JP2017141328A - Transparent conductive adhesive, laminate, and substrate joining method - Google Patents
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Abstract
Description
本発明は、透明導電性接着剤、積層体、及び基板の接合方法に関する。 The present invention relates to a transparent conductive adhesive, a laminate, and a method for bonding substrates.
多接合型の太陽電池や縦型構造の発光素子の作製等において、基板同士を透光性と導電性の両方を確保した状態で接合する技術が求められている。例えば、特許文献１（特開２０１１−１３８７１１号公報）には、透明樹脂と金属ナノワイヤを混合した透明導電性接着剤が開示されている。しかしながら、特許文献１に開示される透明導電性接着剤を用いた接合では、厚み方向での導電性が不十分であった。 In manufacturing a multi-junction solar cell or a vertical light-emitting element, a technique for joining substrates in a state where both translucency and conductivity are secured is required. For example, Patent Document 1 (Japanese Patent Laid-Open No. 2011-138711) discloses a transparent conductive adhesive in which a transparent resin and metal nanowires are mixed. However, in the joining using the transparent conductive adhesive disclosed in Patent Document 1, the conductivity in the thickness direction is insufficient.
また、非特許文献１（T. Sameshima et al., " Multi Junction Solar Cells Stacked with Transparent and Conductive Adhesive", Jpn. J. Appl. Phys. 50 (2011) 052301）では、導電性接着剤と酸化インジウムスズ（ＩＴＯ）粒子を混合することにより、透明導電性接着剤を作製する方法が報告されている。 In Non-Patent Document 1 (T. Sameshima et al., “Multi Junction Solar Cells Stacked with Transparent and Conductive Adhesive”, Jpn. J. Appl. Phys. 50 (2011) 052301), a conductive adhesive and indium oxide are used. A method for producing a transparent conductive adhesive by mixing tin (ITO) particles has been reported.
しかしながら、透明導電性接着剤には、より高い透光性と導電性が望まれる。 However, higher translucency and conductivity are desired for the transparent conductive adhesive.
本発明者らは、今般、透明樹脂接着剤に、特定の粒度分布を有する導電性球状粒子を所定割合で配合することにより、高い導電性と透光性を両立した基板接合を可能とする透明導電性接着剤を提供できるとの知見を得た。 The inventors of the present invention have recently added transparent spherical adhesive having a specific particle size distribution to a transparent resin adhesive in a predetermined ratio, thereby enabling transparent substrate bonding that achieves both high conductivity and translucency. The knowledge that a conductive adhesive can be provided was obtained.
したがって、本発明の目的は、高い導電性と透光性を両立した基板接合を可能とする透明導電性接着剤を提供することにある。 Accordingly, an object of the present invention is to provide a transparent conductive adhesive that enables substrate bonding that achieves both high electrical conductivity and translucency.
本発明の一態様によれば、透明樹脂接着剤１００重量部と、導電性球状粒子０．５〜３０重量部とを含み、
前記導電性球状粒子が、体積基準Ｄ９０粒径の体積基準Ｄ１０粒径に対する比であるＤ９０／Ｄ１０が３．０以下である粒度分布を有する、透明導電性接着剤が提供される。
According to one aspect of the present invention, comprising 100 parts by weight of a transparent resin adhesive and 0.5 to 30 parts by weight of conductive spherical particles,
A transparent conductive adhesive is provided in which the conductive spherical particles have a particle size distribution in which D90 / D10, which is the ratio of the volume-based D90 particle size to the volume-based D10 particle size, is 3.0 or less.
本発明の他の一態様によれば、第一基板と、
前記第一基板と対向して設けられる第二基板と、
前記第一基板及び前記第二基板との間に介在し、上記透明導電性接着剤で構成される透明導電接着層と、
を備え、前記透明導電接着層の厚さが前記導電性球状粒子１個相当の高さに等しい、積層体が提供される。
According to another aspect of the invention, a first substrate;
A second substrate provided facing the first substrate;
A transparent conductive adhesive layer interposed between the first substrate and the second substrate, and configured with the transparent conductive adhesive; and
And a laminated body in which the thickness of the transparent conductive adhesive layer is equal to the height corresponding to one conductive spherical particle.
本発明の他の一態様によれば、第一基板及び第二基板を用意する工程と、
前記第一基板及び前記第二基板の少なくともいずれか一方の表面に上記透明導電性接着剤を塗布する工程と、
前記第一基板と前記第二基板とを前記透明導電性接着剤を挟むように積層して積層体とする工程と、
前記積層体を加圧して、厚さが前記導電性球状粒子１個相当の高さに等しい、前記透明導電性接着剤で構成される透明導電接着層を形成する工程と
を含む、基板の接合方法が提供される。
According to another aspect of the invention, providing a first substrate and a second substrate;
Applying the transparent conductive adhesive to the surface of at least one of the first substrate and the second substrate;
A step of laminating the first substrate and the second substrate so as to sandwich the transparent conductive adhesive;
Pressurizing the laminate to form a transparent conductive adhesive layer composed of the transparent conductive adhesive, the thickness of which is equal to the height corresponding to one conductive spherical particle. A method is provided.
