JPWO2017090623A1 - 整合型電磁波吸収体 - Google Patents
整合型電磁波吸収体 Download PDFInfo
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- JPWO2017090623A1 JPWO2017090623A1 JP2017510915A JP2017510915A JPWO2017090623A1 JP WO2017090623 A1 JPWO2017090623 A1 JP WO2017090623A1 JP 2017510915 A JP2017510915 A JP 2017510915A JP 2017510915 A JP2017510915 A JP 2017510915A JP WO2017090623 A1 JPWO2017090623 A1 JP WO2017090623A1
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- electromagnetic wave
- component
- resin composition
- wave absorber
- composition layer
- Prior art date
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- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000003505 polymerization initiator Substances 0.000 claims abstract description 7
- -1 ester acrylate Chemical class 0.000 claims description 43
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 26
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 18
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims description 8
- 229920001577 copolymer Polymers 0.000 claims description 5
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 5
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- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims description 4
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- 239000000347 magnesium hydroxide Substances 0.000 claims description 3
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- UMHKOAYRTRADAT-UHFFFAOYSA-N [hydroxy(octoxy)phosphoryl] octyl hydrogen phosphate Chemical compound CCCCCCCCOP(O)(=O)OP(O)(=O)OCCCCCCCC UMHKOAYRTRADAT-UHFFFAOYSA-N 0.000 description 3
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- 125000000217 alkyl group Chemical group 0.000 description 2
- ULDHMXUKGWMISQ-UHFFFAOYSA-N carvone Chemical compound CC(=C)C1CC=C(C)C(=O)C1 ULDHMXUKGWMISQ-UHFFFAOYSA-N 0.000 description 2
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- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 2
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- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
