JPH071837B2 - 電磁波吸収材 - Google Patents

電磁波吸収材

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Publication number
JPH071837B2
JPH071837B2 JP16867388A JP16867388A JPH071837B2 JP H071837 B2 JPH071837 B2 JP H071837B2 JP 16867388 A JP16867388 A JP 16867388A JP 16867388 A JP16867388 A JP 16867388A JP H071837 B2 JPH071837 B2 JP H071837B2
Authority
JP
Japan
Prior art keywords
electromagnetic wave
fiber
wave absorber
resin
fibers
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
JP16867388A
Other languages
English (en)
Other versions
JPH01157598A (ja
Inventor
武民 山村
敏弘 石川
昌樹 渋谷
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ube Corp
Original Assignee
Ube Industries Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Ube Industries Ltd filed Critical Ube Industries Ltd
Priority to JP16867388A priority Critical patent/JPH071837B2/ja
Priority to EP88308106A priority patent/EP0306311B1/en
Priority to DE3889042T priority patent/DE3889042T2/de
Priority to CA 576414 priority patent/CA1330704C/en
Publication of JPH01157598A publication Critical patent/JPH01157598A/ja
Priority to US07/550,221 priority patent/US5094907A/en
Publication of JPH071837B2 publication Critical patent/JPH071837B2/ja
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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Description