接着剤
本発明の透明導電性接着剤は、透明樹脂接着剤１００重量部と、導電性球状粒子０．５〜３０重量部とを含む。導電性球状粒子は、体積基準Ｄ９０粒径の体積基準Ｄ１０粒径に対する比であるＤ９０／Ｄ１０が３．０以下である粒度分布を有する。このように、特定の粒度分布を有する導電性球状粒子を所定割合で配合することにより、高い導電性と透光性を両立した基板接合を可能とする透明導電性接着剤を提供することが可能となる。すなわち、Ｄ９０／Ｄ１０が３．０以下である粒度分布は、導電性球状粒子の粒径の均一性が高いことを意味する。これはＤ１０が大きいことは相対的に粒径の小さい導電性球状粒子の割合が少ないことを意味し、Ｄ９０が小さいことは相対的に粒径の大きい導電性球状粒子の割合が少ないことを意味するためである。したがって、Ｄ９０／Ｄ１０が３．０以下と小さいことは、Ｄ９０が小さく、かつ、Ｄ１０が大きいことを意味することから、粒径の大きい導電性球状粒子及び粒径の小さい導電性球状粒子のいずれも少ない、すなわち粒径の均一性が高いことを意味する。そして、透明樹脂接着剤と粒径の均一性が高い導電性球状粒子とを所定割合で含む透明導電性接着剤を用いて基板を接合することで、透光性と導電性の高い基板接合が可能となる。すなわち、粒径の均一性が高いと、図１に示されるように、透明導電性接着剤で構成される透明導電接着層１２の厚さと導電性球状粒子１４の粒径をほぼ等しくすることができ、加圧されることで透明導電接着層１２の厚さが導電性球状粒子１４の１個相当の高さに等しくなる。その結果、透明導電接着層１２の厚さ方向に１個の導電性球状粒子１４で第一基板１８と第二基板２０との間の導通を取ることが可能となる。これにより、少ない導電性球状粒子１４の添加量でも、透明導電接着層１２の厚さ方向に十分に高い導電性を確保することができる。導電性球状粒子１４は透光性が低いが、その添加量が少ないため、透明樹脂接着剤１６によってもたらされる高い透光性を両立することができる。この点、導電性球状粒子１４の粒径の均一性が低い場合（すなわちＤ９０／Ｄ１０が大きい場合）、透明導電接着層１２の厚さ方向に導電性を確保するためには、複数の導電性球状粒子１４を厚さ方向に連結させる（積み上げる）必要があるが、これには多量の導電性球状粒子１４を添加する必要があり、透光性が低下してしまう。これに対し、本発明の透明導電性接着剤においては、透明樹脂接着剤１００重量部に対して、導電性球状粒子の配合量を０．５〜３０重量部と有意に少なくすることにより、透光性の低下を回避する、すなわち高い透光性を確保することができる。こうして透光性と導電性の高い基板接合が可能となる。
Adhesive The transparent conductive adhesive of the present invention contains 100 parts by weight of a transparent resin adhesive and 0.5 to 30 parts by weight of conductive spherical particles. The conductive spherical particles have a particle size distribution in which D90 / D10, which is the ratio of the volume-based D90 particle size to the volume-based D10 particle size, is 3.0 or less. Thus, by blending conductive spherical particles having a specific particle size distribution at a predetermined ratio, it is possible to provide a transparent conductive adhesive that enables substrate bonding that achieves both high conductivity and translucency. It becomes. That is, a particle size distribution with D90 / D10 of 3.0 or less means that the particle size uniformity of the conductive spherical particles is high. This means that a large D10 means that the proportion of conductive spherical particles having a relatively small particle size is small, and a small D90 means that the proportion of conductive spherical particles having a relatively large particle size is small. It is to do. Therefore, D90 / D10 being as small as 3.0 or less means that D90 is small and D10 is large. Therefore, any of conductive spherical particles having a large particle diameter and conductive spherical particles having a small particle diameter can be used. Means that the uniformity of the particle size is high. Then, by bonding the substrate using a transparent conductive adhesive containing a transparent resin adhesive and conductive spherical particles having a high particle size uniformity at a predetermined ratio, the substrate bonding with high translucency and conductivity can be achieved. It becomes possible. That is, when the uniformity of the particle size is high, as shown in FIG. 1, the thickness of the transparent conductive adhesive layer 12 made of a transparent conductive adhesive and the particle size of the conductive spherical particles 14 can be made substantially equal. When the pressure is applied, the thickness of the transparent conductive adhesive layer 12 becomes equal to the height corresponding to one of the conductive spherical particles 14. As a result, it is possible to establish conduction between the first substrate 18 and the second substrate 20 with one conductive spherical particle 14 in the thickness direction of the transparent conductive adhesive layer 12. Thereby, even if the addition amount of the conductive spherical particles 14 is small, sufficiently high conductivity can be secured in the thickness direction of the transparent conductive adhesive layer 12. Although the conductive spherical particles 14 have low translucency, since the addition amount is small, it is possible to achieve both high translucency provided by the transparent resin adhesive 16. In this regard, when the uniformity of the particle diameter of the conductive spherical particles 14 is low (that is, when D90 / D10 is large), in order to ensure conductivity in the thickness direction of the transparent conductive adhesive layer 12, a plurality of conductive Although it is necessary to connect (stack) the spherical particles 14 in the thickness direction, a large amount of the conductive spherical particles 14 need to be added to this, and the translucency is lowered. On the other hand, in the transparent conductive adhesive of the present invention, the amount of conductive spherical particles is significantly reduced to 0.5 to 30 parts by weight with respect to 100 parts by weight of the transparent resin adhesive. A decrease in light property can be avoided, that is, high light transmittance can be ensured. In this way, highly transparent and conductive substrate bonding is possible.
透明樹脂接着剤は市販の透明樹脂接着剤が使用可能であり、硬化後に所望の透明性を呈することができるものであれば、導電性の有無は問わない。透明導電性接着剤層の厚さ方向の導電性は導電性球状粒子によって確保すれば足りるからである。透明導電性接着剤の好ましい例としては、熱硬化型接着剤、紫外線硬化型接着剤が挙げられる。特に好ましくは、透明樹脂接着剤は加熱しながらの加圧により基板接合を望ましい形で効率的に行える点で熱硬化型接着剤である。熱硬化型接着剤の好ましい主成分としては、変性シリコーン樹脂、フェニルレジン、フェニルゴム、フロロゴム、メチルゴム、フェニルゲルが挙げられる。透明樹脂接着剤は１液型であってもよいし、２液型であってもよい。 As the transparent resin adhesive, a commercially available transparent resin adhesive can be used, and it does not matter whether or not it has conductivity as long as it can exhibit desired transparency after curing. This is because the conductivity in the thickness direction of the transparent conductive adhesive layer only needs to be ensured by the conductive spherical particles. Preferable examples of the transparent conductive adhesive include a thermosetting adhesive and an ultraviolet curable adhesive. Particularly preferably, the transparent resin adhesive is a thermosetting adhesive in that the substrate can be bonded efficiently in a desired form by applying pressure while heating. Preferable main components of the thermosetting adhesive include modified silicone resin, phenyl resin, phenyl rubber, fluoro rubber, methyl rubber, and phenyl gel. The transparent resin adhesive may be a one-component type or a two-component type.
