JP2010043256A - 導電性ポリマー発泡体、その作製方法、ならびにその物品およびその使用 - Google Patents
導電性ポリマー発泡体、その作製方法、ならびにその物品およびその使用 Download PDFInfo
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- JP2010043256A JP2010043256A JP2009181437A JP2009181437A JP2010043256A JP 2010043256 A JP2010043256 A JP 2010043256A JP 2009181437 A JP2009181437 A JP 2009181437A JP 2009181437 A JP2009181437 A JP 2009181437A JP 2010043256 A JP2010043256 A JP 2010043256A
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- Prior art keywords
- foam
- precursor composition
- particles
- polymer foam
- conductive
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/228—Forming foamed products
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- C—CHEMISTRY; METALLURGY
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Abstract
【解決手段】前駆体組成物から、第一の表面および反対側の第二の表面を有する物品を形成するステップであって、前記前駆体組成物が、ポリマー発泡前駆体組成物と、複数の磁性導電性粒子を含む充てん剤組成物とを含むステップと;前記前駆体組成物を発泡させて、前記前駆体組成物中に複数のセルを形成するステップと;前記発泡前駆体組成物に磁場を印加するステップであって、前記磁場が、前記物品の前記第一の表面と前記反対側の第二の表面との間で互いに孤立したチェーンへと前記導電性の磁性粒子を整列させるために有効な強度を有し、また有効な時間印加されるステップと;前記ポリマー発泡前駆体組成物を凝固させて、特定の密度、および特定の体積抵抗率を有するポリマー発泡複合体を得るステップとを含む。
【選択図】なし
Description
本開示は、導電性ポリマー発泡体およびその作製方法、ならびにこれらポリマー発泡体を含む物品に関する。
ポリマー発泡複合体を作製する方法は、前駆体組成物から、第一の表面および反対側の第二の表面を有する物品を形成するステップであって、前記前駆体組成物が、ポリマー発泡前駆体組成物と、複数の磁性導電性粒子を含む充てん剤組成物とを含むステップと;前記前駆体組成物を発泡させて、前記前駆体組成物中に複数のセルを形成するステップと;前記発泡前駆体組成物に磁場を印加するステップであって、前記磁場が、前記物品の前記第一の表面と前記反対側の第二の表面との間で互いに孤立したチェーンへと前記導電性の磁性粒子を整列させるために有効な強度を有し、また有効な時間印加されるステップと;前記ポリマー発泡前駆体組成物を凝固させて、約1〜約125ポンド/立方フィートの密度を有し、60ポンド/平方インチの圧力で約10-3ohm−cm〜約103ohm−cmの体積抵抗率を有するポリマー発泡複合体を得るステップとを含む。
ここで例示的な図面を参照するが、いくつかの図面において同様の要素には、同様に番号付けされている。
本明細書には、ポリマー発泡体が開示されており、これらポリマー発泡体において、導電性高アスペクト比粒子を発泡体内でカラムへと磁気的に整列させることで、ポリマー発泡体に電気電導性を付与している。このような磁気整列は、固体ポリマーにおいては実証されているが、この技法を使用してセル状ポリマー(cellular polymers)に電気電導性を提供することもできることは予期せぬことである。
所望の導電性を実現するために、他の導電性充てん剤を加えて使用することができ、カーボンブラック;PAN繊維などの炭素繊維;金属被覆ガラス繊維、金属被覆炭素繊維、金属被覆有機繊維、金属被覆セラミック球、金属被覆ガラスビーズなどの金属被覆繊維または球;微粒子状またはフィブリル状のポリアニリン、ポリピロール、ポリチオフェンなど本質的に導電性のポリマー;酸化スズや酸化インジウムスズなどの導電性金属酸化物;および上記導電性充てん剤の少なくとも1種を含む組み合わせを使用することもできる。磁性導電性充てん剤対導電性充てん剤の相対比率は、使用する充てん剤の種類および発泡体の所望の特性によってかなり大きく異なることがある。一般に、充てん剤組成物は、それぞれ充てん剤組成物の総重量に基づき、50〜100重量パーセント(wt%)の磁性導電性材料と、0〜50wt%の導電性充てん剤とを、より特別には75〜99wt%の磁性導電性充てん剤と、1〜25wt%の導電性充てん剤とを含むことができる。
