる。接着性向上の観点から、有機微粒子として、（メタ）アクリル酸アルキル−ブタジエン−スチレン共重合体、（メタ）アクリル酸アルキル−シリコーン共重合体、シリコーン−（メタ）アクリル共重合体、シリコーンと（メタ）アクリル酸との複合体、（メタ）アクリル酸アルキル−ブタジエン−スチレンとシリコーンとの複合体及び（メタ）アクリル酸アルキルとシリコーンとの複合体を用いることが好ましい。また、（Ｅ）成分として、コアシェル型の構造を有し、コア層とシェル層で組成が異なる有機微粒子を用いることもできる。コアシェル型の有機微粒子として、具体的には、シリコーン−アクリルゴムをコアとてアクリル樹脂をグラフトした粒子、アクリル共重合体にアクリル樹脂をグラフトとした粒子が挙げられる。   Examples of the organic fine particles include an acrylic resin, silicone resin, butadiene rubber, polyester, polyurethane, polyvinyl butyral, polyarylate, polymethyl methacrylate, acrylic rubber, polystyrene, NBR, SBR, a silicone-modified resin as a component. Is mentioned. From the viewpoint of improving adhesiveness, as organic fine particles, (meth) acrylic acid alkyl-butadiene-styrene copolymer, (meth) acrylic acid alkyl-silicone copolymer, silicone- (meth) acrylic copolymer, silicone and ( It is preferable to use a complex of (meth) acrylic acid, a complex of (meth) acrylic acid alkyl-butadiene-styrene and silicone, and a complex of (meth) acrylic acid alkyl and silicone. Further, as the component (E), organic fine particles having a core-shell structure and having different compositions in the core layer and the shell layer can also be used. Specific examples of the core-shell type organic fine particles include particles obtained by grafting an acrylic resin with a silicone-acrylic rubber core, and particles obtained by grafting an acrylic resin on an acrylic copolymer.

（ｅ）成分を配合する場合、その配合量は、（ａ）成分１００質量部に対して、２０〜５０質量部であることが好ましく、３０〜４０質量部であることがより好ましい。（ｅ）成分の配合量を上記範囲とすることで、樹脂層３の被着体に対する接着性と支持フィルムの剥離性とのバランスを調整しやすい傾向にある。   (E) When mix | blending a component, it is preferable that the compounding quantity is 20-50 mass parts with respect to 100 mass parts of (a) component, and it is more preferable that it is 30-40 mass parts. (E) By making the compounding quantity of a component into the said range, it exists in the tendency which is easy to adjust the balance with the adhesiveness with respect to the to-be-adhered body of the resin layer 3, and the peelability of a support film.

さらに、回路接続材料１（樹脂層３）は、充填材、軟化剤、促進剤、老化防止剤、着色剤、難燃化剤、チキソトロピック剤、カップリング剤、フェノール樹脂、メラミン樹脂及びイソシアネート類を含有することもできる。充填材を含有した場合、接続信頼性等の向上が得られるので好ましい。充填材の最大径が導電性粒子５の粒径未満であれば使用でき、配合量は、５〜６０体積％の範囲が好ましい。６０体積％を超すと信頼性向上の効果が飽和する。カップリング剤としては、ビニル基、アクリル基、アミノ基、エポキシ基又はイソシアネート基を有する化合物が、接着性の向上の点から好ましい。   Further, the circuit connecting material 1 (resin layer 3) is composed of a filler, a softener, an accelerator, an anti-aging agent, a colorant, a flame retardant, a thixotropic agent, a coupling agent, a phenol resin, a melamine resin, and isocyanates. Can also be contained. The inclusion of a filler is preferable because it improves connection reliability and the like. If the maximum diameter of a filler is less than the particle size of the electroconductive particle 5, it can be used, and the compounding quantity has the preferable range of 5-60 volume%. If it exceeds 60% by volume, the effect of improving reliability is saturated. As the coupling agent, a compound having a vinyl group, an acrylic group, an amino group, an epoxy group or an isocyanate group is preferable from the viewpoint of improving the adhesiveness.