【発明の詳細な説明】 （産業上の利用分野） 本発明は、高い強度及び弾性率、並びに優れた耐熱性を
有し、かつ特定周波数の電磁波を選択的に吸収する、構
造材料として使用可能な電磁波吸収材に関する。
（従来の技術） 電磁波吸収材は、マイクロ波加熱調理器、電波暗室など
の隙間におけるマイクロ波漏洩防止用としての用途を有
している。さらに、電磁波吸収材は、船舶、航空機等が
レーダーに捕捉されることを防止するためのレーダー波
吸収材としての用途をも有している。
電磁波吸収材についてはいくつかの提案がされている。
特公昭53-31275号公報には、樹脂にカーボンブラック及
び金属微細物を配合して形成した電磁波吸収材が開示さ
れている。この電磁波吸収材は、強度及び弾性率が低
く、構造材料としてはとうてい使用することができな
い。
特開昭57-66699号公報には、周波数10GHzにおける複素
比誘電率εが〔ε＝（８〜12）−ｊ（３〜５）〕の炭素
繊維と樹脂との複合材料からなる電磁波吸収材が開示さ
れている。
炭素繊維は、金属電導を示す繊維であるため、温度の上
昇につれて比抵抗が大きくなり、電磁波吸収特性が大幅
に低下する。電磁波吸収材には広い温度幅にわたって電
磁波吸収特性が変化しないことが要求され、この観点か
らすると、上記公開公報に記載の電磁波吸収材は実用上
満足し得るものではない。
特開昭62-267329号公報には、ケイ素、炭素、チタン又
はジルコニウム、及び酸素からなる非晶質あるいは微結
晶質の無機繊維とプラスチックスとからなる、無機繊維
強化プラスチック複合材料が記載されている。しかし、
この公報には、使用される無機繊維の比抵抗について
も、特定の比抵抗を有する無機繊維とプラスチックとの
複合材料が電磁波吸収材として使用されることに関して
も記載がない。
（問題点を解決するための技術的手段） 本発明の目的は、広い温度範囲にわたって電磁波吸収特
性が優れ、かつ構造材料として使用可能な高い強度及び
弾性率を有する電磁波吸収材を提供することにある。
本発明によれば、下記ｉ）、ii）及びiii）からなる群
から選択される無機質物質で構成され、10-2〜102Ω・c
m比抵抗を有する繊維とマトリックスとの複合材料から
なることを特徴とする電磁波吸収材が提供される。
ｉ） Si、Ｍ、Ｃ及びＯからなる非晶質物質。
ii） 結晶質物質の集合体であって、β−SiC、Ｃ及びM
C、並びにβ−SiCとMCとの固溶体及び／又はMC1-xから
構成され、各結晶質物質の粒径が500Å以下である結晶
質物質。
iii） 上記ｉ）の非晶質物質と上記ii）の結晶質物質
の集合体との混合物。
（上式中、ＭはTi又はZrを示し、ｘは０より大きく１未
満の数である。） 本発明において、繊維の構成成分である上記ii）の結晶
質物質は、非晶質のSiO2及びMO2を含むことができる。
本発明の電磁波吸収材に使用される繊維は、例えば特公
昭58-5286号公報、同60-20485号公報に記載の方法に従
って調製することができる。
まず、主として（Si-CH2）結合単位からなり、数平均分
子量が200〜10000のポリカルボシランとチタンアルコキ
シド又はジルコニウムアルコキシドとを不活性雰囲気下
に加熱反応させて、ポリカルボシランのケイ素原子の少
なくとも一部を上記アルコキシドのチタン又はジルコニ
ウムと酸素原子を介して結合させることにより、数平均
分子量が1000〜50000のポリチタノカルボシランあるい
はポリジルコノカルボシランを生成させ、ついで、これ
ら有機ケイ素重合体の紡糸原液を調製し紡糸し、紡糸繊
維を不融化し、最後に不融化繊維を真空中、不活性ガス
あるいは還元性ガス雰囲気中で1300〜1500℃で加熱処理
することによって上記繊維を調製することができる。加
熱処理温度を上記温度範囲で高めるにつれて得られる繊
維の比抵抗が低下する。
本発明の電磁波吸収材に使用される繊維の別の調製法と
して、特公昭60-1405号公報、同59-44403号公報に記載
の方法を採用することもできる。これら公報に記載の方
法は、数平均分子量500〜1000のポリカルボシランと数
平均分子量500〜1000のポリチタノカルボシランあるい
はポリジルコノカルボシランとを、有機溶媒中、不活性
ガス雰囲気下に加熱して、ポリカルボシラン中の少なく
とも一部のケイ素原子とポリチタノカルボシランあるい
はポリジルコノカルボシランのケイ素原子、チタン原子
あるいはジルコニウム原子と酸素を介して結合させるこ