Q(NCO)i
式中、iは2以上の整数、Qはi価の有機ラジカルであり、iの平均値は2を超える。Qは、置換または無置換炭化水素基であってよく、芳香族官能基、または式Q1−Z−Q1の基(Q1は、C1-36アルキレンまたはC6-36アリーレン基であり、Zは、−O−、−O−Q2−O、−CO−、−S−、−S−Q2−S−、−SO−、−SO2−、C1-24アルキレンまたはC6-24アリーレン)を含んでもよい。このようなポリイソシアネート類の例として、ヘキサメチレンジイソシアネート、1,8−ジイソシアネート−p−メタン、キシリルジイソシアネート、ジイソシアナートシクロヘキサン、フェニレンジイソシアネート、2,4−トリレンジイソシアネート、2,6−トリレンジイソシアネートおよび粗トリレンジイソシアネートを含めたトリレンジイソシアネート、ビス(4−イソシアナートフェニル)メタン、クロロフェニレンジイソシアネート、ジフェニルメタン−4,4’−ジイソシアネート(4,4’−ジフェニルメタンジイソシアネートまたはMDIとしても知られている)およびその付加物、ナフタレン−1,5−ジイソシアネート、トリフェニルメタン−4,4’,4’’−トリイソシアネート、イソプロピルベンゼン−アルファ−4−ジイソシアネート、ならびにポリメチレンポリフェニルイソシアネートなどの高分子量イソシアネートが挙げられる。
R[(OCnH2n)zOH]a
式中、Rは水素または多価炭化水素ラジカルで、aはRの価数と等しい整数(すなわち、1または2〜6〜8)で、nはそれぞれ2から4を含めた整数(特別には3)で、zはそれぞれ2〜約200、特別には15〜約100の値の整数である。一実施形態においては、ポリエーテルポリオールが、ジプロピレングリコール、1,4−ブタンジオール、2−メチル−1,3−プロパンジオール等のうちの1種または複数種の混合物、あるいは上記ポリエステルポリオールのうちの少なくとも1種を含む組み合わせを含む。
以下の試験を使用して導電率を決定した。公知のように、体積抵抗率および静電シールドについての個々の値は、その個々の試験方法および条件に依存することになる。例えば、試験中にサンプルにかかる圧力に伴って体積抵抗率および静電シールドが変化することがあることが知られている。以下のサンプルの体積抵抗率を測定するために有用な電気器具および試験装置は以下のとおりである。装置は、金板2.5cm×2.5cm(1インチ×1インチ)方形の電気接点を有する特注のプレスである。この装置には、オペレータがサンプルの表面に加わる力を制御し調節することを可能にするデジタルフォースゲージが装備されている。電源は、サンプル表面に0〜2アンペア供給することができる。サンプルを通しての電圧降下およびオームは、HP34420A Nano Volt/Micro Ohmmeterを用いて測定する。装置の電子部品を暖機してもよく、HP34420Aの場合、内部較正チェックを行う。試料を、試験環境の条件まで24時間平衡に保ってもよい。適切な試験環境は、室温23℃(70°F)で相対湿度50%(%RH)である。被検サンプルを、試験装置のプラテン間に設置し、表面に荷重を印加する。印加する荷重は被検サンプルの種類に依存し、軟質発泡体は小さい荷重を用いて試験するが、固形物は約63,279〜約210,930キログラム/平方メートル(90〜300ポンド/平方インチ)の荷重範囲を用いて試験する。荷重を印加したら、サンプルに電流を流し、サンプル厚さを通しての電圧降下を測定する。適切な試験には、0.5、1.0、1.6および2.0アンペアの4つの異なるアンペア設定における測定が含まれる。導電性複合体については、4つのアンペア設定すべてについて結果として得られる計算した体積抵抗率が類似している。体積抵抗率についての計算は、以下のとおりである:
体積抵抗率(ohm−cm)=(E/I)*(A/T)
式中、E=電圧降下(V)、I=電流(アンペア)、A=面積(cm2)、T=厚さ(cm)である。
シリコーン発泡体中の導電性充てん剤としてのニッケルおよびニッケル被覆セラミック微小球の評価を行った。シリコーン(Dow Corning Silicone 8137、およびNusil Technology LLC製のNUSIL 6033)と、充てん剤微小球と、シリコーン硬化抑制剤(Aldrich Chemical Co.製の1−オクチン−3−オール)とを、Flaktekスピードミキサ内で混ぜ合わせ、制御した厚さを有するPETフィルム上でキャストし、調節可能な磁場にさらされているオーブン内に設置した。一般に、化学的にブローさせ硬化させた発泡体の厚さは、70〜80ミル(1778〜2032マイクロメートル)であった。