導電性粒子５としては、Ａｕ、Ａｇ、Ｎｉ、Ｃｕ、はんだ等の金属を含む金属粒子、並びにカーボン粒子が挙げられる。導電性粒子５は、好ましくはＡｕ、Ａｇ、白金族の貴金属類、より好ましくはＡｕからその表層が構成されていることがより好ましい。導電性粒子５の表層がこれらの金属から構成されていることにより、十分なポットライフを得ることができる。導電性粒子５は、Ｎｉ等の遷移金属類の表面をＡｕ等の貴金属類で被覆したものでもよい。あるいは、非導電性のガラス、セラミック、プラスチック等に前記した導通層を被覆等により形成し、最外層を貴金属類としたものでもよい。最外層を貴金属類、核体をプラスチック又は熱溶融金属とした被覆粒子の場合、加熱加圧により変形性を有するので接続時に電極との接触面積が増加し信頼性が向上するので好ましい。   Examples of the conductive particles 5 include metal particles including metals such as Au, Ag, Ni, Cu, and solder, and carbon particles. The conductive particles 5 preferably have a surface layer made of Au, Ag, platinum group noble metals, more preferably Au. When the surface layer of the conductive particles 5 is made of these metals, a sufficient pot life can be obtained. The conductive particles 5 may be those in which the surface of a transition metal such as Ni is coated with a noble metal such as Au. Alternatively, the conductive layer described above may be formed by coating or the like on non-conductive glass, ceramic, plastic, or the like, and the outermost layer may be a noble metal. In the case of coated particles in which the outermost layer is a noble metal and the core is plastic or a hot melt metal, it is preferable because it has deformability by heating and pressurization, so that the contact area with the electrode is increased at the time of connection and the reliability is improved.

導電性粒子の配合量は用途により適宜設定するが、通常は、回路接続材料のうち導電性粒子を除いた成分１００体積部に対して０．１〜３０体積部の範囲である。過剰な導電性粒子による隣接回路の短絡等を防止するためには０．１〜１０体積部とするのがより好ましい。   Although the compounding quantity of electroconductive particle is suitably set according to a use, Usually, it is the range of 0.1-30 volume parts with respect to 100 volume parts of components except electroconductive particle among circuit connection materials. In order to prevent a short circuit of an adjacent circuit due to excessive conductive particles, the content is more preferably 0.1 to 10 parts by volume.

本発明に係る回路接続材料は、図１に示される構成に限定されるものではない。例えば、回路接続材料が、組成の異なる２層以上の層から構成された積層構造を有していてもよい。この場合、潜在性硬化剤と導電性粒子とがそれぞれ別の層に含まれていてもよい。これにより回路接続材料の保存安定性（ポットライフ）が向上する。また、回路接続材料は導電性粒子を含んでいなくてもよい。   The circuit connection material according to the present invention is not limited to the configuration shown in FIG. For example, the circuit connection material may have a laminated structure composed of two or more layers having different compositions. In this case, the latent curing agent and the conductive particles may be included in separate layers. Thereby, the storage stability (pot life) of the circuit connecting material is improved. The circuit connecting material may not contain conductive particles.

本発明に係る回路接続材料は、例えば、半導体チップ、抵抗体チップ、コンデンサチップ等のチップ部品、並びにプリント基板のような、１又は２以上の回路電極（接続端子）を有する回路部材同士が接続された接続構造体を形成するために好適に用いられる。   In the circuit connection material according to the present invention, for example, chip components such as a semiconductor chip, a resistor chip, a capacitor chip, and circuit members having one or more circuit electrodes (connection terminals) such as a printed circuit board are connected. It is preferably used to form a connected structure.

図２は、接続構造体の一実施形態を示す断面図である。図２に示す接続構造体１００は、第一の基板１１及びこれの主面上に形成された第一の回路電極１３を有する第一の回路部材１０と、第二の基板２１及びこれの主面上に形成された第二の回路電極２３を有し、第二の回路電極２３と第一の回路電極１３とが対向するように配置された第二の回路部材２０と、第一の回路部材１０及び第二の回路部材２０の間に介在する接続部１ａとを備える。対向する第一の回路電極１３と第二の回路電極２３とは、電気的に接続されている。   FIG. 2 is a cross-sectional view showing an embodiment of a connection structure. The connection structure 100 shown in FIG. 2 includes a first circuit member 10 having a first substrate 11 and a first circuit electrode 13 formed on the main surface of the first substrate 11, a second substrate 21, and a main body thereof. A second circuit member 20 having a second circuit electrode 23 formed on the surface and disposed so that the second circuit electrode 23 and the first circuit electrode 13 face each other; And a connecting portion 1a interposed between the member 10 and the second circuit member 20. The first circuit electrode 13 and the second circuit electrode 23 facing each other are electrically connected.