とにより有機ケイ素重合体を調製し、ついでこの重合体
の紡糸原液を調製し紡糸し、紡糸繊維を不融化し、最後
に不融化繊維を真空中、不活性ガスあるいは還元性ガス
雰囲気中で1300〜1500℃で加熱処理することによって上
記繊維を調製する方法である。
繊維中の各元素の割合は一般に Si:28〜60重量％、 C:23〜60重量％、 Ti又はZr:0.5〜30重量％、 O:1〜30重量％ である。
繊維の形状については特別の制限はないが、直径５〜15
μｍの連続繊維であることが、機械的特性及び電磁波吸
収特性の良好な電磁波吸収材を得るうえで好ましい。
繊維は繊維そのものを単軸方向、多軸方向に配向させる
方法、あるいは平織、朱子織、模紗織、綾織、からみ
織、らせん織、三次元織などの各織物にして使用する方
法などがある。
本発明の電磁波吸収材に使用されるマトリックスとして
は、プラスチックス又はセラミックスが挙げられる。
プラスチックマトリックスの具体例としては、エポキシ
樹脂、ポリエステル樹脂、ポリイミド樹脂、フェノール
樹脂、ポリウレタン樹脂、ポリアミド樹脂、ポリカーボ
ネート樹脂、シリコン樹脂、フェノキシ樹脂、ポリフェ
ニレンサルファイド樹脂、フッソ樹脂、炭化水素樹脂、
含ハロゲン樹脂、アクリル酸系樹脂及びアクリロニトリ
ル・ブタジエン・スチレン樹脂、超高分子量ポリエチレ
ン、ポリスチレン等が挙げられる。
これらのプラスチックマトリックスの中でもエポキシ樹
脂が好んで使用される。エポキシ樹脂は、ポリエポキシ
ド、硬化剤、硬化触媒などからなる樹脂組成物である。
ポリエポキシドとしては、例えば、ビスフェノールＡ、
Ｆ及びＳのグリシジル化合物、クレゾールノボラック又
はフェノールノボラックのグリシジル化合物及び脂環族
ポリエポキシドなどが挙げられる。ポリエポキシドの別
の例としては、多価フェノール、多価アルコール又は芳
香族アミンのグリシジル化合物が挙げられる。
これらのポリエポキシドの内、ビスフェノールＡのグリ
シジル化合物、ジミノジフェニルメタンのグリシジル化
合物、アミノフェノールのグリシジル化合物が一般に使
用される。また、本発明の電磁波吸収材を航空機の一次
構造材料のような高機能を要求される部材として使用す
る場合は、上記ポリエポキシドの中でも、ジミノジフェ
ニルメタンなどの多官能アミンのグリシジル化合物を使
用することが好ましい。
セラミックマトリックスの具体例としては、炭化珪素、
炭化チタン、炭化ジルコニウム、炭化ニオブ、炭化タン
タル、炭化ホウ素、炭化クロム、炭化タングステン、炭
化モリブデンのような炭化物セラミック；窒化珪素、窒
化チタン、窒化ジルコニウム、窒化バナジウム、窒化ニ
オブ、窒化タンタル、窒化ホウ素、窒化ハフニウムのよ
うな窒化物セラミック；アルミナ、マグネシア、ムライ
ト、コージライトのような酸化物セラミックが挙げられ
る。
繊維及びマトリックスからなる複合材料はそれ自体公知
の方法に従って調製することができる。
マトリックスがプラスチックスである場合には、ハンド
レイアップ法、マッチドメタルダイ法、プレークアウェ
イ法、フィラメントワインディング法、ホットプレス
法、オートブレーク法、連続引抜法などを採用すること
ができる。
マトリックスがセラミックスである場合には、繊維とセ
ラミック粉末との集合体を調製し、この集合体を焼結す
る方法を採用することができる。上記集合体の調製方法
としては、セラミック粉末に繊維を埋没させる方法、繊
維とセラミック粉末を交互に配設する方法、予め繊維を
配置しておき、その間隙にセラミック粉末を充填する方
法などが採用される。
本発明の電磁波吸収材は、一般にマトリックス中に前記
した各種形状の繊維が配設された複合体を複数枚一体と
して積層した構造である。特にマトリックス中に一方向
に引き揃えられた繊維が配設された複合体を複数枚積層
した構造であることが好ましい。積層方法としては、繊
維の向きを揃えて複合体を積層する方法、繊維の向きを
交互に直交させて複合体を積層する方法などを採用する
ことができる。良好な電磁波吸収特性を得るためには、
後者の積層方法であることが好ましい。
電磁波吸収材の厚さは通常１〜10mmである。また、電磁
波吸収材中における繊維の割合は、30〜80体積％、特に
45〜65体積％であることが好ましい。
本発明の電磁波吸収材は、電磁波が入射する面に電磁波
透過材が積層された構造であることができる。
空気の誘電率よりも極端に大きな誘電率を有する材料に