導電性球状粒子は少なくともその表面が導電性を有するあらゆる球状粒子が使用可能である。したがって、本発明の透明導電性接着剤は非球状粒子（例えば針状粒子、板状粒子、ナノワイヤ等）を含まないのが好ましい。導電性球体粒子の少なくとも表面は金属等の導電性材料で構成されるのが好ましい。導電性球体粒子の全体が導電性材料で構成されてもよい。導電性球状粒子の配合量は、透明樹脂接着剤１００重量部に対して、０．５〜３０重量部であり、好ましくは０．５〜２５重量部、より好ましくは０．５〜２０重量部、さらに好ましくは１．０〜１５重量部、特に好ましくは１．０〜１０重量部、最も好ましくは１．０〜５．０重量部である。このような範囲内であると、透明樹脂接着剤による接着機能を十分に確保しながら、透明導電接着層において高い導電性と透明性をより望ましく実現することができる。 As the conductive spherical particles, any spherical particles having at least a surface having conductivity can be used. Therefore, it is preferable that the transparent conductive adhesive of the present invention does not contain non-spherical particles (for example, acicular particles, plate-like particles, nanowires, etc.). It is preferable that at least the surface of the conductive sphere particles is made of a conductive material such as metal. The entirety of the conductive sphere particles may be made of a conductive material. The blending amount of the conductive spherical particles is 0.5 to 30 parts by weight, preferably 0.5 to 25 parts by weight, more preferably 0.5 to 20 parts by weight with respect to 100 parts by weight of the transparent resin adhesive. More preferably, it is 1.0 to 15 parts by weight, particularly preferably 1.0 to 10 parts by weight, and most preferably 1.0 to 5.0 parts by weight. Within such a range, it is possible to more desirably realize high conductivity and transparency in the transparent conductive adhesive layer while sufficiently securing the bonding function of the transparent resin adhesive.
導電性球状粒子は、体積基準Ｄ９０粒径の体積基準Ｄ１０粒径に対する比であるＤ９０／Ｄ１０が３．０以下である粒度分布を有するのが好ましく、より好ましくは２．８以下、さらに好ましくは２．５以下、特に好ましくは２．３以下、最も好ましくは２．０以下である。Ｄ９０／Ｄ１０の下限値は特に限定されないが、現実的には１．０５、より現実的には１．１である。このような範囲内であると粒径の均一性が有意に高くなるため、導電性の更なる向上につながる。体積基準Ｄ９０粒径及び体積基準Ｄ１０粒径は、市販のレーザー回折・散乱式粒度分析計により測定することができる。 The conductive spherical particles preferably have a particle size distribution in which D90 / D10, which is the ratio of the volume-based D90 particle size to the volume-based D10 particle size, is 3.0 or less, more preferably 2.8 or less, and still more preferably It is 2.5 or less, particularly preferably 2.3 or less, and most preferably 2.0 or less. The lower limit value of D90 / D10 is not particularly limited, but is actually 1.05, and more realistically 1.1. Within such a range, the uniformity of the particle size is significantly increased, leading to further improvement in conductivity. The volume standard D90 particle size and the volume standard D10 particle size can be measured by a commercially available laser diffraction / scattering particle size analyzer.
導電性球状粒子は、体積基準Ｄ５０粒径が１〜２０μｍであるのが好ましく、より好ましくは１〜１５μｍ、さらに好ましくは１〜１２μｍ、特に好ましくは２〜１０μｍ、最も好ましくは２〜８μｍである。このような範囲内であると、透明導電接着層において高い導電性と透明性をより望ましく実現することができる。体積基準Ｄ５０粒径は、市販のレーザー回折・散乱式粒度分析計により測定することができる。 The conductive spherical particles preferably have a volume-based D50 particle size of 1 to 20 μm, more preferably 1 to 15 μm, still more preferably 1 to 12 μm, particularly preferably 2 to 10 μm, and most preferably 2 to 8 μm. . Within such a range, high conductivity and transparency can be more desirably realized in the transparent conductive adhesive layer. The volume standard D50 particle size can be measured by a commercially available laser diffraction / scattering particle size analyzer.
本発明の好ましい態様によれば、導電性球状粒子は、樹脂で構成されるコア粒子と、コア粒子の表面を被覆する導電性層とを含む。このような構成の導電性球状粒子は市販されている。この場合、導電性球状粒子は、コア粒子が樹脂で構成されるため、プレスされた際に変形しやすい。このため、図１に示されるように各導電性球状粒子が２枚の基板の双方とも接点を確保しやすくなり、その結果、透明導電性接着剤層の導電性の向上につながる。コア粒子を構成する樹脂は特に限定されず、公知の種々の樹脂であることができる。例えば、アクリル、ジビニルベンゼンポリマーである。導電性層は導電性材料で構成されていればよく特に限定されないが、例えばＡｕ、Ａｇ、Ｃｕ、はんだ、Ｎｉ、Ａｌ等の金属であることができる。導電性層を構成する特に好ましい金属は、酸化されにくいが故に高い導電性を長期間維持できる点でＡｕ又はＡｇである。 According to a preferred aspect of the present invention, the conductive spherical particles include core particles made of a resin and a conductive layer that covers the surface of the core particles. Conductive spherical particles having such a structure are commercially available. In this case, the conductive spherical particles are easily deformed when pressed because the core particles are made of resin. For this reason, as shown in FIG. 1, each conductive spherical particle can easily secure a contact point on both of the two substrates, and as a result, the conductivity of the transparent conductive adhesive layer is improved. The resin constituting the core particle is not particularly limited, and may be various known resins. For example, acrylic and divinylbenzene polymers. The conductive layer is not particularly limited as long as it is made of a conductive material. For example, the conductive layer can be a metal such as Au, Ag, Cu, solder, Ni, and Al. A particularly preferable metal constituting the conductive layer is Au or Ag because it is difficult to oxidize and can maintain high conductivity for a long period of time.