接続部１ａは、回路接続材料１が硬化して形成された硬化物であり、硬化した樹脂層３ａと導電性粒子５とから構成されている。接続部１ａは、対向する第一の回路電極１３と第二の回路電極２３とが電気的に接続されるように、第一の回路部材１０と第二の回路部材２０とを接着している。対向する第一の回路電極１３と第二の回路電極２３とは、導電性粒子５を介して電気的に接続されている。なお、接続部が導電性粒子を含有していない場合、第一の回路電極１３と第二の回路電極２３とが直接接着することにより電気的な接続が可能である。   The connection portion 1a is a cured product formed by curing the circuit connection material 1, and includes a cured resin layer 3a and conductive particles 5. The connection portion 1a bonds the first circuit member 10 and the second circuit member 20 so that the first circuit electrode 13 and the second circuit electrode 23 facing each other are electrically connected. . The opposing first circuit electrode 13 and second circuit electrode 23 are electrically connected via the conductive particles 5. In addition, when the connection part does not contain conductive particles, the first circuit electrode 13 and the second circuit electrode 23 are directly bonded to each other so that electrical connection is possible.

第一の基板１１は、ポリエステルテレフタレート、ポリエーテルサルフォン、エポキシ樹脂、アクリル樹脂及びポリイミド樹脂からなる群より選ばれる少なくとも１種の樹脂を含む樹脂フィルムである。第一の回路電極１３は、電極として機能し得る程度の導電性を有する材料（好ましくは金、銀、錫、白金族の金属及びインジウム−錫酸化物からなる群より選ばれる少なくとも一種）から形成されている。   The first substrate 11 is a resin film containing at least one resin selected from the group consisting of polyester terephthalate, polyethersulfone, epoxy resin, acrylic resin, and polyimide resin. The first circuit electrode 13 is formed from a material having conductivity that can function as an electrode (preferably at least one selected from the group consisting of gold, silver, tin, platinum group metals, and indium-tin oxide). Has been.

第二の基板２１はガラス基板である。第二の回路電極は、好ましくは透明導電性材料から形成される。透明導電性材料としては典型的にはＩＴＯが用いられる。   The second substrate 21 is a glass substrate. The second circuit electrode is preferably formed from a transparent conductive material. Typically, ITO is used as the transparent conductive material.

回路部材の接続構造体１００は、例えば、第一の回路部材１０と、上述のフィルム状の回路接続材料１と、第二の回路部材２０とを、第一の回路電極１３と第二の回路電極２３とが対峙するようにこの順に積層した積層体を加熱及び加圧することにより、第一の回路電極１３と第二の回路電極２３とが電気的に接続されるように第一の回路部材１０と第二の回路部材２０とを接続する方法によって、得られる。   The circuit member connection structure 100 includes, for example, the first circuit member 10, the above-described film-like circuit connection material 1, and the second circuit member 20, and the first circuit electrode 13 and the second circuit. The first circuit member is configured so that the first circuit electrode 13 and the second circuit electrode 23 are electrically connected by heating and pressurizing the laminate laminated in this order so as to face the electrode 23. 10 and the second circuit member 20 are obtained.

この方法においては、まず、支持フィルム上に形成されているフィルム状の回路接続材料１を第二の回路部材２０上に貼り合わせた状態で加熱及び加圧して回路接続材料１を仮接着し、支持フィルムを剥離してから、第一の回路部材１０を回路電極を位置合わせしながら載せて、積層体を準備することができる。なお、接続の際の加熱によって発生する揮発成分による接続への影響を防止するために、接続工程の前に回路部材を予め加熱処理しておくことが好ましい。   In this method, first, the circuit-connecting material 1 formed on the support film is temporarily bonded to the second circuit member 20 by heating and pressurizing the circuit-connecting material 1 while being bonded together, After peeling off the support film, the first circuit member 10 can be placed while aligning the circuit electrodes to prepare a laminate. In addition, in order to prevent the influence on the connection by the volatile component which generate | occur | produces by the heating in the case of a connection, it is preferable to heat-process a circuit member previously before a connection process.

図３は、回路接続材料を用いた仮圧着方法の一実施形態を概略断面図により示す工程図である。   FIG. 3 is a process diagram showing a schematic cross-sectional view of one embodiment of a temporary pressure-bonding method using a circuit connecting material.

