JPH0428743B2 - - Google Patents

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Publication number
JPH0428743B2
JPH0428743B2 JP56060540A JP6054081A JPH0428743B2 JP H0428743 B2 JPH0428743 B2 JP H0428743B2 JP 56060540 A JP56060540 A JP 56060540A JP 6054081 A JP6054081 A JP 6054081A JP H0428743 B2 JPH0428743 B2 JP H0428743B2
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filler
particles
composition
polymer
resistivity
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JPS56161464A (en
Inventor
Uorinton Fuutsu Junia Robaato
Enu Esu O Andoryuu
Ii Miraa Baaton
Jefurii Gotsuchaa Aran
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Raychem Corp
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Raychem Corp
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01C—RESISTORS
    • H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
    • H01C7/02—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having positive temperature coefficient
    • H01C7/027—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material having positive temperature coefficient consisting of conducting or semi-conducting material dispersed in a non-conductive organic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Ceramic Engineering (AREA)
  • Electromagnetism (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Thermistors And Varistors (AREA)
  • Conductive Materials (AREA)

Description

【発明の詳細な説明】
本発明はPTC導電性ポリマー組成物を使用し
た回路保護装置に関する。 導電性ポリマー組成物、およびそれからなる装
置は公知であり、例えば米国特許第2978665号、
3243753号、3351882号、3571777号、3793716号、
3823217号、3861029号、3983075号、4017715号、
4177376号、4237441号および4246468号；イギリ
ス国特許第1534715号；J.Phys Ｄ，Appl.Phys.
第巻、1457〜1462頁；R.F.Blahaの「The
PTC Resistor」と題する記事（in Proceedings
of the Electronic Components Conference，
1971）；H.ShulmanおよびJohn Barthoの
「Solid State Bistable Power Switch Study」
と題する報告（1968年８月，under Contract
NAS−12−647、the National Aeronautics
and Space Administrationにより出板）；J.
Applied Polymer Science 19 813−815
（1975）、Klason and Kubat；Polymer
Engineering and Science 18 649−653
（1978）、Narkis et al；および西独国特許出願
公開第2634999号、2755077号、2746602号、
2755076号、2821799号、2948281号、2949173号お
よび3002721号などに記載されている。さらに、
この分野における極く最近の進歩について米国特
許出願第41071号、67207号、88304号、141984号、
141987号、141988号、141989号、142053号および
142054号などに詳しく記載されている。 これらの先行技術は、導電性ポリマー組成物中
になんらかの導電性粒子を使用する可能性につい
て言及しているが、カーボンブラツクと比較し
て、金属粒子はあまり使用されていない。その大
きな理由の１つは、既知の金属充填剤組成物、特
にPTC組成物は内部アークを起こしやすく、そ
れが為に衰弱が早くなり、時には爆発や火災を起
こし、特に10ボルトまたはそれ以上の電圧では特
にそうであることが知られているからである。 本発明者らは、金属粒子またはそれと同程度の
高い導電性を有するその他の物質を含んだPTC