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- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
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- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 2
- WRXCBRHBHGNNQA-UHFFFAOYSA-N (2,4-dichlorobenzoyl) 2,4-dichlorobenzenecarboperoxoate Chemical compound ClC1=CC(Cl)=CC=C1C(=O)OOC(=O)C1=CC=C(Cl)C=C1Cl WRXCBRHBHGNNQA-UHFFFAOYSA-N 0.000 description 1
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 1
- KDGNCLDCOVTOCS-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy propan-2-yl carbonate Chemical compound CC(C)OC(=O)OOC(C)(C)C KDGNCLDCOVTOCS-UHFFFAOYSA-N 0.000 description 1
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- NLBJAOHLJABDAU-UHFFFAOYSA-N (3-methylbenzoyl) 3-methylbenzenecarboperoxoate Chemical compound CC1=CC=CC(C(=O)OOC(=O)C=2C=C(C)C=CC=2)=C1 NLBJAOHLJABDAU-UHFFFAOYSA-N 0.000 description 1
- NOBYOEQUFMGXBP-UHFFFAOYSA-N (4-tert-butylcyclohexyl) (4-tert-butylcyclohexyl)oxycarbonyloxy carbonate Chemical compound C1CC(C(C)(C)C)CCC1OC(=O)OOC(=O)OC1CCC(C(C)(C)C)CC1 NOBYOEQUFMGXBP-UHFFFAOYSA-N 0.000 description 1
- RIPYNJLMMFGZSX-UHFFFAOYSA-N (5-benzoylperoxy-2,5-dimethylhexan-2-yl) benzenecarboperoxoate Chemical compound C=1C=CC=CC=1C(=O)OOC(C)(C)CCC(C)(C)OOC(=O)C1=CC=CC=C1 RIPYNJLMMFGZSX-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
≪整合型電磁波吸収体≫
本発明の整合型電磁波吸収体は、例えば、アルミ箔等の電磁波反射層の片面に、所定の複素比誘電率を持った樹脂組成物層(電磁波吸収層)を、対象周波数に応じて所定の厚みに設けたものであり、樹脂組成物層表面で反射した電磁波と、積層された電磁波反射層と樹脂組成物層の界面で反射されて戻ってくる電磁波とが打ち消しあうよう、それらの振幅と位相をコントロールして設計されたものである。電磁波が垂直に入射する場合において、無反射となる場合の樹脂組成物層(電磁波吸収層)の複素比誘電率の実部(εr)と虚部(εi)の関係は、d/λ(d:樹脂組成物層の厚み、λ:電磁波の波長)に応じて変化し、図1に示す無反射曲線で表される。なお、本発明の整合型電磁波吸収体は、図2に示されるように、電磁波反射層と樹脂組成物層とが直接積層されたものであってもよいし、図3に示されるように、電磁波反射層と樹脂組成物層とがその他の層(例えば、接着剤層)を介して積層されたものであってもよい(この場合、その他の層を熱接着や電磁波吸収特性に影響を与えない程度の薄い層とするか、或いはその他の層の厚みを考慮して電磁波反射層と樹脂組成物層とを設計すればよい)。
本発明に係る電磁波反射層としては、アルミニウム、銅、鉄やステンレス等の金属板、金属箔や、高分子フィルムに真空蒸着やめっき等で上記金属の薄膜を形成したもの、上記金属や炭素繊維等の導電材の織布や不織布で樹脂等を補強したものなどの他、電磁波を反射可能な材料であれば上記以外のものであっても用いることができる。
本発明に係る樹脂組成物層とは、(A)成分:アクリル系重合性樹脂と(B)成分:重合開始剤(B)成分から成る樹脂組成物の硬化物中に、(C)成分:アスペクト比が5以上のフィラーと(D)成分:アスペクト比が5未満のフィラーとが分散固定された構成を有するものを指す。