基板の接合方法及び積層体
本発明の透明導電性接着剤を用いることで、高い導電性と透光性を両立した基板の接合を可能とすることができ、それにより高い導電性と透光性を両立した積層体を提供することができる。本発明による基板の接合方法は、基板の用意、透明導電性接着剤の塗布、基板の積層、及び積層体の加圧を含む。
Bonding method and laminate of substrate By using the transparent conductive adhesive of the present invention, it is possible to bond a substrate having both high conductivity and translucency, and thereby high conductivity and translucency. Can be provided. The substrate bonding method according to the present invention includes preparing a substrate, applying a transparent conductive adhesive, laminating the substrates, and pressing the laminate.
（１）基板の用意
まず、第一基板１８及び第二基板２０を用意する。第一基板１８及び第二基板２０はいずれも透明樹脂接着剤によって接着可能ないかなる基板であってもよく、特に限定されない。もっとも、本発明の透明導電性接着剤によってもたらされる導電性の利点を享受するためには、第一基板１８の第二基板２０と接合される表面と、第二基板２０の第一基板１８と接合されるべき表面とが導電性を有するのが好ましいのはいうまでもない。例えば、第一基板１８の第二基板２０と接合される表面と、第二基板２０の第一基板１８と接合されるべき表面とが、それぞれ酸化物セラミックスで構成されるのが好ましい。典型的には、第一基板１８及び／又は第二基板２０が酸化物セラミックスで構成され、より典型的には第一基板１８及び第二基板２０の両方が同種又は異種の酸化物セラミックスで構成される。酸化物セラミックスの例としては、酸化亜鉛、インジウム−スズ酸化物、酸化チタン、酸化スズが挙げられ、特に好ましくは酸化亜鉛である。酸化物セラミックスには導電性を付与又は向上させるためのドーパントが添加されているのが好ましく、そのようなドーパントの例としてはＡｌ、Ｇａ、Ｉｎ、Ｎｂ、Ｆ、及びそれらの任意の組合せが挙げられる。また、本発明の透明導電性接着剤によってもたらされる透明性の利点を享受するためには、第一基板１８及び第二基板２０の少なくともいずれか一方が透明であるのが好ましく、より好ましくは第一基板１８及び第二基板２０の両方が透明である。
(1) Preparation of substrate First, the first substrate 18 and the second substrate 20 are prepared. The first substrate 18 and the second substrate 20 may be any substrates that can be bonded by a transparent resin adhesive, and are not particularly limited. However, in order to enjoy the conductive advantage provided by the transparent conductive adhesive of the present invention, the surface of the first substrate 18 bonded to the second substrate 20, the first substrate 18 of the second substrate 20, and Needless to say, the surfaces to be joined preferably have electrical conductivity. For example, the surface of the first substrate 18 to be bonded to the second substrate 20 and the surface of the second substrate 20 to be bonded to the first substrate 18 are preferably made of oxide ceramics. Typically, the first substrate 18 and / or the second substrate 20 are made of oxide ceramics, and more typically both the first substrate 18 and the second substrate 20 are made of the same or different oxide ceramics. Is done. Examples of oxide ceramics include zinc oxide, indium-tin oxide, titanium oxide, and tin oxide, with zinc oxide being particularly preferred. It is preferable that a dopant for imparting or improving conductivity is added to the oxide ceramic, and examples of such a dopant include Al, Ga, In, Nb, F, and any combination thereof. It is done. Further, in order to enjoy the advantage of transparency brought about by the transparent conductive adhesive of the present invention, it is preferable that at least one of the first substrate 18 and the second substrate 20 is transparent, more preferably the first substrate. Both the one substrate 18 and the second substrate 20 are transparent.
（２）透明導電性接着剤の塗布
次いで、第一基板１８及び第二基板２０の少なくともいずれか一方の表面に上記透明導電性接着剤を塗布する。塗布の仕方は公知の手法に従えばよく特に限定されないが、薄く均一に塗布するのが後述する積層後の加圧の際に、透明導電接着層１２の望ましい厚さを実現しやすい点で好ましい。
(2) Application of transparent conductive adhesive Next, the transparent conductive adhesive is applied to the surface of at least one of the first substrate 18 and the second substrate 20. The method of application is not particularly limited as long as it follows a known method, but it is preferable to apply thinly and uniformly from the viewpoint of easily achieving the desired thickness of the transparent conductive adhesive layer 12 during pressurization after lamination, which will be described later. .
透明導電性接着剤は、透明樹脂接着剤１６と導電性球状粒子１４を均一に混合することにより製造するのが好ましい。この混合は自転・公転ミキサー等のミキサーで気泡ができるだけ入らないように行うのが好ましい。また、得られた混合物を真空中で保持して脱泡を行うのがより好ましい。透明樹脂接着剤１６と導電性球状粒子１４を別個に保管しておき上記混合を基板接合の直前に行ってもよい。あるいは、透明樹脂接着剤１６と導電性球状粒子１４を予め混合しておくことでそのまま使える透明導電性接着剤として保管及び提供してもよい。 The transparent conductive adhesive is preferably produced by uniformly mixing the transparent resin adhesive 16 and the conductive spherical particles 14. This mixing is preferably carried out so that bubbles do not enter as much as possible with a mixer such as a rotation / revolution mixer. Further, it is more preferable to perform defoaming by holding the obtained mixture in a vacuum. The transparent resin adhesive 16 and the conductive spherical particles 14 may be stored separately, and the above mixing may be performed immediately before substrate bonding. Or you may store and provide as a transparent conductive adhesive which can be used as it is by mixing the transparent resin adhesive 16 and the conductive spherical particles 14 in advance.