本実施形態では、まず、支持フィルム７と、該支持フィルム７の一方面上に設けられ、フィルム状の回路接続材料１からなる接着剤層１ｂとを備えるフィルム状接着剤２を用意する（図３（ａ））。   In this embodiment, first, a film-like adhesive 2 provided with a support film 7 and an adhesive layer 1b formed on one surface of the support film 7 and made of a film-like circuit connection material 1 is prepared (FIG. 3 (a)).

次に、接着剤層１ｂの側を第二の回路部材２０の回路電極２３が形成されている面に向けるようにして載せ、貼り合わせた状態で加熱及び加圧して接着剤層１ｂを第二の回路部材２０に仮接着する（図３（ｂ））。仮接着の温度は、８０℃以下であり、７０℃以下であることが好ましく、６０℃以下であることがさらに好ましい。仮接着温度の下限値は特に限定されないが、生産性の観点から５０℃程度である。仮接着の時間は接着温度により適宜調整されるが、０．１〜５秒間で行うことが好ましく、０．５〜３秒間がより好ましい。   Next, the adhesive layer 1b is placed with the side of the second circuit member 20 facing the surface on which the circuit electrode 23 is formed, and the adhesive layer 1b is heated and pressed in the bonded state to apply the second adhesive layer 1b. Is temporarily bonded to the circuit member 20 (FIG. 3B). The temperature for temporary bonding is 80 ° C. or lower, preferably 70 ° C. or lower, and more preferably 60 ° C. or lower. The lower limit of the temporary bonding temperature is not particularly limited, but is about 50 ° C. from the viewpoint of productivity. The temporary bonding time is appropriately adjusted depending on the bonding temperature, but is preferably 0.1 to 5 seconds, and more preferably 0.5 to 3 seconds.

次いで、支持フィルム７を剥離して、接着剤層１ｂを第二の基板２１の主面上に転写する（図３（ｃ））。   Next, the support film 7 is peeled off, and the adhesive layer 1b is transferred onto the main surface of the second substrate 21 (FIG. 3C).

このようにして、接着剤層１ｂが第二の回路部材２０上に仮圧着された後、第一の回路部材１０を、第一の回路電極１３を第二の回路部材２０の側に向けるようにして接着剤層１ｂ上に載せて形成される積層体を加熱及び加圧することで接続構造体１００が得られる。   In this way, after the adhesive layer 1b is temporarily pressure-bonded onto the second circuit member 20, the first circuit member 10 is directed to the first circuit electrode 13 toward the second circuit member 20. Then, the connection structure 100 is obtained by heating and pressurizing the laminate formed on the adhesive layer 1b.

上記積層体を加熱及び加圧する条件は、回路接続材料中の接着剤組成物の硬化性等に応じて、回路接続材料が硬化して十分な接着強度が得られるように、適宜調整される。   Conditions for heating and pressurizing the laminate are appropriately adjusted so that the circuit connecting material is cured and sufficient adhesive strength is obtained in accordance with the curability of the adhesive composition in the circuit connecting material.

接着剤層１ｂの加熱により、第一の回路電極１３と第二の回路電極２３との間の距離を十分に小さくした状態で接着剤層１ｂが硬化して、第一の回路部材１０と第二の回路部材２０とが接続部１ａを介して強固に接続される。   By heating the adhesive layer 1b, the adhesive layer 1b is cured in a state where the distance between the first circuit electrode 13 and the second circuit electrode 23 is sufficiently small, and the first circuit member 10 and the first circuit electrode 10 The second circuit member 20 is firmly connected via the connecting portion 1a.

接着剤層１ｂの硬化により接続部１ａが形成されて、図２に示すような接続構造体１００が得られる。なお、接続の条件は、使用する用途、回路接続材料、回路部材によって適宜選択される。   The connection portion 1a is formed by curing the adhesive layer 1b, and the connection structure 100 as shown in FIG. 2 is obtained. The connection conditions are appropriately selected depending on the intended use, circuit connection material, and circuit member.

本発明は上記実施形態に限定されるものではない。本発明は、その要旨を逸脱しない範囲で様々な変形が可能である。例えば、接続構造体を構成する回路部材が有する基板は、シリコーン及びガリウム／ヒ素等の半導体チップ、並びに、ガラス、セラミックス、ガラス／エポキシ複合体、及びプラスチック等の絶縁基板であってもよい。   The present invention is not limited to the above embodiment. The present invention can be variously modified without departing from the gist thereof. For example, the substrate included in the circuit member constituting the connection structure may be a semiconductor chip such as silicone and gallium / arsenic, and an insulating substrate such as glass, ceramics, glass / epoxy composite, and plastic.