(A)成分:アクリル系重合性樹脂としては、ビニル基を有するエポキシアクリレート、ウレタンアクリレート、エステルアクリレート、共重合アクリレート、ブタジエンアクリレート、シリコンアクリレート、及び/又はアミノ樹脂アクリレートを用いることが好ましく、より好ましくは、繰り返し単位が2〜20程度のアクリル系オリゴマーであり、末端に2〜6個のビニル基を持っているエポキシアクリレート、ウレタンアクリレート、ポリエステルアクリレート、共重合アクリレート、ブタジエンアクリレート、シリコンアクリレート、及び、アミノ樹脂アクリレート等が挙げられるが、中でも3官能以下のものが樹脂の硬化収縮を抑えやすい点において好ましい。また、これらは単独または2種類以上組み合わせて用いることが可能であり、中でも重量平均分子量が500〜10,000、粘度が3,000〜500,000mPa・s/25℃のウレタンアクリレートが無溶剤系での塗工が容易に行える点においてより好ましい。樹脂組成物層を形成する際に、溶剤を使用しないことで残留溶剤の揮発による樹脂組成物層の寸法変化を抑制しやすくなる。尚、重量平均分子量は、JIS K7252に準拠して、ゲルパーメーションクロマトグラフィー(日本分光株式会社製)を用いて測定される値であり、粘度はE型粘度計を用いて測定される値である。
本発明に係る(B)成分:重合開始剤としては、公知のものを使用可能であるが、有機過酸化物が好ましい。有機過酸化物は、常温から300℃程度の温度範囲において、無溶剤でアクリル系樹脂組成物を重合硬化させる温度を自由に設定できる点において好適である。上記有機過酸化物としては、メチルエチルケトンパーオキサイド、シクロヘキサンパーオキサイド、3,3,5−トリメチルシクロヘキサノンパーオキサイド、メチルシクロヘキサノンパーオキサイド、メチルアセトアセテートパーオキサイド、アセチルアセトンパーオキサイド、1,1−ビス(t−ブチルパーオキシ)−3,3,5トリメチルヘキサン、1,1−ビス(t−ブチルパーオキシ)−シクロヘキサン、2,2−ビス(t−ブチルパーオキシ)オクタン、n−ブチル−4,4−ビス(t−ブチルパーオキシ)バレート、2,2−ビス(t−ブチルパーオキシ)ブタン、t−ブチルハイドロパーオキサイド、クメンハイドロパーオキサイド、ジ−イソプロピルベンゼンハイドロパーオキサイド、p−メンタンハイドロパーオキサイド、2,5−ジメチルヘキサン−2,5−ジハイドロパーオキサイド、1,1,3,3−テトラメチルブチルハイドロパーオキサイド、1,1,3,3−テトラメチルブチルパーオキシ−2−エチルヘキサネート、ジ−t−ブチルパーオキサイド、t−ブチルクミルパーオキサイド、ジ−クミルパーオキサイド、α,α’−ビス(t−ブチルパーオキシ−m−イソプロピル)ベンゼン、2,5−ジメチル−2,5−ジ(t−ブチルパーオキシ)ヘキサン、2,5−ジメチル−2,5−ジ(t−ブチルパーオキシ)ヘキシン、アセチルパーオキサイド、イソブチルパーオキサイド、オクタノイルパーオキサイド、デカノイルパーオキサイド、ベンゾイルパーオキサイド、ラウロイルパーオキサイド、ジラウロイルパーオキサイド、3,5,5−トリメチルヘキサノイルパーオキサイド、スクシニックアシッドパーオキサイド、2,4−ジクロロベンゾイルパーオキサイド、m−トルオイルパーオキサイド、ジ−イソプロピルパーオキシジカーボネート、ジ−2−エチルヘキシルパーオキシジカーボネート、ジ−n−プロピルパーオキシジカーボネート、ビス−(4−t−ブチルシクロヘキシル)パーオキシジカーボネート、ジ−ミリスティルパーオキシジカーボネート、ジ−2−エトキシエチルパーオキシジカーボネート、ジ−メトキシイソプロピルパーオキシジカーボネート、ジ(3−メチル−3−メトキシブチル)パーオキシジカーボネート、ジ−アリルパーオキシジカーボネート、t−ブチルパーオキシアセテート、t−ブチルパーオキシイソブチレート、t−ブチルパーオキシピバレート、t−ブチルパーオキシネオデカネート、クミルパーオキシネオデカネート、t−ブチルパーオキシ−2−エチルヘキサネート、t−ブチルパーオキシ−3,5,5−トリメチルヘキサネート、t−ブチルパーオキシラウレート、t−ブチルパーオキシベンゾエート、ジ−t−ブチルパーオキシイソフタレート、2,5−ジメチル−2,5−ジ(ベンゾイルパーオキシ)ヘキサン、t−ブチルパーオキシマレイン酸、t−ブチルパーオキシイソプロピルカーボネート、クミルパーオキシオクテート、t−ヘキシルパーオキシネオデカネート、t−ヘキシルパーオキシピバレート、t−ブチルパーオキシネオヘキサネート、アセチルシクロヘキシルスルフォニルパーオキサイド、t−ブチルパーオキシアリルカーボネート等が挙げられ、これらは単独または2種類以上組み合わせて使用することが出来る。