組成物の安定性は、導電性が実質的により低くそ
して／または平均粒子サイズが実質的により小さ
い別の粒子充填剤をかなりの量までその組成物に
含ませることにより改善することができることを
見い出した。 即ち、本発明は、(1)ポリマー成分およびポリマ
ー成分中に分散している充填剤成分からなり、
PTC挙動を示す導電性ポリマー組成物からなる
PTC要素、および(2)PTC要素に電流を流す少な
くとも２個の電極を有して成る回路保護装置であ
つて、 ポリマー成分が(A)(1)ポリオレフイン、(2)(a)１種
またはそれ以上のオレフインおよび(b)極性基を含
有する１種またはそれ以上のオレフイン性不飽和
モノマーから誘導された単位からなるコポリマ
ー、ならびに(3)ハロゲン化ビニルおよびビニリデ
ンポリマーから成る群から選択された熱可塑性ポ
リマーであり、および(B)少なくとも20％の結晶度
を有しており、 充填剤成分が (a) (i)組成物の少なくとも10容量％を占め、(ii)
0.1〜５ミクロンの平均粒子寸法d1を有し、25
℃における固有抵抗が10-3オーム・cmよりも小
さい導電性ニツケル粒子からなる第１充填剤、
および (b) 組成物の少なくとも４容量％を占め、(i)第１
充填剤の粒子よりも低い導電性を有し、(ii)
0.001〜50ミクロンの平均粒子寸法d2を有し、
および(iii)カーボンブラツクまたは非導電性物質
からなる粒子の形態である第２充填剤 からなる充填剤成分であり、 導電性ポリマー組成物が(i)スイツチング温度が
TsであるPTC挙動を示し、(ii)−40℃とTsの間で
1.0オーム・cmより小さい最小固有抵抗Rminを有
し、および(iii)Tsと（Ts＋100）℃の間で最小固
有抵抗Rminの少なくとも10000倍の最大固有抵
抗を有することを特徴とする回路保護装置を提供
するものである。 最小固有抵抗（抵抗率）は、好ましくは0.1オ
ーム・cm以下、より好ましくは10-2オーム・cm以
下、特に10-4オーム・cm以下である。最大固有抵
抗は、最小固有抵抗の少なくとも100000倍である
ことが好ましく、好ましくは少なくとも103オー
ム・cm、より好ましくは少なくとも104オーム・
cm、特に少なくとも105オーム・cmである。第１
充填剤の量は、組成物の容量の好ましくは10〜75
％、特に30〜60％である。第２充填剤の量は、組
成物容量の好ましくは４〜50％、より好ましくは
６〜25％、特に好ましくは８〜20％である。 本発明に係る新規組成物は、23℃における固有
抵抗を低く、即ち唯一の導電性充填剤としてカー
ボンブラツクを含有している組成物よりずつと低
くすることができ、回路保護装置に特に有用であ
る。 第１充填剤はニツケルからなる。 第１充填剤の粒子の粒子サイズは通常、0.1〜
５、特に好ましくは0.5〜２ミクロンであること
が好ましい。球形の粒子が好ましいが、他の形状
のもの、例えばフレークや棒状のものも使用する
ことができる。 第２充填剤は導電性粒子および／または非導電
性粒子からなつていてよく、カーボンブラツクま
たは金属粒子からなつていることが好ましい。第
１充填剤の平均粒子サイズをd1とし、第２充填剤
の平均粒子サイズをd2とすると、d1／d2比は好ま
しくは２ないし10000、より好ましくは10ないし
5000、特に好ましくは100ないし1000である。第
２充填剤の粒子の導電性が第１充填剤の粒子のそ
れと同程度であるかあるいはそれより大きい場合
（そして好ましくは第２充填剤の粒子が、その25
℃における固有抵抗が10-3オーム・センチ以下で
ある物質、例えば金属で構成されている場合はい
つでも）、d1／d2比は少なくとも２、好ましくは
少なくとも10である。第２充填剤が金属粒子から
なる場合、その金属は第１充填剤について既述し
た金属のいずれかであつてよい。第１充填剤およ
び第２充填剤が共に金属粒子からなつている場
合、その金属は同一であつても異なつていてもよ
い。好ましい第２充填剤は平均粒子サイズが約
0.01〜約0.07ミクロンであるカーボンブラツクで
ある。第２充填剤として使用することができる非
導電性粒子には、アルミナ３水和物、シリカ、ガ
ラスビーズおよび硫化亜鉛が包含される。第２充
填剤は平均粒子サイズが0.001〜50ミクロン、特
に0.01〜５ミクロンであることが好ましい。 本発明の新規組成物のポリマー成分は架橋され
ているものであつても架橋のないものであつても
よく、また、１またはそれ以上のポリマーからな
つていてよい。その成分の結晶化度は少なくとも
５％、特に少なくとも10％、特別には少なくとも
20％であることが好ましい。その成分は本質的に
１またはそれ以上の熱可塑性樹脂または架橋熱可
塑性樹脂よりなることが好ましいが、１またはそ
れ以上の熱可塑性エラストマー、エラストマー、
熱硬化性樹脂またはその混合物を含んでいてもよ
い。好ましいポリマーはポリオレフイン類、例え
ばポリエチレン；(a)１またはそれ以上のオレフイ
ン類、例えばエチレンおよびプロピレン、および
(b)極性基を含有している１またはそれ以上のオレ
フイン性不飽和モノマー類、例えばビニルエステ
ル類および酸類およびα，β−不飽和有機酸類の
エステル類から導かれる単位からなるコポリマー
類；ハロゲン化ビニルおよびビニリデンポリマー
類、例えばポリビニルクロリド、ポリビニリデン
クロリド、ポリビニルフルオライドおよびポリビ
ニリデンフルオライド；ポリアミド類；ポリスチ
レン；ポリアクリロニトリル；熱可塑性シリコン
樹脂；熱可塑性ポリエーテル類；熱可塑性変性セ
ルロース；およびポリスルホン類などである。そ
の他の好適なポリマー類は既述した特許および特