（３）基板の積層
続けて、第一基板１８と第二基板２０とを透明導電性接着剤を挟むように積層して積層体とする。これにより透明導電性接着剤を介して第一基板１８と第二基板２０とが接合される。第一基板１８と第二基板２０との間の接着は、透明導電性接着剤に含まれる透明樹脂接着剤１６の持つ接着機能によって可能とされる。積層は、第一基板１８と第二基板２０との間に気泡が入り込まないように行うのが好ましい。
(3) Lamination of Substrate Subsequently, the first substrate 18 and the second substrate 20 are laminated so as to sandwich the transparent conductive adhesive to form a laminate. Thereby, the 1st board | substrate 18 and the 2nd board | substrate 20 are joined via a transparent conductive adhesive. Adhesion between the first substrate 18 and the second substrate 20 is made possible by the adhesion function of the transparent resin adhesive 16 included in the transparent conductive adhesive. The lamination is preferably performed so that bubbles do not enter between the first substrate 18 and the second substrate 20.
（４）積層体の加圧
この積層体を加圧して透明導電性接着剤で構成される透明導電接着層１２を形成する。加圧は透明導電接着層１２の厚さが導電性球状粒子１４の１個相当の高さに等しくなるように行われる。こうして得られる積層体１０は透明導電接着層１２の厚さ方向に１個の導電性球状粒子１４で第一基板１８と第二基板２０との間の導通を取ることが可能となるため、導電性が有意に向上する。このとき、導電性球状粒子１４を加圧により厚さ方向に変形させながら第一基板１８と第二基板２０とを接合させることが好ましい。こうすることで、接触抵抗をより一層低減できるとともに、できるだけ多数の導電性球状粒子１４を、透明導電接着層１２の厚さ方向の基板１８，２０間の直接的な電気的接続（１個の粒子による電気的接続）に関与させることができる。その結果、透明導電接着層１２の厚み方向に１個の導電性球状粒子１４でもたらされる導通をより一層多く確保することができる。この加圧は１〜５００ｋｇｆ／ｃｍ２の圧力で行われるのが好ましく、より好ましくは４〜５００ｋｇｆ／ｃｍ２、さらに好ましくは２０〜４００ｋｇｆ／ｃｍ２、特に好ましくは８０〜３００ｋｇｆ／ｃｍ２、最も好ましくは１００〜３００ｋｇｆ／ｃｍ２である。加圧は加熱しながら行ってもよい。特に、透明樹脂接着剤１６が熱硬化型接着剤の場合、加熱しながらの加圧により、導電性球状粒子１４による基板１８，２０間の導通をできるだけ多く確保しながら、接着剤を望ましく硬化させることができる。加圧は、重しや押し板等の公知の手段を用いて行えばよく特に限定されないが、好ましくは、ホットプレート付きのプレス機を用いることで加熱しながら効率的に加圧を行うことができる。加熱は透明樹脂接着剤１６（特に熱硬化型接着剤）の硬化を促進させることが可能な温度であるのが好ましく、例えば６０〜３００℃、より好ましくは８０〜２００℃である。
(4) Pressurization of laminated body This laminated body is pressurized and the transparent conductive adhesive layer 12 comprised with a transparent conductive adhesive is formed. The pressing is performed so that the thickness of the transparent conductive adhesive layer 12 is equal to the height corresponding to one of the conductive spherical particles 14. Since the laminated body 10 thus obtained can establish electrical continuity between the first substrate 18 and the second substrate 20 with one conductive spherical particle 14 in the thickness direction of the transparent conductive adhesive layer 12. Sex is significantly improved. At this time, it is preferable to join the first substrate 18 and the second substrate 20 while deforming the conductive spherical particles 14 in the thickness direction by pressurization. In this way, the contact resistance can be further reduced, and as many conductive spherical particles 14 as possible can be directly connected between the substrates 18 and 20 in the thickness direction of the transparent conductive adhesive layer 12 (one piece). Electrical connection by particles). As a result, it is possible to further secure the electrical conduction provided by one conductive spherical particle 14 in the thickness direction of the transparent conductive adhesive layer 12. This pressurization is preferably performed at a pressure of 1 to 500 kgf / cm 2 , more preferably 4 to 500 kgf / cm 2 , still more preferably 20 to 400 kgf / cm 2 , particularly preferably 80 to 300 kgf / cm 2 , most preferably Preferably it is 100-300 kgf / cm < 2 >. Pressurization may be performed while heating. In particular, when the transparent resin adhesive 16 is a thermosetting adhesive, the adhesive is desirably cured while ensuring as much conduction as possible between the substrates 18 and 20 by the conductive spherical particles 14 by applying pressure while heating. be able to. The pressurization is not particularly limited as long as it is performed using a known means such as a weight or a push plate. Preferably, the pressurization can be efficiently performed while heating by using a press machine with a hot plate. it can. The heating is preferably at a temperature that can accelerate the curing of the transparent resin adhesive 16 (particularly thermosetting adhesive), for example, 60 to 300 ° C, more preferably 80 to 200 ° C.
加圧は、透明樹脂接着剤が完全に硬化する前に行うのが好ましく、第一基板１８と第二基板２０との接合直後に又は接合と同時に行われるのがより好ましい。 The pressurization is preferably performed before the transparent resin adhesive is completely cured, and more preferably is performed immediately after the first substrate 18 and the second substrate 20 are bonded or simultaneously with the bonding.