以下に、本発明を実施例に基づいて具体的に説明するが、本発明はこれに限定されるものではない。   Hereinafter, the present invention will be specifically described based on examples, but the present invention is not limited thereto.

本実施例における回路接続材料を構成する各成分は、以下の通りである。
「ＥＰ−４０１０Ｓ」：プロピレンオキサイド変成エポキシ樹脂（エポキシ当量３３０〜３９０、ＡＤＥＫＡ製）
「ＹＬ９８３Ｕ」：ビスフェノールＦ型エポキシ樹脂（エポキシ当量１６５〜１７５、ジャパンエポキシレジン製）
「ＢＰＡ３２８」：アクリル微粒子分散型エポキシ樹脂（アクリル微粒子を１７質量％含有、エポキシ当量２２０〜２４０、日本触媒製）
「ＥＰ−１０３２Ｈ６０」：クレゾールノボラック型エポキシ樹脂（エポキシ当量１６３〜１７５）
「ＨＸ３９４１ＨＰ」：アニオン重合型潜在性硬化剤含有エポキシ樹脂（イミダゾール系マイクロカプセル型硬化剤を３５質量％含有ビスフェノールＦ型及びＡ型エポキシ樹脂混合タイプ、エポキシ当量１６０〜１９０、旭化成ケミカルズ製）
「ＺＸ１３５６−２」：ビスフェノールＡ・Ｆ共重合型フェノキシ樹脂（Ｍｗ５００００、東都化成製）
「ＰＫＨＣ」：ビスフェノールＡ型フェノキシ樹脂（Ｍｗ４５０００、インケム・コーポレーション製）
「アクリルゴムＡ」：ブチルアクリレート４０質量部−エチルアクリレート３０質量部―アクリロニトリル３０質量部―グリシジルメタクリレート３質量部の共重合体（Ｍｗ約８５万）
「ＥＸＬ−２６５５」：有機微粒子（ブタジエン−スチレン−メタクリレート共重合体から形成されたコアシェルポリマー、ローム・アンド・ハース社製）
「ＥＶ４０Ｗ」：エチレン−酢酸ビニル共重合体（酢酸ビニル含有率４１％、Ｍｗ８００００、融点４０℃、メルトフローレート６５ｇ／１０分、三井・デュポンポリケミカル製）
「ＥＶ１５０」：エチレン−酢酸ビニル共重合体（酢酸ビニル含有率３３％、融点６１℃、メルトフローレート３０ｇ／１０分、Ｍｗ１２００００、三井・デュポンポリケミカル製）
「ＡＵＬ−７０４」：平均粒径４μｍのポリスチレン球状粒子の表面に０．１μｍのＮｉ層及びＡｕ層を設けた導電性粒子（積水化学製）
「ＳＨ６０４０」：シランカップリング剤（γ−グリシドキシプロピルトリメトキシシラン、東レ・ダウコーニング・シリコーン（株）製）
「ＳＩ−６０ＬＡ」：カチオン重合型潜在性硬化剤（芳香族スルホニウム塩、三新化学製） Each component which comprises the circuit connection material in a present Example is as follows.
"EP-4010S": propylene oxide modified epoxy resin (epoxy equivalent 330-390, manufactured by ADEKA)
"YL983U": Bisphenol F type epoxy resin (epoxy equivalents 165 to 175, manufactured by Japan Epoxy Resin)
“BPA328”: Acrylic fine particle-dispersed epoxy resin (containing 17% by mass of acrylic fine particles, epoxy equivalent of 220 to 240, manufactured by Nippon Shokubai)
"EP-1032H60": Cresol novolac type epoxy resin (epoxy equivalents 163 to 175)
"HX3941HP": Anionic polymerization type latent curing agent-containing epoxy resin (Bisphenol F type and A type epoxy resin mixed type containing 35% by mass of imidazole microcapsule type curing agent, epoxy equivalents 160 to 190, manufactured by Asahi Kasei Chemicals)
"ZX1356-2": Bisphenol A / F copolymerization type phenoxy resin (Mw 50000, manufactured by Tohto Kasei)
“PKHC”: Bisphenol A type phenoxy resin (Mw 45000, manufactured by Inchem Corporation)
“Acrylic rubber A”: copolymer of butyl acrylate 40 parts by mass—ethyl acrylate 30 parts by mass—acrylonitrile 30 parts by mass—glycidyl methacrylate 3 parts by mass (Mw about 850,000)
"EXL-2655": Organic fine particles (core-shell polymer formed from butadiene-styrene-methacrylate copolymer, manufactured by Rohm and Haas)
“EV40W”: ethylene-vinyl acetate copolymer (vinyl acetate content 41%, Mw 80000, melting point 40 ° C., melt flow rate 65 g / 10 min, manufactured by Mitsui DuPont Polychemical)
“EV150”: ethylene-vinyl acetate copolymer (vinyl acetate content 33%, melting point 61 ° C., melt flow rate 30 g / 10 min, Mw 120,000, manufactured by Mitsui DuPont Polychemicals)
“AUL-704”: Conductive particles (manufactured by Sekisui Chemical Co., Ltd.) provided with a 0.1 μm Ni layer and an Au layer on the surface of polystyrene spherical particles having an average particle diameter of 4 μm
“SH6040”: Silane coupling agent (γ-glycidoxypropyltrimethoxysilane, manufactured by Toray Dow Corning Silicone Co., Ltd.)
“SI-60LA”: Cationic polymerization latent curing agent (aromatic sulfonium salt, Sanshin Chemical)