許出願明細書に開示されている。 その他の添加剤を組成物に含ませてもよい。こ
の様な添加剤としては抗酸化剤、難燃剤および架
橋剤などが含まれる。 本発明の組成物は常法により、好ましくはポリ
マー成分と充填剤を溶融混合することにより製造
することができる。高充填剤量の組成物を得るに
は長時間混合する必要がある。 以下に実施例を挙げて本発明を更に詳細に説明
する。ただし実施例１および19は比較例である。 実施例 １〜19 本発明の導電性組成物を以下の表に示した成分
および量を用いて製造した。 実施例１〜４、10、12、13および15〜19の組成
物は以下の方法により製造した。7.6cmの電気ロ
ールミル（練りロール機）をポリマー融点より25
〜40℃高い温度に加熱する。ポリマーを加えて溶
融し、バンド状に巻付ける。抗酸化剤を加えて分
散させる。第１充填剤および第２充填剤を少量づ
つゆつくりと添加し、金属粒子がロールと接触
し、それによつてポリマーがロールからはずれな
い様に混合する。組成物が均一になるまで処理
し、そしてそれからさらに約３分間ロールミルで
処理する。得られた組成物をロール機からはずし
てシート状とし、圧縮成型してスラブにする前に
冷却する。 実施例５〜９および11は以下の手順によつた。
ブラベンダーミキサーの空胴部をポリマーの融点
より約20〜40℃高い温度に加熱する。20rpmの回
転速度でペレツト状のポリマーを加え、溶融する
まで混合する。抗酸化剤を添加し分散させる。少
量づつ増量しながら第１および第２充填剤を添加
する。全成分が混合されたら回転速度を60rpmに
上げ、この組成物を約２分間混合する。ブラベン
ダーのスイツチを切り、混合物を羽根および壁か
ら削り取り、冷却する。この組成物を圧縮成型し
てスラブにする。 実施例14は次の様にして行なつた。バンバリー
ミキサーを蒸気で150〜180℃に予め加熱する。約
500rpmの速度でポリマーおよび抗酸化剤を添加
する。ポリマーが溶け始めたら、温度を一定に保
ちながら第１および第２充填剤を少量づつ添加す
る。たたき打ちしながら組成物を５分間混合し、
次いでミキサーから出し、冷却し、顆粒化する。
顆粒を圧縮成型してスラブするか、テープに押し
出す。 それぞれの実施例において、温度を上昇させな
がら組成物の固有抵抗を測定した。表にはそれぞ
れの組成物について、固有抵抗比、即ち25℃に於
ける固有抵抗に対する実測ピーク固有抵抗の比を
記載した。実施例１〜８および19の組成物につ
き、固有抵抗／樹脂曲線をそれぞれ第１図〜第９
図に示した（曲線頂上の水平線は、単に装置がそ
れより高い固有抵抗を測定できないことを示すだ
けである）。実施例１〜７および14〜19の組成物
はまた、電気安定性試験にかけた。ここでは組成
物中の過渡電流をオシロスコープを用いて観察し
た。この過渡電流はトラツキングや短絡を起すこ
とともにスパークや内部アークの存在を示すと考
えられている。3.8×0.64cmの組成物のそれぞれ
の短端に沿つて幅0.64cmの導電性銀メツキを施
し、2.5×0.64cmの試験区域をつくる。この試料
を１オームの抵抗体および電圧可変手段
（variac）によつて電圧を０から120ボルトまで変
えることのできる完全にひずみのない60ヘルツの
電力源（可聴信号から導かれる）を持つた回路に
入れる。抵抗体の端子間電圧（これは導電性ポリ
マー素子を流れる電流の尺度である）を、電圧を
10、20、60または120ボルトの一定電圧に保ちな
がら５分間に渡つてオシロスコープでモニターす
る。オシロスコープ上、鋭い不規則なスパイクと
して観察される導電性ポリマー中の過渡電流は、
その試料の電気的不安定さを示している。比較例
である実施例１および19で製造された試料はこの
試験において、不安定であることがわかつた。実
施例２〜７で製造した試料は安定であつた。実施
例14〜18で製造した試料も安定であつた。 表中に示した種々の成分についての記号は、以
下の意義を有する。 HDPE……高密度ポリエチレン（Phillps
Marlex6003） LDPE……低密度ポリエチレン（Union
Carbide DYNH−１） MDPE……中密度ポリエチレン（Gulf
2604M） EEA……エチレン−エチルアクリレートコポ
リマー（Uuion Carbide DPD6169） EAA……エチレン−アクリル酸コポリマー
（Dow Chemical Co.EAA455） FEP……ヘキサフルオロエチレン−テトラフ
ルオロエチレンコポリマー（Du Pont
FEP100） PVF2……ポリビニリデンフルオライド
（Pennwalt Kynar461） Epon828……Shell Chemical Coから販売され
ているエポキシ樹脂 Versamid140……General Millsから販売され
ているポリアミド硬化剤 AO……抗酸化剤、米国特許第3986981号に記
載されている平均重合化度が３〜４である
４，4′−チオビス（３−メチル−６−tertブ
チルフエノール）のオリゴマー Hydral……Alcoaから販売されている、粒子
の大部分が0.0005〜２ミクロンの範囲にある
アルミナ３水和物 Cab−Ｏ−Sil……Cabot Corporationから販売
されている、粒子の大部分が0.007〜0.016ミ
クロンの範囲にある粒子状シリカ ガラスビーズ……Potters Industriesから販売
されている粒子サイズが0.004〜44ミクロン
の間にあるビーズ CaCO3……OMYA Inc.から販売されている炭
酸カルシウム（Omya BSH）
【表】
【表】 【図面の簡単な説明】
第１図〜第９図は、それぞれ実施例１〜８およ
び19で製造した本発明組成物についての固有抵抗
と温度との関係を示すグラフである。