電磁波が入射した場合、表面層における電磁波の反射が
大きくなることは良く知られた事実である。電磁波吸収
材としては、表面における反射量がきわめて小さいもの
が要求される。また、表面から徐々に誘電率が大きくな
るような積層構造にすると、上方の表面積での電磁波の
反射は大幅に減少する。
本発明の電磁波吸収材と組み合わせて使用することがで
きる電磁波透過材の具体例としては、ガラス繊維あるい
は芳香族ポリアミド繊維で強化されたポリエステル樹脂
が挙げられる。
好ましい電磁波透過材は、ケイ素、炭素、チタン又はジ
ルコニウム、及び酸素からなり実質的に非晶質の物質で
構成され、105〜1010Ω・cmの比抵抗を有する繊維とマ
トリックスとからなる複合材料である。
上記の繊維は、不融化繊維の加熱処理を800〜1300℃の
範囲内の温度で行う以外は、電磁波透過材に使用される
繊維と同様の方法で調製することができる。
電磁波透過材に使用される上記繊維中の各元素の割合
は、一般に、 Si:26〜58重量％、 C:25〜62重量％、 Ti又はZr:0.5〜30重量％、 O:1〜30重量％ である。
電磁波透過材に使用されるマトリックス、繊維とマトリ
ックスとの複合体の調製方法は、電磁波吸収材における
方法と同じである。
電磁波吸収材の表面に積層して形成される電磁波透過材
層の厚さは通常0.1〜5mmである。また、電磁波透過材中
における繊維の割合は、30〜80体積％、特に45〜65体積
％であることが好ましい。
（発明の効果） 本発明の電磁波吸収材は500〜3000GHzのマイクロ波、特
に２〜20GHzのマイクロ波を選択的に吸収することがで
きる。また、本発明の電磁波吸収材に使用される繊維
は、半導体的性質を有しており、電気電導度の活性化エ
ネルギーが0.01eV以下と非常に小さく、温度が変化して
も電磁波吸収特性が変化しないため、本発明の電磁波吸
収材は広い温度範囲にわたって優れた電磁波吸収性能を
示す。さらに、この電磁波吸収材は、強度及び弾性率が
高く、優れた耐熱性を有しており、船舶、航空機などの
一次構造材料として使用することができる。
（実施例） 以下に実施例を示す。実施例において、電磁波吸収材の
電磁波反射減衰量は、22.86mm×10.16mm×2.00mmのサン
プルについて、横川・ヒューレッドパッカード社製のＳ
−パラメーター測定装置を使用して測定した。この装置
は、Ｓ−パラメーター測定器HP8515A、ネットワークア
ナライザーHP8510及びシンセサイズドスイーパーHP8340
Aから構成されている。電磁波吸収材の電磁波反射減衰
量（db）の測定は25℃で行った。
参考例１ 無水キシレン2.5l及びナトリウム400gを窒素ガス気流下
にキシレンの沸点まで加熱し、ジメチルクロロシラン１
を１時間で滴下した。滴下終了後、10時間加熱還流
し、沈澱物を生成させた。沈澱を濾過し、メタノールつ
いで水で洗浄して白色粉末のポリジメチルシラン420gを
得た。
このポリジメチルシラン400gを、ガス導入管、撹拌機、
冷却器及び留出管を備えたフラスコに仕込み、撹拌しな
がら窒素ガス気流下420℃で加熱処理して、留出受器に3
50gの無色透明な少し粘性のある液体を得た。この液体
の数平均分子量は蒸気圧浸透法で測定したところ470で
あった。この物質はIRスペクトル測定の結果、（Si-C
H2）結合単位の全数対（Si-Si）結合単位の全数の比率
が約1:3の有機珪素重合体であることが判明した。
この有機珪素重合体100gにポリボロジフェニルシロキサ
ン3gを添加し、窒素ガス雰囲気下に350℃で熱縮合し
て、式 （Si-CH2）のカルボシラン単位から主としてなる主鎖骨
格を有し、カルボシラン単位の珪素原子に水素原子及び
メチル基を有するポリカルボシランを得た。このポリカ
ルボシランにテトラブトキシチタンを加えて、窒素ガス
雰囲気中、340℃で架橋重合させることにより（Si-C
H2）単位100部と式（Ti−Ｏ）単位10部とからなるポリ
チタノカルボシランを得た。この重合体を溶融紡糸し、
空気中190℃で不融化処理し、引き続いて窒素ガス雰囲
気中1500℃で焼成した。
得られた繊維（繊維〔Ｉ〕）は、径10μｍ、引張強度30
0kg/mm2、引張弾性率16t/mm2、比抵抗1.5Ω・cmであっ
た。
参考例２ 参考例１で得られた不融化繊維を1200℃で焼成した以外
は参考例１と同様の方法を繰り返した。