（実施例１）
「ＥＰ−４０１０Ｓ」３０質量部、「ＹＬ９８３Ｕ」１５質量部、「ＺＸ１３５６−２」のトルエン／酢酸エチル（＝５０／５０）４０質量％溶液５０質量部（不揮発分換算で２０質量部）、「ＰＫＨＣ」のトルエン／酢酸エチル（＝５０／５０）４０質量％溶液５０質量部（不揮発分換算で２０質量部）、「ＥＸＬ−２６５５」１５質量部、「ＥＶ４０Ｗ」の２０質量％トルエン溶液１０質量部（不揮発分換算で２質量部）、「ＡＵＬ−７０４」４質量部、「ＳＨ６０４０」（γ−グリシドキシプロピルトリメトキシシラン、東レ・ダウコーニング・シリコーン（株）製）１質量部及び「ＳＩ−６０ＬＡ」３質量部を配合して混合溶液を得た。得られた混合溶液をアプリケータでＰＥＴフィルム上に塗布し、７０℃１０分間の熱風乾燥により、接着剤層の厚み２０μｍであるフィルム状の回路接続材料を得た。 Example 1
30 parts by weight of “EP-4010S”, 15 parts by weight of “YL983U”, 50 parts by weight of a 40% by weight toluene / ethyl acetate (= 50/50) solution of “ZX1356-2” (20 parts by weight in terms of nonvolatile content), “ 50 parts by mass of toluene / ethyl acetate (= 50/50) 40% by mass (20 parts by mass in terms of non-volatile content) of “PKHC”, 15 parts by mass of “EXL-2655”, 10% by mass of 20% by mass toluene solution of “EV40W” Parts (2 parts by mass in terms of nonvolatile content), 4 parts by mass of “AUL-704”, 1 part by mass of “SH6040” (γ-glycidoxypropyltrimethoxysilane, manufactured by Toray Dow Corning Silicone Co., Ltd.) and “ 3 parts by mass of “SI-60LA” was blended to obtain a mixed solution. The obtained mixed solution was applied onto a PET film with an applicator, and dried with hot air at 70 ° C. for 10 minutes to obtain a film-like circuit connection material having an adhesive layer thickness of 20 μm.

（実施例２）
「ＹＬ９８３Ｕ」２０質量部、「ＢＰＡ３２８」３０質量部、「ＰＫＨＣ」のトルエン／酢酸エチル（＝５０／５０）４０質量％溶液１２５質量部（不揮発分換算で５０質量部）、「ＥＶ４０Ｗ」の２０質量％トルエン溶液１０質量部（不揮発分換算で２質量部）、「ＡＵＬ−７０４」４質量部、「ＳＨ６０４０」１質量部及び「ＳＩ−６０ＬＡ」３質量部となるように各成分を配合した以外は実施例１と同様にして、フィルム状の回路接続材料を得た。 (Example 2)
20 parts by weight of “YL983U”, 30 parts by weight of “BPA328”, 125 parts by weight of a toluene / ethyl acetate (= 50/50) 40% by weight solution of “PKHC” (50 parts by weight in terms of nonvolatile content), 20 of “EV40W” Each component was blended so as to be 10 parts by mass of a toluene solution (2 parts by mass in terms of nonvolatile content), 4 parts by mass of “AUL-704”, 1 part by mass of “SH6040” and 3 parts by mass of “SI-60LA”. Except for this, a film-like circuit connecting material was obtained in the same manner as in Example 1.