Claims (1)

  1. 【特許請求の範囲】 １ (1)ポリマー成分およびポリマー成分中に分散
    している充填剤成分からなり、PTC挙動を示す
    導電性ポリマー組成物からなるPTC要素、およ
    び(2)PTC要素に電流を流す少なくとも２個の電
    極を有して成る回路保護装置であつて、 ポリマー成分が(A)(1)ポリオレフイン、(2)(a)１種
    またはそれ以上のオレフインおよび(b)極性基を含
    有する１種またはそれ以上のオレフイン性不飽和
    モノマーから誘導された単位からなるコポリマ
    ー、ならびに(3)ハロゲン化ビニルおよびビニリデ
    ンポリマーから成る群から選択された熱可塑性ポ
    リマーであり、および(B)少なくとも20％の結晶度
    を有しており、 充填剤成分が (a) (i)組成物の少なくとも10容量％を占め、(ii)
    0.1〜５ミクロンの平均粒子寸法d1を有し、25
    ℃における固有抵抗が10-3オーム・cmよりも小
    さい導電性ニツケル粒子からなる第１充填剤、
    および (b) 組成物の少なくとも４容量％を占め、(i)第１
    充填剤の粒子よりも低い導電性を有し、(ii)
    0.001〜50ミクロンの平均粒子寸法d2を有し、
    および(iii)カーボンブラツクまたは非導電性物質
    からなる粒子の形態である第２充填剤 からなる充填剤成分であり、 導電性ポリマー組成物が(i)スイツチング温度が
    TsであるPTC挙動を示し、(ii)−40℃とTsの間で
    1.0オーム・cmより小さい最小固有抵抗Rminを有
    し、および(iii)Tsと（Ts＋100）℃の間で最小固
    有抵抗Rminの少なくとも10000倍の最大固有抵
    抗を有することを特徴とする回路保護装置。 ２ ポリマー成分が、ポリビニリデンフルオライ
    ドを含んで成る特許請求の範囲第１項記載の装
    置。 ３ ポリマー成分がポリエチレンを含んで成る特
    許請求の範囲第１項記載の装置。 ４ ポリマー成分が架橋されている特許請求の範
    囲第１〜３項のいずれかに記載の装置。 ５ (1)ポリマー成分がポリエチレンを含んで成
    り、(2)充填剤成分が、(i)組成物の10〜60容量％を
    占める第１充填剤、および(ii)0.01〜0.07ミクロン
    の平均粒子寸法d2を有するカーボンブラツク粒子
    から本質的になり、組成物の４〜50容量％を占め
    る第２充填剤からなる特許請求の範囲第４項記載
    の装置。 ６ 0.01オーム・cmより小さい最小固有抵抗を有
    する特許請求の範囲第１〜５項のいずれかに記載
    の装置。
JP6054081A 1980-04-21 1981-04-21 Filler-containing ptc electroconductive polymer composition Granted JPS56161464A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US06/141,991 US4545926A (en) 1980-04-21 1980-04-21 Conductive polymer compositions and devices