更には、(A)成分と(B)成分を合わせた樹脂組成物中の(A)成分/(B)成分で表される質量比は、10〜2,000であることが好ましく、20〜1,000であることがより好ましく、33〜200であることがさらに好ましい。質量比が、2000を超える比率であると、硬化反応が不十分となり、長期に渡って高温状態におかれた場合、残留未硬化成分の重量減少により、樹脂組成物層に収縮が生じ、電磁波吸収性能が所望の周波数帯からズレを生ずる恐れがある。また、10未満であると、樹脂組成物層の硬化収縮率が大きくなり電磁波吸収体を生産する際に層厚の制御が難しくなる恐れがある。
また、最も理想的な電磁波吸収性能を得るための樹脂組成物中の[(A)成分+(B)成分]の含有量は、吸収目的の電磁波の周波数とこれに応じた複素比誘電率により任意に決定すればよい。
本発明に係る(C)成分のフィラーのアスペクト比は5以上であり、更に好ましくは12以上である。アスペクト比の上限は特に無いが、樹脂組成物層の表面の平滑性を乱す程、長くなりすぎない程度に設定すればよい(例えば、アスペクト比1000以下)。アスペクト比が5以上のフィラーとしては、酸化チタン繊維、ガラス繊維、ロックウール、炭素繊維、アルミナ繊維、ウォラストナイトやチタン酸カリウム繊維等の無機繊維等が挙げられる他、天然繊維である綿、麻、絹、合成繊維であるアラミド、ポリアミド、ポリエステル、ポリエチレン、アクリル、レーヨン等の有機繊維等が挙げられる。また、これら以外であっても、樹脂組成物層中で骨材的な働きを示し、樹脂組成物層の膨張抑制或いは収縮抑制に寄与できるものであれば、いずれのものも使用することができるが、導電性フィラーであることが好適である。(C)成分をアスペクト比5以上とすることで、当該フィラーが樹脂組成物層の膨張や収縮等を防止する所謂骨材的な働きを顕著に示し、その結果樹脂組成物層の寸法安定性に寄与できたもの推察される。
本発明に係る(D)成分のフィラーは、アスペクト比が5未満であり、更に好ましくは2以下である。また、アスペクト比が5未満のフィラーは、酸化物、水酸化物、炭酸塩、硫酸塩、珪酸塩等の無機粉末が好ましい。これらは単独または2種類以上組み合わせて用いることが可能であり、中でも難燃性を付与できる点で水酸化物、取り分け、水酸化アルミニウム、水酸化マグネシウムが好ましい。なお、(D)成分は、(C)成分とは異種の材料{例えば、(C)成分が導電性酸化チタンの場合には、導電性酸化チタン以外}である。(D)成分の平均粒径は0.01〜10μmであることが好ましく、更に好ましくは、0.05〜5μmである。平均粒径が0.01μmを下回ると樹脂組成物層中への均一分散性が悪化する恐れがあり、10μmを超えると樹脂組成物層の分子鎖に入り込み難くなるためと推察されるが、スペーサー的効果が低下する傾向がある。このような長軸、短軸を顕著に有さないフィラーを用いることで、特に(A)成分の分子鎖中にフィラーがスペーサーとして存在しやすくなり、樹脂組成物層が熱に曝された場合であっても寸法変化を抑えやすくなるものと推察される。ここで、(D)成分の「平均径」、「平均長」、「アスペクト比」の値は、(D)成分をSEM観察し、少なくとも100個の粒子を観察測定し、その平均値から求めた値である。すなわち、平均径と平均長は100粒子の測定値平均、アスペクト比については、100粒子の長軸と短軸の長さを測定し、それぞれの平均値の比から求めた値である。また、平均粒径は、同じく(D)成分をSEM観察し、少なくとも100個の粒子を観察測定し、その投影面積平均の円相当径をいう。
また、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は、0.1〜0.5であることが好ましく、更に好ましくは0.1〜0.25である。体積比が0.1より小さいと(C)成分の骨材的効果及び、(D)成分のスペーサー的効果が発揮されないものと推察され、樹脂組成物層の寸法変化が生じる恐れがあり、0.5よりも大きいと、骨材的効果及びスペーサー的効果は発揮されるものの、硬化した樹脂組成物層の可撓性が低下し、狭小箇所や複雑形状への対応が出来難くなる恐れがある。
(C)成分と(D)成分の体積比は、吸収したい周波数帯によって任意に決定すれば良く、特に(C)成分は吸収周波数帯を決定する上で重要な役割を果たす。樹脂組成物層の寸法安定性に及ぼす影響としては、(C)成分と(D)成分双方を有することが必要であるが、その体積比に関しては、任意に設定することが出来る。すなわち、(C)成分リッチであれば骨材的効果が優位となり、(D)成分リッチであればスペーサー的効果が優位に働き、本発明の目的を達成することが出来るものと推察される。
また、樹脂組成物には、電磁波吸収効果を損なわない範囲で、必要に応じて、難燃剤、難燃助剤、充填剤、離型剤、表面処理剤、粘度調節剤、可塑剤、抗菌剤、防黴剤、レベリング剤、消泡剤、着色剤、安定剤、カップリング剤、分散剤、滑剤、酸化防止材、紫外線吸収剤、光安定剤、帯電防止剤、反応性希釈剤等の任意成分(以下、総じて、整合型電磁波吸収体の任意成分という)を添加してもよい。