表2は、100%ニッケル微小球を用いた追加の実験の結果を示す。18〜40ミル(457〜1016マイクロメートル)の厚さで配合物をキャストして、発泡体サンプルを調製した。
以下に示したような上部キャリアを有する場合についても有していない場合についても共に、100%Ni球または銀被覆ニッケル球を用いてより薄い発泡体を調製した。プレミックスを冷蔵庫の中で冷却した。結果を表3Aに示す。
実施例4〜5においては、以下の試験を利用した。体積抵抗率を測定するために、使用した装置は、Stable Micoro Systems(SMS)TA HD Plus Texture Analyserであった。50Kgのロードセルを使用して、圧縮試験中の材料の抵抗を記録した。サンプル(直径1/2インチ)を試験環境の条件、ここでは室温23℃(70°F)で相対湿度50%(%RH)まで24時間平衡に保った。オーム計の設定(2または20オーム)を選択し、設定に変化がある場合には、オーム計を較正した。フレームのたわみを較正し、10gの力の予荷重に到達するまで0.5mm/秒の速度で予備試験を行った。試験速度は、目標の力9.00Kgに到達するまで0.01mm/秒であった。抵抗および圧縮荷重をひずみの増大として記録した。体積抵抗率は、抵抗測定およびサンプル寸法に基づき計算した。体積抵抗率についての計算は上述のとおりである。
以下の手順によってポリウレタン複合発泡体を調製した。
実施例3で観察された直径範囲を有する、ニッケル被覆ステンレス鋼球を用いてポリウレタン複合発泡体を調製し、追加の発泡体一式を配合し、表5Aに示すように試験した。充てん剤は、100%Ni微小球、または銀被覆ニッケル球からなっていた。これらの実験すべてにおいて、PET上部キャリアを使用した。さらにこれらの実験すべてにおいて、プレミックスを冷蔵庫内で冷却した。
シリコーン発泡体を形成するために、シリコーン樹脂(Dow Corning Silicone 8137)と、表3に示したような充てん剤微小球と、シリコーン硬化抑制剤(Aldrich Chemical Co.製の1−オクチン−3−オール)とを、Flaktekスピードミキサ内で混ぜ合わせ、制御した厚さを有するPETフィルム上でキャストし、発泡体上に上部キャリアを設置した。この発泡体をオーブン内に設置し、調節可能な磁場へ暴露して発泡体を硬化させた。サンプルを機械的には発泡させなかった。加えて、発泡は磁場の印加後継続した。外層の除去は行わなかった。発泡体それぞれの検査は、発泡体の厚さが発泡体のセルの平均高さとほぼ同じであることを示していた。
表7に示すようにより厚い発泡体(25〜40ミル)も調製した。使用した充てん剤は、100%ニッケル球またはニッケル被覆鋼球で、全体に寸法がより大きかった(75〜150マイクロメートル、100〜150マイクロメートル、150〜177マイクロメートルまたは177〜200マイクロメートル)。充てん剤の使用量は、8、12および14(その表内に13%のレベルの例は見られない)体積パーセントであった。配合物を第一のPET剥離層上に厚さ7ミルの厚さまでキャストし、その上にPET上部キャリアを配置した。それら発泡体を指示した密度および継続時間の磁場にさらす一方、表7に示すように70℃で発泡させ硬化させた。
Claims (24)
- ポリマー発泡複合体を作製する方法であって、
前駆体組成物から、第一の表面および反対側の第二の表面を有する物品を形成するステップであって、前記前駆体組成物が、
ポリマー発泡前駆体組成物と、
複数の磁性導電性粒子を含む充てん剤組成物と
を含むステップと;
前記前駆体組成物を発泡させて、前記前駆体組成物中に複数のセルを形成するステップと;
前記発泡前駆体組成物に磁場を印加するステップであって、前記磁場が、前記物品の前記第一の表面と前記反対側の第二の表面との間で互いに孤立したチェーンへと前記導電性の磁性粒子を整列させるために有効な強度を有し、また有効な時間印加されるステップと;
前記ポリマー発泡前駆体組成物を凝固させて、約1〜約125ポンド/立方フィートの密度を有し、60ポンド/平方インチの圧力で約10-3ohm−cm〜約103ohm−cmの体積抵抗率を有する前記ポリマー発泡複合体を得るステップと
を含む方法。 - 前記発泡させるステップが、前記磁場を印加するステップの前に実質的に完了している請求項1に記載の方法。
- 前記発泡させるステップが、前記物品を形成するステップの前の機械的発泡によるものである請求項1〜2のいずれかに記載の方法。
- 前記凝固させるステップが、前記互いに孤立したチェーンへと前記導電性金属粒子を整列させるステップの後である請求項1〜3のいずれかに記載の方法。