Publications (2)

Publication Number Publication Date
JPS56161464A JPS56161464A (en) 1981-12-11
JPH0428743B2 true JPH0428743B2 (ja) 1992-05-15

Family

ID=22498121

Family Applications (1)

Application Number Title Priority Date Filing Date
JP6054081A Granted JPS56161464A (en) 1980-04-21 1981-04-21 Filler-containing ptc electroconductive polymer composition

Country Status (7)

Country Link
US (1) US4545926A (ja)
EP (1) EP0038714B1 (ja)
JP (1) JPS56161464A (ja)
AT (1) ATE25892T1 (ja)
CA (1) CA1165996A (ja)
DE (1) DE3175988D1 (ja)
GB (1) GB2074585B (ja)

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US3976600A (en) * 1970-01-27 1976-08-24 Texas Instruments Incorporated Process for making conductive polymers
US3686139A (en) * 1970-03-10 1972-08-22 Globe Union Inc Resistive coating compositions and resistor elements produced therefrom
GB1369210A (en) * 1972-02-01 1974-10-02 Ici Ltd Aromatic polymers
GB1444722A (en) * 1972-08-25 1976-08-04 Harris Barbara Joan Electrical heating elements
JPS50748A (ja) * 1973-05-02 1975-01-07
US3983075A (en) * 1974-06-21 1976-09-28 Kennecott Copper Corporation Copper filled conductive epoxy
JPS5313466B2 (ja) * 1974-11-20 1978-05-10
JPS5947843B2 (ja) * 1976-08-28 1984-11-21 ジェイエスアール株式会社 高感度感圧抵抗体およびその製造方法
GB1602372A (en) * 1977-05-18 1981-11-11 Hotfoil Ltd Electrically conductive rubber composition
US4147668A (en) * 1977-06-30 1979-04-03 Polaroid Corporation Conductive compositions and coating compositions for making the same
US4308314A (en) * 1978-08-04 1981-12-29 Sekisui Kagaku Kogyo Kabushiki Kaisha Electric recording material
US4237441A (en) * 1978-12-01 1980-12-02 Raychem Corporation Low resistivity PTC compositions

Also Published As

Publication number Publication date
GB2074585A (en) 1981-11-04
EP0038714B1 (en) 1987-03-11
US4545926A (en) 1985-10-08
JPS56161464A (en) 1981-12-11
EP0038714A3 (en) 1981-11-18
GB2074585B (en) 1984-07-25
EP0038714A2 (en) 1981-10-28
DE3175988D1 (en) 1987-04-16
CA1165996A (en) 1984-04-24
ATE25892T1 (de) 1987-03-15

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