本発明の整合型電磁波吸収体は、電磁波反射層に塗料(樹脂組成物)を直接塗工することにより得ることも出来るし、PETフィルム等に塗工した樹脂組成物を硬化後、接着剤等を介して電磁波反射層に貼り付ける方法等によって得ることも出来る。接着剤等により樹脂組成物層と電磁波吸収層を接着する場合には、接着剤層の厚みを考慮して吸収周波数設計をすれば良い。
(A)成分:重量平均分子量2,500、粘度6,500mPa・s/25℃のポリウレタンアクリレート(商品名:「ビームセット505A−6」、荒川化学工業社製)100質量部、(B)成分:1,1,3,3−テトラメチルブチル パーオキシ−2−エチルヘキサネート(商品名:「パーオクタO」:日油社製)1.0質量部、(C)成分:平均径0.5μm、平均長10.0μmの導電性針状酸化チタン(商品名:「FT−4000」石原産業社製)22.8質量部、(D)成分:平均粒径1.2μm、アスペクト比1.7の微粒水酸化アルミニウム(商品名:BF013日本軽金属社製)54.6質量部を加え、公知の方法で攪拌して、樹脂組成物層を形成するための塗料を得た。
(C)成分の添加量を18.8質量部、(D)成分の添加量を40.0質量部に変更したこと以外は実施例1と同様にして、樹脂組成物層厚515μm、60GHz複素比誘電率の実数項が6.3、虚数項が3.1の実施例2のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.2であった。
(C)成分の添加量を23.3質量部、(D)成分の添加量を31.5質量部に変更したこと以外は実施例1と同様にして、樹脂組成物層厚370μm、79GHz複素比誘電率の実数項が7.0、虚数項が3.2の実施例3のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.18であった。
(C)成分を、平均径0.4μm、平均長5.0μmの導電性針状酸化チタン(商品名:「FT−3000」石原産業社製)19.2質量部に変更したこと以外は、実施例1と同様にして、樹脂組成物層厚365μm、76.5GHz複素比誘電率の実数項が7.6、虚数項が3.4の実施例4のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.24であった。
(C)成分を、平均径0.15μm、平均長2.0μmの導電性針状酸化チタン(商品名:「FT−1000」石原産業社製)23.6質量部に変更したこと以外は、実施例1と同様にして、樹脂組成物層厚345μm、76.5GHz複素比誘電率の実数項が8.5、虚数項が3.6の実施例5のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.25であった。
(A)成分を、重量平均分子量2,600、粘度300,000mPa・s/25℃のポリウレタンアクリレート(商品名:「ビームセット504H」、荒川化学工業社製)に変更したこと以外は、実施例1と同様にして、樹脂組成物層厚380μm、76.5GHz複素比誘電率の実数項が7.0、虚数項が3.2の実施例6のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.25であった。
(B)成分を、ジラウロイル パーオキサイド(商品名:「パーロイルL」、日油社製)に変更したこと以外は、実施例1と同様にして、樹脂組成物層厚385μm、76.5GHz複素比誘電率の実数項が6.9、虚数項が3.2の実施例7のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)+(D)]/樹脂組成物層で表される体積比は0.25であった。
(A)成分の添加量を75質量部、(C)成分の添加量を25質量部に変更し、反応性希釈剤としてN−ビニルホルムアミドを25質量部添加したこと以外は、実施例1と同様にして、樹脂組成物層厚385μm、76.5GHz複素比誘電率の実数項が7.0、虚数項が3.2の実施例8のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.25であった。
(D)成分の添加量を15.0質量部に変更したこと以外は、実施例1と同様にして、樹脂組成物層厚312μm、76.5GHz複素比誘電率の実数項が7.1、虚数項が2.9の実施例9のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.12であった。
厚さ12μmのアルミ箔(電磁波反射層)に換えて、厚さ12μmの銅箔を電磁波反射層として用いたこと以外は、実施例1と同様にして、樹脂組成物層厚さ385μm、76.5GHz複素比誘電率の実数項が6.9、虚数項が3.2の実施例10のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.25であった。