（実施例３）
「ＥＶ４０Ｗ」に変えて、「ＥＶ１５０」を用いた以外は、実施例１と同様にして、フィルム状の回路接続材料を得た。 (Example 3)
A film-like circuit connection material was obtained in the same manner as in Example 1 except that “EV150” was used instead of “EV40W”.

（実施例４）
「ＥＰ−１０３２Ｈ６０」５質量部、「ＨＸ３９４１ＨＰ」３５質量部、「ＰＫＨＣ」のトルエン／酢酸エチル（＝５０／５０）４０質量％溶液５０質量部（不揮発分換算で２０質量部）、「アクリルゴムＡ」のトルエン／酢酸エチル（＝５０／５０）１０質量％溶液２００質量部（不揮発分換算で２０質量部）、「ＥＸＬ−２６５５」２０質量部、「ＥＶ４０Ｗ」の２０質量％トルエン溶液１０質量部（不揮発分換算で２質量部）、「ＡＵＬ−７０４」４質量部及び「ＳＨ６０４０」１質量部となるように各成分を配合した以外は実施例１と同様にして、フィルム状の回路接続材料を得た。 Example 4
5 parts by weight of “EP-1032H60”, 35 parts by weight of “HX3941HP”, 50 parts by weight of a toluene / ethyl acetate (= 50/50) 40% by weight solution of “PKHC” (20 parts by weight in terms of nonvolatile content), “acrylic rubber” A "toluene / ethyl acetate (= 50/50) 10 mass% solution 200 mass parts (20 mass parts in terms of non-volatile content)," EXL-2655 "20 mass parts," EV40W "20 mass% toluene solution 10 mass Parts (2 parts by mass in terms of non-volatile content), 4 parts by mass of “AUL-704” and 1 part by mass of “SH6040”, except that each component was blended in the same manner as in Example 1 to form a film-like circuit connection Obtained material.

（実施例５）
「ＢＰＡ３２８」１０質量部、「ＨＸ３９４１ＨＰ」４０質量部、「ＰＫＨＣ」のトルエン／酢酸エチル（＝５０／５０）４０質量％溶液３７．５質量部（不揮発分換算で１５質量部）、「アクリルゴムＡ」のトルエン／酢酸エチル（＝５０／５０）１０質量％溶液３５０質量部（不揮発分換算で３５質量部）、「ＥＶ４０Ｗ」の２０質量％トルエン溶液１０質量部（不揮発分換算で２質量部）、「ＡＵＬ−７０４」４質量部及び「ＳＨ６０４０」１質量部となるように各成分を配合した以外は実施例１と同様にして、フィルム状の回路接続材料を得た。 (Example 5)
10 parts by weight of “BPA328”, 40 parts by weight of “HX3941HP”, 37.5 parts by weight of a toluene / ethyl acetate (= 50/50) 40% by weight solution of “PKHC” (15 parts by weight in terms of nonvolatile content), “acrylic rubber” A "toluene / ethyl acetate (= 50/50) 10 mass% solution 350 mass parts (non-volatile content conversion 35 mass parts)," EV40W "20 mass% toluene solution 10 mass parts (non-volatile content conversion 2 mass parts) ), 4 parts by mass of “AUL-704” and 1 part by mass of “SH6040” In the same manner as in Example 1 except that each component was blended, a film-like circuit connection material was obtained.

（比較例１）
「ＥＶ４０Ｗ」を添加しなかった以外は、実施例１と同様にして、フィルム状の回路接続材料を得た。 (Comparative Example 1)
A film-like circuit connection material was obtained in the same manner as in Example 1 except that “EV40W” was not added.

（比較例２）。
「ＥＶ４０Ｗ」を添加しなかった以外は、実施例２と同様にして、フィルム状の回路接続材料を得た。 (Comparative example 2).
A film-like circuit connecting material was obtained in the same manner as in Example 2 except that “EV40W” was not added.