得られた繊維（繊維〔II〕）は、径10μｍ、引張強度28
0kg/mm2、引張弾性率15.5t/mm2比抵抗２×10５Ω・cmで
あった。
参考例３ 参考例１で得られた不融化繊維を1050℃で焼成した以外
は参考例１と同様の方法を繰り返して繊維〔III〕を得
た。
繊維〔III〕は、径10.5μｍ、引張強度260kg/mm2、引張
弾性率15t/mm2、比抵抗３×10７Ω・cmであった。
参考例４ 焼成温度を1400℃に変えて以外は参考例１と同様にして
繊維（繊維〔IV〕）を調製した。
繊維〔IV〕は、径10μｍ、引張強度305kg/mm2、引張弾
性率16.5t/mm2、比抵抗40Ω・cmであった。
参考例５ 参考例１におけると同様にして調製したポリカルボシラ
ンにジルコニウムテトラブトキシドを添加し、窒素ガス
雰囲気中、250℃で架橋重合させることにより（Si-C
H2）単位100部と式（Zr−Ｏ）単位10部とからなるポリ
ジルコノカルボシランを得た。この重合体を溶融紡糸
し、空気中190℃で不融化処理し、引き続いて窒素ガス
雰囲気中1500℃で焼成した。
得られた繊維（繊維〔Ｖ〕）は、径10μｍ、引張強度31
0kg/mm2、引張弾性率16.5t/mm2、比抵抗2.0Ω・cmであ
った。
実施例１ ビスフェノールＡ型エポキシ樹脂（チバガイギー社製、
XB2879A）100重量部及びジシアンアミド硬化剤（チバガ
イギー社製、XB2879B）20重量部を均一に混合した後
に、混合物を重量比で1:1のメチルセロソルブとアセト
ンとの混合溶媒に溶解して、上記混合物の28重量％溶液
を調製した。
繊維〔Ｉ〕に上記溶液を含浸した後に、ドラムワインダ
ーを用いて一方向に巻き取り、熱風循環オーブン中で10
0℃で14分間加熱することによって、半硬化状態のプリ
プレグを調製した。このプリプレグの樹脂含有量は50体
積％、厚さは0.2mmであった。
このプリプレグ11枚を隣合うプリプレグの繊維の向きが
互いに直交するように積層し、積層体を130℃、プレス
圧力11kg/cm2で90分間プレス成形して、250mm×250mm×
2mmの複合体Ａを得た。
これとは別に、繊維〔III〕を使用した以外は上記と同
様にして、樹脂含有量50体積％、厚さ0.2mmのプリプレ
グを調製した。このプリプレグ16枚を用いた以外は上記
と同様にして、250mm×250mm×2mmの複合体Ｂを得た。
上記両複合体から22.86mm×10.16mm×2mmの板状の複合
体Ａ及びＢを切り出し、両複合体を、繊維の配列方向を
揃えて、プリプレグの調製用に使用したエポキシ樹脂溶
液で貼り合わせて、電磁波吸収材を作成した。
この電磁波吸収材に繊維〔II〕を含む複合体の方向から
マイクロ波を導入したところ、５〜20GHzの周波数領域
で15db以上の反射減衰量（反射率3.2％以下）を示し
た。
また、この電磁波吸収材の繊維方向の曲げ強度は102kg/
mm2、引張強度は95kg/mm2であった。
実施例２ 繊維〔II〕に代えて繊維〔III〕を使用した以外は実施
例１におけると同様にして複合体Ｃを調製した。
ついで、この複合体Ｃ及び実施例１で得られた複合体Ａ
から実施例１におけると同様にして、電磁波吸収材を作
成した。
この電磁波吸収材に繊維〔III〕を含む複合体の方向か
らマイクロ波を導入したところ、10GHzで40dbの反射減
衰量を示した。
また、この電磁波吸収材の繊維方向の曲げ強度は108kg/
mm2、引張強度は97kg/mm2であった。
実施例３ 繊維〔Ｉ〕に代えて繊維〔IV〕を使用した以外は実施例
１におけると同様にして、樹脂含有量50体積％、厚さは
0.2mmのプリプレグを調製した。
このプリプレグ16枚を用いた以外は実施例１におけると
同様にして、250mm×250mm×3mmの複合体からなる電磁
波吸収材を得た。
この電磁波吸収材にマイクロ波を導入したところ、10GH
zで30dbの反射減衰量を示した。
また、この電磁波吸収材の繊維方向の曲げ強度は105kg/
mm2、引張強度は96kg/mm2であった。
実施例４ 繊維〔Ｉ〕に代えて繊維〔Ｖ〕を使用した以外は実施例
１と同様にして、電磁波吸収材を作成した。
この電磁波吸収材に繊維〔II〕を含む複合体の方向から
マイクロ波を導入したところ、５〜20GHzの周波数領域
で14db以上の反射減衰量を示した。
また、この電磁波吸収材の繊維方向の曲げ強度は105kg/
mm2、引張強度は96kg/mm2であった。