(C)成分の導電性針状酸化チタンを添加しないこと以外は実施例1と同様にして、樹脂組成物層厚385μm、76.5GHz複素比誘電率の実数項が3.4、虚数項が0.0の比較例1のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.21であった。
(D)成分を添加しないこと以外は実施例1と同様にして、樹脂組成物層厚385μm、76.5GHz複素比誘電率の実数項が7.0、虚数項が3.2の比較例2のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.06であった。
(A)成分に換えて、塩素化ポリエチレン(塩素化PE)を用い、(B)成分を未添加としたこと以外は、実施例1と同様にして、樹脂組成物層厚380μm、76.5GHz複素比誘電率の実数項が7.0、虚数項が3.2の比較例3のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.25であった。
(C)成分を平均粒径0.25μm、アスペクト比1.6の導電性球状酸化チタン(商品名:「ET−500W」石原産業社製)に変えたこと以外は実施例1と同様にして、樹脂組成物層厚385μm、76.5GHz複素比誘電率の実数項が3.7、虚数項が0.0の比較例1のシート形状をなす整合型電磁波吸収体を得た。この時、[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.25であった。
表1に従う成分及び組成とした以外は、実施例1と同様にして、実施例11〜18及び比較例5に係る整合型電磁波吸収体を得た。尚、実施例11は、(D)成分を164質量部{したがって[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.46}である例であり;実施例12は、(D)成分を25質量部{したがって[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.16}である例であり;実施例13は、(D)成分を100質量部{したがって[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.36}である例であり;実施例14は、(C)成分としてカーボンファイバー(アスペクト比=10.9)を使用し、(C)成分を10質量部、(D)成分を62質量部とした例であり;実施例15は、(C)成分としてアスペクト比が10.6(径0.5μm、長さ5.3μm)を使用した例であり;実施例16は、(C)成分としてアスペクト比が7.2(径0.5μm、長さ3.6μm)を使用した例であり;実施例17は、(D)成分を218質量部{したがって[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.53}である例であり;実施例18は、(D)成分を7質量部{したがって[(C)成分+(D)成分]/樹脂組成物層で表される体積比は0.09}である例であり;比較例5は、(C)成分のアスペクト比が4.2(径0.5μm、長さ2.1μm)である例である。
得られた実施例1〜18及び比較例1〜5の整合型電磁波吸収体について、50〜110GHz周波数帯域における複素比誘電率、反射減衰量、高温長期耐熱信頼性、柔軟性の評価を以下の方法で実施した。その評価結果を表2に示す。
<複素比誘電率>
実施例1〜18及び比較例1〜5で作製した塗料を用いて、樹脂組成物層の層厚が各実施例、比較例に記載の厚さとなるように剥離性PET基材に塗工し、乾燥・硬化後剥離性PET基材から剥離して、各々の評価用樹脂組成物層を得た。次に、評価用樹脂組成物層を150mm長×150mm幅に断裁して、試験片とし、それぞれの試験片について、関東電子応用開発社製の「フリースペース型Sパラメータ測定装置」を用い、試験片を透過する50〜110GHz周波数帯域における電磁波をキーサイトテクノロジー社製の「PNAネットワークアナライザーN5225A」で測定することにより、実施例及び比較例の樹脂組成物層の複素比誘電率を算出した。
実施例1〜18及び比較例1〜5で得られたシート形状をなす整合型電磁波吸収体を150mm長×150mm幅に断裁して、試験片とし、50〜110GHz周波数帯域における電磁波の反射減衰量を測定した。測定には、関東電子応用開発社製の「フリースペース型Sパラメータ測定装置」を用い、キーサイトテクノロジー社製の「PNAネットワークアナライザーN5225A」で測定した。評価は、目的周波数での反射減衰量が20dB以上を合格「○」、20dB以下を不合格「×」と判定した。反射減推率が20dB以上であれば入射電磁波に対しての反射電磁波は100分の1以下であり、実用上十分な吸収性能と判断できる。