（比較例３）
「ＥＶ４０Ｗ」を添加しなかった以外は、実施例４と同様にして、フィルム状の回路接続材料を得た。 (Comparative Example 3)
A film-like circuit connection material was obtained in the same manner as in Example 4 except that “EV40W” was not added.

（比較例４）。
「ＥＶ４０Ｗ」を添加しなかった以外は、実施例５と同様にして、フィルム状の回路接続材料を得た。 (Comparative Example 4).
A film-like circuit connecting material was obtained in the same manner as in Example 5 except that “EV40W” was not added.

実施例で作製した回路接続材料の組成を質量部（不揮発分換算）で表１に、比較例で作製した回路接続材料の組成を質量部（不揮発分換算）で表２にそれぞれ示す。   The composition of the circuit connection material produced in the examples is shown in Table 1 in terms of parts by mass (in terms of nonvolatile content), and the composition of the circuit connection material produced in the comparative example is shown in Table 2 in terms of parts by mass (in terms of nonvolatile content).

Figure 2015091957
Figure 2015091957

Figure 2015091957
Figure 2015091957

［仮圧着性の評価］
上記フィルム状の回路接続材料の接着剤層面を、全面に酸化インジウム（ＩＴＯ）の薄層を有する厚み０．７ｍｍのガラス板に、それぞれ６０℃、７０℃、８０℃で１ＭＰａの条件で、１秒間又は３秒間仮接着した後ＰＥＴフィルムを剥離することで、仮圧着性を評価した。接着剤層が均一にＩＴＯ上に転写されている状態を「Ａ」、接着剤層が部分的にＩＴＯ上に転写されている状態を「Ｂ」、接着剤層がＩＴＯ上に全く転写されない状態を「Ｃ」とした。実施例の評価結果を表３に、比較例の評価結果を表４に示す。 [Evaluation of temporary press bonding]
The adhesive layer surface of the film-like circuit connecting material is formed on a 0.7 mm-thick glass plate having a thin layer of indium oxide (ITO) on the entire surface under conditions of 1 MPa at 60 ° C., 70 ° C. and 80 ° C., respectively. After temporarily bonding for 3 seconds or 3 seconds, the PET film was peeled off to evaluate the temporary press bonding property. The state where the adhesive layer is uniformly transferred onto the ITO is “A”, the state where the adhesive layer is partially transferred onto the ITO is “B”, and the state where the adhesive layer is not transferred onto the ITO at all. Was “C”. Table 3 shows the evaluation results of the examples, and Table 4 shows the evaluation results of the comparative examples.

Figure 2015091957
Figure 2015091957

Figure 2015091957
Figure 2015091957

本発明に係るフィルム状の回路接続材料は、６０℃１秒間と極めて低温かつ短時間の条件においても仮圧着性に十分に優れることが確認された。   It was confirmed that the film-like circuit connecting material according to the present invention was sufficiently excellent in temporary press bonding properties even at a very low temperature and a short time of 60 ° C. for 1 second.

１…回路接続材料、２…フィルム状接着剤、１ａ…接続部、１ｂ…接着剤層、３…樹脂層、３ａ…硬化した樹脂層、５…導電性粒子、７…支持フィルム、１０…第一の回路部材、１１…第一の基板、１３…第一の回路電極、２０…第二の回路部材、２１…第二の基板、２３…第二の回路電極、１００…接続構造体。   DESCRIPTION OF SYMBOLS 1 ... Circuit connection material, 2 ... Film adhesive, 1a ... Connection part, 1b ... Adhesive layer, 3 ... Resin layer, 3a ... Hardened resin layer, 5 ... Conductive particle, 7 ... Support film, 10 ... No. 1 circuit member, 11 ... first substrate, 13 ... first circuit electrode, 20 ... second circuit member, 21 ... second substrate, 23 ... second circuit electrode, 100 ... connection structure.

Claims (1)

対向する回路電極同士を電気的に接続する回路接続材料であって、
（ａ）エポキシ樹脂と、
（ｂ）潜在性硬化剤と、
（ｃ）フィルム形成材と、
（ｄ）カルボン酸ビニルエステルをモノマー単位として含む熱可塑性ポリマーと、
を含有する回路接続材料。 A circuit connection material for electrically connecting opposing circuit electrodes,
(A) an epoxy resin;
(B) a latent curing agent;
(C) a film forming material;
(D) a thermoplastic polymer containing a carboxylic acid vinyl ester as a monomer unit;
A circuit connecting material containing.
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