（５）積層体
上記のようにして作製された積層体１０は、図１に示されるように、第一基板１８と、第二基板２０と、透明導電接着層１２とを備える。第二基板２０は、第一基板１８と対向して設けられる。透明導電接着層１２は、第一基板１８及び第二基板２０との間に介在し、上記透明導電性接着剤で構成される。そして、透明導電接着層１２の厚さが導電性球状粒子１４の１個相当の高さに等しい。かかる積層体によれば透明導電接着層１２の厚さ方向に１個の導電性球状粒子１４で第一基板１８と第二基板２０との間の導通を取ることが可能となるため、少ない導電性球状粒子１４の添加量でも、透明導電接着層１２の厚さ方向に十分に高い導電性を確保することができる。こうして高い導電性と透光性を両立した基板接合がなされた積層体を得ることができる。
(5) Laminated body The laminated body 10 produced as mentioned above is equipped with the 1st board | substrate 18, the 2nd board | substrate 20, and the transparent conductive contact bonding layer 12, as FIG. 1 shows. The second substrate 20 is provided to face the first substrate 18. The transparent conductive adhesive layer 12 is interposed between the first substrate 18 and the second substrate 20 and is composed of the transparent conductive adhesive. The thickness of the transparent conductive adhesive layer 12 is equal to the height corresponding to one conductive spherical particle 14. According to such a laminated body, it becomes possible to establish conduction between the first substrate 18 and the second substrate 20 with one conductive spherical particle 14 in the thickness direction of the transparent conductive adhesive layer 12, and therefore, less conductive Even with the addition amount of the conductive spherical particles 14, sufficiently high conductivity can be ensured in the thickness direction of the transparent conductive adhesive layer 12. In this way, it is possible to obtain a laminate in which substrate bonding that achieves both high conductivity and translucency is achieved.
本発明を以下の例によってさらに具体的に説明する。 The present invention is more specifically described by the following examples.
例１
（１）透明導電性接着剤の調製
導電性球状粒子として、市販のＡｕ被覆樹脂粒子（ミクロパールＡＵ、積水化学工業株式会社製、粒径カタログ値：６μｍ）を用意した。この粒子の体積基準Ｄ１０粒径、Ｄ５０粒径及びＤ９０粒径をレーザー回折・散乱式粒度分析計（Ｍｉｃｒｏｔｒａｃ ＭＴ３３００ ＥＸＩＩ、日機装株式会社製）にて測定した。得られた結果を表１に示す。この導電性球状粒子０．４ｇと市販の透明樹脂接着剤（ＳＣＲ−１０１６Ａ／Ｂ、信越シリコーン製、Ａ剤とＢ剤を１対１で混合）９．６ｇを自転・公転ミキサー（あわとり錬太郎、株式会社シンキー製）にて混合した。得られた混合物を、脱泡を目的として、真空中で５分間保持した。こうして透明導電性接着剤を得た。
Example 1
(1) Preparation of transparent conductive adhesive Commercially available Au-coated resin particles (Micropearl AU, manufactured by Sekisui Chemical Co., Ltd., particle size catalog value: 6 μm) were prepared as conductive spherical particles. The volume-based D10 particle size, D50 particle size, and D90 particle size of the particles were measured with a laser diffraction / scattering particle size analyzer (Microtrac MT3300 EXII, manufactured by Nikkiso Co., Ltd.). The obtained results are shown in Table 1. 0.4 g of this conductive spherical particle and 9.6 g of a commercially available transparent resin adhesive (SCR-1016A / B, manufactured by Shin-Etsu Silicone, A and B mixed in a one-to-one relationship) 9.6 g Taro, manufactured by Shinky Corporation). The resulting mixture was held in a vacuum for 5 minutes for defoaming purposes. A transparent conductive adhesive was thus obtained.
（２）透光性評価用積層体試料の作製
ガラス基板（スライドガラス、松浪硝子工業株式会社製、１０ｍｍ×１０ｍｍ×厚さ１ｍｍ）の上に上記透明導電性接着剤０．１ｇを滴下し、その上に同様のガラス基板を気泡が入らないように注意しながら載置した。得られたガラス基板の積層体をホットプレート付きのプレス機を用い、加熱しながら圧力２００ｋｇｆ／ｃｍ２にてプレスして接着剤を硬化させた。この加熱は、まず１００℃で１時間保持し、続けて１５０℃で５時間保持することにより行った。得られた透光性評価用積層体試料の断面（研磨面）をＳＥＭで観察したところ、図２に示されるＳＥＭ像が得られた。このＳＥＭ像から、透明導電接着層の厚さ方向には導電性粒子が１つのみ存在するとともに、導電性球状粒子がやや潰れていることが確認された。
(2) Preparation of a laminate sample for translucency evaluation 0.1 g of the transparent conductive adhesive is dropped on a glass substrate (slide glass, Matsunami Glass Industrial Co., Ltd., 10 mm × 10 mm × thickness 1 mm), A similar glass substrate was placed thereon with care not to allow bubbles to enter. The obtained laminate of glass substrates was pressed at a pressure of 200 kgf / cm 2 while being heated using a press machine with a hot plate to cure the adhesive. This heating was performed by first holding at 100 ° C. for 1 hour and then holding at 150 ° C. for 5 hours. When the cross section (polished surface) of the obtained laminate sample for translucency evaluation was observed with SEM, the SEM image shown in FIG. 2 was obtained. From this SEM image, it was confirmed that only one conductive particle was present in the thickness direction of the transparent conductive adhesive layer, and the conductive spherical particles were slightly crushed.