≪寸法安定性≫
実施例1〜18及び比較例2、3、5で得られたシート形状をなす整合型電磁波吸収体を100mm長×100mm幅に断裁し、試験片とした。この試験片について、高温長期耐熱信頼性加速試験(120℃で2,000時間)前後の試験片の厚さをマイクロメーターで測定した。評価は、厚さ変化が3%未満の場合を○、3%以上の場合を×とした。厚さの変化が3%を超えると吸収性能の低下及び吸収ピーク周波数のずれが生じ易い傾向がある。また、120℃、2,000時間の高温長期耐熱信頼性加速試験において、厚さ変化が3%未満であれば、例えば車載用途等においても充分な長期使用耐性が期待できる。尚、比較例1と4の整合型電磁波吸収体は、下記反射減衰量値が20dB未満であったため、本試験を割愛した。
[評価基準]
○:厚さ変化が3%未満。
×:厚さ変化が3%以上。
実施例1〜18及び比較例2、3、5で得られた整合型電磁波吸収体について、高温長期耐熱信頼性試験(120℃で2,000時間)後の反射減衰率を上記方法で測定した。目的周波数での反射減衰量が20dB以上を合格「○」、20dB未満を不合格「×」と判定した。
実施例1〜18及び比較例1〜5で得られたシート形状をなす整合型電磁波吸収体を200mm長×50mm幅に断裁して、試験片とし、図4に示すように5mmφの鉄製の丸棒に180°になるように巻き付け評価した。
表2に示すように、実施例1〜18の整合型電磁波吸収体は、いずれも反射減衰量が20dB以上(「○」)であり、目的周波数における電磁波吸収特性に優れたものであった。加えて、実施例1〜18の整合型電磁波吸収体は、高温耐熱信頼性試験後の寸法安定性、及び、反射減衰量が共に「○」であり、高温に長期間曝されたとしても寸法安定性が高く、GHz帯域の電磁波を効率よく吸収することが出来た。一方、アスペクト比が5以上のフィラーを有さない比較例1の整合型電磁波吸収体は、反射減衰量が0.8dBしかなく、目的GHz帯域の電磁波を効率良く吸収することが出来なかった。また、アスペクト比が5未満のフィラーを有さない比較例2の整合型電磁波吸収体は、反射減衰量は「○」であり、目的周波数における電磁波吸収特性に優れたものであったが、高温耐熱信頼性試験後の寸法安定性、及び、反射減衰量が共に「×」であり、高温に曝された場合に、樹脂組成物層に寸法変化を生じてしまい、目的GHz帯域の電磁波を効率良く吸収することが出来なかった。次に、(A)成分として、塩素化ポリエチレンを使用した比較例3の整合型電磁波吸収体は、反射減衰量が「○」であり、目的周波数における電磁波吸収特性に優れたものであったが、高温耐熱信頼性試験後の寸法安定性、及び、反射減衰量が共に「×」であり、高温に曝された場合に、樹脂組成物層に寸法変化を生じてしまい、目的GHz帯域の電磁波を効率良く吸収することが出来なかった。(C)成分としてアスペクト比が1.6の導電性球状酸化チタンを使用した比較例4の整合型電磁波吸収体は、反射減衰量が0.1dBしかなく、目的GHz帯域の電磁波を効率良く吸収することが出来なかった。
2・・・・・・・樹脂組成物層
3・・・・・・・アスペクト比5未満のフィラー
4・・・・・・・アスペクト比5以上のフィラー
5・・・・・・・接着剤層
Claims (6)
- 少なくとも樹脂組成物層と電磁波反射層から成る積層構造を有し、
該樹脂組成物層は、(A)成分:アクリル系重合性樹脂と(B)成分:重合開始剤とを有する樹脂組成物の硬化物中に、(C)成分:アスペクト比が5以上のフィラーと(D)成分:アスペクト比が5未満のフィラーとが分散固定されていることを特徴とする整合型電磁波吸収体。 - [前記(C)成分+前記(D)成分]/樹脂組成物層で表される体積比が、0.1〜0.5であることを特徴とする請求項1に記載の整合型電磁波吸収体。
- 前記(C)成分:アスペクト比が5以上のフィラーが導電性フィラー、
前記(D)成分:アスペクト比が5未満のフィラーが水酸化アルミニウム及び/又は水酸化マグネシウムであることを特徴とする請求項1または2に記載の整合型電磁波吸収体。 - 前記導電性フィラーが、導電性酸化チタンであり、且つ、平均長が0.5〜50μmであることを特徴とする請求項3に記載の整合型電磁波吸収体。
- 前記(A)成分:アクリル系重合性樹脂は、ビニル基を有するエポキシアクリレート、ウレタンアクリレート、エステルアクリレート、共重合アクリレート、ブタジエンアクリレート、シリコンアクリレート、アミノ樹脂アクリレートから選ばれるいずれか1種または2種以上を含むことを特徴とする請求項1乃至4いずれか一項に記載の整合型電磁波吸収体。
- 前記(B)成分:重合開始剤が、有機過酸化物であることを特徴とする請求項1乃至5いずれか一項に記載の整合型電磁波吸収体。
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