Claims (1)

    【特許請求の範囲】
  1. 【請求項１】下記ｉ）、ii）及びiii）からなる群から
    選択される無機質物質で構成され、10-2〜102Ω・cmの
    比抵抗を有する繊維とマトリックスとの複合材料からな
    ることを特徴とする電磁波吸収材。 ｉ） Si、Ｍ、Ｃ及びＯからなる非晶質物質。 ii） 結晶質物質の集合体であって、β−SiC、Ｃ及びM
    C、並びにβ−SiCとMCとの固溶体及び／又はMC1-xから
    構成され、各結晶質物質の粒径が500Å以下である結晶
    質物質。 iii） 上記ｉ）の非晶質物質と上記ii）の結晶質物質
    の集合体との混合物。 （上式中、ＭはTi又はZrを示し、ｘは０より大きく１未
    満の数である。）
JP16867388A 1987-09-04 1988-07-08 電磁波吸収材 Expired - Lifetime JPH071837B2 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
JP16867388A JPH071837B2 (ja) 1987-09-04 1988-07-08 電磁波吸収材
EP88308106A EP0306311B1 (en) 1987-09-04 1988-09-01 Electromagnetic wave absorbing material
DE3889042T DE3889042T2 (de) 1987-09-04 1988-09-01 Elektromagnetische Wellen absorbierendes Material.
CA 576414 CA1330704C (en) 1987-09-04 1988-09-02 Electromagnetic wave absorbing material
US07/550,221 US5094907A (en) 1987-09-04 1990-07-10 Electromagnetic wave absorbing material

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP22023387 1987-09-04
JP62-220233 1987-09-04
JP16867388A JPH071837B2 (ja) 1987-09-04 1988-07-08 電磁波吸収材

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Publication Number Publication Date
JPH01157598A JPH01157598A (ja) 1989-06-20
JPH071837B2 true JPH071837B2 (ja) 1995-01-11

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EP (1) EP0306311B1 (ja)
JP (1) JPH071837B2 (ja)
CA (1) CA1330704C (ja)
DE (1) DE3889042T2 (ja)

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Also Published As

Publication number Publication date
JPH01157598A (ja) 1989-06-20
DE3889042T2 (de) 1994-07-21
CA1330704C (en) 1994-07-19
DE3889042D1 (de) 1994-05-19
EP0306311B1 (en) 1994-04-13
US5094907A (en) 1992-03-10
EP0306311A1 (en) 1989-03-08

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