（３）透光性の評価
透光性評価用積層体試料に対して、分光光度計（Ｌａｍｂｄａ ９００、Ｐｅｒｋｉｎ Ｅｌｍｅｒ製）を用い、波長３８０ｎｍ〜８００ｎｍにて全光線透過率を測定し、平均透過率を求めた。また、導電性球状粒子を添加せずにガラス基板２枚を上記透明樹脂接着剤のみで接合して参照用積層体試料を作製し、上記同様にして平均全光線透過率を求めた。透光性評価用積層体試料での平均全光線透過率をＡ（％）とし、参照用積層体試料での平均全光線透過率をＢ（％）として、（Ａ／Ｂ）×１００（％）により算出される値を、透明導電性接着剤の透光性の指標とした。
(3) Evaluation of translucency For a laminate sample for translucency evaluation, a spectrophotometer (Lambda 900, manufactured by Perkin Elmer) was used to measure the total light transmittance at a wavelength of 380 nm to 800 nm, and the average transmittance. The rate was determined. Further, two glass substrates were joined with only the transparent resin adhesive without adding the conductive spherical particles to prepare a reference laminate sample, and the average total light transmittance was determined in the same manner as described above. (A / B) × 100 (%) where A (%) is the average total light transmittance in the laminate sample for translucency evaluation, and B (%) is the average total light transmittance in the reference laminate sample. ) Was used as an index of translucency of the transparent conductive adhesive.
（４）導電性評価用試料の作製
粒径１μｍのダイヤモンドスラリーを用いて表面を平滑に研磨した銅基板（２０ｍｍ×２０ｍｍ×厚さ１ｍｍ）を用意した。また、同様にして鏡面をもたらすように研磨した銅線埋設基板（１０ｍｍ×１０ｍｍ×厚さ１ｍｍ）を用意した。図３Ａ及び３Ｂに示されるように、この銅線埋設基板１００は、エポキシ系樹脂基板１０２と、この基板１０２の格子点状に離間された位置に、厚さ方向に埋設された直径１００μｍの銅線１０４とで構成されるものである。銅線１０４同士の間隔は４００μｍである。この銅線埋設基板１００を上記銅基板１０６と上記透明導電性接着剤１０８を用いて接合した。こうして得られた積層体試料に対し、図４に示されるようにプローブ１１０を銅線１０４に当て、格子点状の各測定位置における透明導電性接着剤の抵抗値を測定した。測定された抵抗値から、別途測定した接触抵抗値を差し引くことで、導電性接着剤のみの抵抗とした。この接触抵抗値ＲｃはＲｃ＝（Ｒ１＋Ｒ２）／２（式中、Ｒ１は銅線埋設基板１００の同一の銅線１０４上に両プローブ１１０を接触させた時に測定される抵抗値であり、Ｒ２は銅基板１０６上に両プローブ１１０を接触させた時に測定される抵抗値である）により算出される値である。銅線埋設基板１００上のプローブ１１０の位置として、隣接する銅線９点（縦３点×横３点）を選択し、各点において抵抗値を測定した。得られた抵抗値に銅線の面積７８５０μｍ２を乗じ、接合抵抗値を算出し、その平均値及び標準偏差を求めた。こうして導電性の面内均一性を評価した。
(4) Preparation of Sample for Conductivity Evaluation A copper substrate (20 mm × 20 mm × thickness 1 mm) whose surface was polished smoothly using a diamond slurry having a particle diameter of 1 μm was prepared. Similarly, a copper wire embedded substrate (10 mm × 10 mm × thickness 1 mm) was prepared so as to provide a mirror surface. As shown in FIGS. 3A and 3B, this copper wire embedded substrate 100 is composed of an epoxy resin substrate 102 and a copper having a diameter of 100 μm embedded in the thickness direction at positions spaced apart by lattice points of the substrate 102. And the line 104. The interval between the copper wires 104 is 400 μm. The copper wire embedded substrate 100 was bonded to the copper substrate 106 using the transparent conductive adhesive 108. With respect to the laminate sample thus obtained, the probe 110 was applied to the copper wire 104 as shown in FIG. 4, and the resistance value of the transparent conductive adhesive at each of the lattice point measurement positions was measured. By subtracting the separately measured contact resistance value from the measured resistance value, the resistance of only the conductive adhesive was obtained. This contact resistance value R c is R c = (R 1 + R 2 ) / 2 (where R 1 is a resistance measured when both probes 110 are brought into contact with the same copper wire 104 of the copper wire embedded substrate 100). R 2 is a value calculated by the following equation: R 2 is a resistance value measured when both probes 110 are brought into contact with the copper substrate 106. Nine adjacent copper wires (3 vertical points × 3 horizontal points) were selected as the positions of the probes 110 on the copper wire embedded substrate 100, and the resistance value was measured at each point. The obtained resistance value was multiplied by the copper wire area of 7850 μm 2 to calculate the junction resistance value, and the average value and the standard deviation were obtained. Thus, the in-plane uniformity of conductivity was evaluated.
例２
導電性球状粒子として、別の市販の導電性球状粒子（Ａｕ被覆樹脂粒子、ミクロパールＡＵ、積水化学工業株式会社製、粒径カタログ値：３μｍ、粒度分布は表１に示される）を用いたこと以外は例１と同様にして、透明導電性接着剤を調製するとともに、透光性及び導電性を評価した。
Example 2
As the conductive spherical particles, another commercially available conductive spherical particles (Au coated resin particles, Micropearl AU, manufactured by Sekisui Chemical Co., Ltd., particle size catalog value: 3 μm, particle size distribution is shown in Table 1) were used. A transparent conductive adhesive was prepared in the same manner as in Example 1 except that the translucency and conductivity were evaluated.
例３
導電性球状粒子として、別の市販の導電性球状粒子（Ａｕ被覆樹脂粒子、ミクロパールＡＵ、積水化学工業株式会社製、粒径カタログ値：１０μｍ、粒度分布は表１に示される）を用いたこと以外は例１と同様にして、透明導電性接着剤を調製するとともに、透光性及び導電性を評価した。
Example 3
As the conductive spherical particles, another commercially available conductive spherical particles (Au coated resin particles, Micropearl AU, manufactured by Sekisui Chemical Co., Ltd., particle size catalog value: 10 μm, particle size distribution is shown in Table 1) were used. A transparent conductive adhesive was prepared in the same manner as in Example 1 except that the translucency and conductivity were evaluated.
例４
導電性球状粒子の添加量を０．１ｇとし、透明樹脂接着剤の添加量を９．９ｇとしたこと以外は例１と同様にして、透明導電性接着剤を調製するとともに、透光性及び導電性を評価した。
Example 4
A transparent conductive adhesive was prepared in the same manner as in Example 1 except that the addition amount of the conductive spherical particles was 0.1 g and the addition amount of the transparent resin adhesive was 9.9 g. Conductivity was evaluated.
例５
導電性球状粒子の添加量を２ｇ、透明樹脂接着剤の添加量を８ｇとしたこと以外は例１と同様にして、透明導電性接着剤を調製するとともに、透光性及び導電性を評価した。
Example 5
A transparent conductive adhesive was prepared and the translucency and conductivity were evaluated in the same manner as in Example 1 except that the addition amount of the conductive spherical particles was 2 g and the addition amount of the transparent resin adhesive was 8 g. .
例６
プレス時の圧力を５ｋｇｆ／ｃｍ２としたこと以外は例１と同様にして、透明導電性接着剤を調製するとともに、透光性及び導電性を評価した。
Example 6
A transparent conductive adhesive was prepared and the translucency and conductivity were evaluated in the same manner as in Example 1 except that the pressure during pressing was 5 kgf / cm 2 .
例７
導電性球状粒子として、別の市販の導電性球状粒子（Ａｇ被覆樹脂粒子、三菱マテリアル電子化成製、銀被覆粉、粒径カタログ値：２μｍ）を用いたこと以外は例１と同様にして、透明導電性接着剤を調製するとともに、透光性及び導電性を評価した。
Example 7
Except that another commercially available conductive spherical particle (Ag-coated resin particle, manufactured by Mitsubishi Materials Electronic Chemicals, silver-coated powder, particle size catalog value: 2 μm) was used as the conductive spherical particle, While preparing the transparent conductive adhesive, the translucency and electroconductivity were evaluated.
例８（比較）
導電性球状粒子の代わりに、銀ナノワイヤ（断面径３０ｎｍ×長さ２０μｍ）を用いた以外は例１と同様にして、透明導電性接着剤を調製するとともに、透光性及び導電性を評価した。本例においては、透光性は高いが、導電性が不十分であるとともに、接合抵抗のバラツキ（標準偏差）も大きかった。
Example 8 (Comparison)
A transparent conductive adhesive was prepared in the same manner as in Example 1 except that silver nanowires (cross-sectional diameter 30 nm × length 20 μm) were used in place of the conductive spherical particles, and the translucency and conductivity were evaluated. . In this example, the translucency is high, but the conductivity is insufficient, and the variation (standard deviation) in the junction resistance is large.
結果
例１〜９の測定結果は以下の表１に示されるとおりであった。
The measurement results of Result Examples 1 to 9 were as shown in Table 1 below.
１０ 積層体
１２ 透明導電接着層
１４ 導電性球状粒子
１６ 透明樹脂接着剤
１８ 第一基板
２０ 第二基板
１００ 銅線埋設基板
１０２ エポキシ系樹脂基板
１０４ 銅線
１０６ 銅基板
１０８ 透明導電性接着剤
１１０ プローブ
DESCRIPTION OF SYMBOLS 10 Laminated body 12 Transparent conductive adhesive layer 14 Conductive spherical particle 16 Transparent resin adhesive 18 1st board | substrate 20 2nd board | substrate 100 Copper wire embedding board | substrate 102 Epoxy-type resin board | substrate 104 Copper wire 106 Copper board | substrate 108 Transparent conductive adhesive 110 Probe
Claims (14)
前記導電性球状粒子が、体積基準Ｄ９０粒径の体積基準Ｄ１０粒径に対する比であるＤ９０／Ｄ１０が３．０以下である粒度分布を有する、透明導電性接着剤。 Including 100 parts by weight of a transparent resin adhesive and 0.5 to 30 parts by weight of conductive spherical particles,
A transparent conductive adhesive, wherein the conductive spherical particles have a particle size distribution in which D90 / D10, which is a ratio of volume-based D90 particle size to volume-based D10 particle size, is 3.0 or less.
前記第一基板と対向して設けられる第二基板と、
前記第一基板及び前記第二基板との間に介在し、請求項１〜４のいずれか一項に記載の透明導電性接着剤で構成される透明導電接着層と、
を備え、前記透明導電接着層の厚さが前記導電性球状粒子１個相当の高さに等しい、積層体。 A first substrate;
A second substrate provided facing the first substrate;
A transparent conductive adhesive layer interposed between the first substrate and the second substrate, the transparent conductive adhesive layer comprising the transparent conductive adhesive according to any one of claims 1 to 4,
And the thickness of the transparent conductive adhesive layer is equal to the height corresponding to one conductive spherical particle.
前記第一基板及び前記第二基板の少なくともいずれか一方の表面に請求項１〜８のいずれか一項に記載の透明導電性接着剤を塗布する工程と、
前記第一基板と前記第二基板とを前記透明導電性接着剤を挟むように積層して積層体とする工程と、
前記積層体を加圧して、厚さが前記導電性球状粒子１個相当の高さに等しい、前記透明導電性接着剤で構成される透明導電接着層を形成する工程と
を含む、基板の接合方法。 Preparing a first substrate and a second substrate;
Applying the transparent conductive adhesive according to any one of claims 1 to 8 on at least one surface of the first substrate and the second substrate;
A step of laminating the first substrate and the second substrate so as to sandwich the transparent conductive adhesive;
Pressurizing the laminate to form a transparent conductive adhesive layer composed of the transparent conductive adhesive, the thickness of which is equal to the height corresponding to one conductive spherical particle. Method.
The method according to claim 9, wherein the pressurization is performed while heating.
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