- 前記凝固発泡体の前記第一および/または第二の表面を、前記互いに孤立したチェーンの端部を少なくとも部分的に露出させるのに十分な量を取り除くステップをさらに含む請求項1〜4のいずれかに記載の方法。
- 前記物品が層であり、物品を形成するステップが、第一のキャリア上で前記ポリマー発泡前駆体組成物をキャストするステップを含み、前記第一の表面が第一のキャリア上に接触して配置されている請求項1〜5のいずれかに記載の方法。
- 前記凝固発泡体の前記第一の表面を、前記互いに孤立したチェーンの端部を少なくとも部分的に露出させるのに十分な量を取り除くステップをさらに含む請求項1〜6のいずれかに記載の方法。
- 前記層の前記第二の表面上に第二のキャリアを配置するステップをさらに含む請求項1〜6のいずれかに記載の方法。
- 前記凝固発泡体の前記第一および第二の表面を、前記互いに孤立したチェーンの端部を少なくとも部分的に露出させるのに十分な量を取り除くステップをさらに含む請求項1〜8のいずれかに記載の方法。
- 前記第一のキャリアが導電性である請求項6のいずれかに記載の方法。
- 前記第一のキャリアが磁性を有する、または磁性と導電性とを有する請求項6のいずれかに記載の方法。
- 請求項1〜12のいずれかに記載の方法によって作製されるポリマー発泡複合体。
- ポリマー発泡複合体を作製する方法であって、
前駆体組成物を機械的に発泡させて、前記前駆体組成物中に複数のセルを形成するステップであって、前記前駆体組成物が、
ポリマー発泡前駆体組成物と、
複数の磁性導電性粒子を含む充てん剤組成物と
を含むステップと;
前記機械的に発泡させた前駆体組成物から第一の表面および反対側の第二の表面を有する物品を形成するステップと;
前記物品の前記第一の表面と前記反対側の第二の表面との間で互いに孤立したチェーンへと前記磁性導電性粒子を整列させるために有効な強度を有する磁場を、有効な時間印加するステップであって、前記発泡させるステップが、前記磁性導電性粒子の完全な整列前に実質的に完了しているステップと;
前記ポリマー前駆体組成物を硬化させて、約1〜約125ポンド/立方フィートの密度を有し、60ポンド/平方インチの圧力で約10-3ohm−cm〜約103ohm−cmの体積抵抗率を有する前記ポリマー発泡複合体を得るステップと
を含む方法。 - ポリマー発泡複合体を作製する方法であって、
前駆体組成物から第一の表面および反対側の第二の表面を有する物品を形成するステップであって、前記前駆体組成物が、
ポリマー発泡前駆体組成物と、
複数の磁性導電性粒子を含む充てん剤組成物と
を含むステップと;
前記前駆体組成物を発泡させて、前記前駆体組成物中に複数のセルを形成するステップと;
前記発泡前駆体組成物に磁場を印加するステップであって、前記磁場が、前記物品の前記第一の表面と前記反対側の第二の表面との間で互いに孤立したチェーンへと前記導電性の磁性粒子を整列させるために有効な強度を有し、また有効な時間印加されるステップと;
前記ポリマー発泡前駆体組成物を凝固させるステップと;
前記凝固発泡体の前記第一および/または第二の表面を、前記互いに孤立したチェーンの端部を少なくとも部分的に露出させるのに十分な量を取り除いて、約1〜約125ポンド/立方フィートの密度を有し、60ポンド/平方インチの圧力で約10-3ohm−cm〜約103ohm−cmの体積抵抗率を有する前記ポリマー発泡複合体を得るステップと
を含む方法。 - ポリウレタン発泡複合体を作製する方法であって、
ポリイソシアネート成分と、前記ポリイソシアネート成分と反応する活性水素含有成分と、界面活性剤と、触媒と、複数の磁性導電性粒子を含む充てん剤組成物とを含む前駆体組成物を機械的に発泡させてセルを形成するステップと;
前記発泡前駆体組成物をキャストして、第一の表面および反対側の第二の表面を有する層を形成するステップと;
前記層を磁場にさらして、前記第一の表面と前記第二の表面との間で本質的に連続的に前記層の橋渡しをする互いに孤立したチェーンへと前記磁性導電性粒子を整列させるステップであって、前記発泡させるステップが、前記磁場を印加するステップの前に実質的に完了しているステップと;
前記層を硬化させて、60ポンド/平方インチの圧力で約10-3ohm−cm〜約103ohm−cmの体積抵抗率を有する前記ポリウレタン発泡複合体を生成するステップであって、前記第一表面と前記第二の表面との間の距離が、前記セルの平均直径の1.5倍を超えているステップと
を含む方法。 - シリコーン発泡体を作製する方法であって、
水素化物置換基を有するポリシロキサンポリマーと、触媒と、複数の磁性導電性粒子を含む充てん剤組成物とを含む混合物をキャストして、第一の表面および反対側の第二の表面を有する層を形成するステップと;
前記混合物を発泡させるステップと;
印加磁場内で前記混合物を硬化させて、前記発泡体の第一の表面と第二の反対側の表面との間で本質的に連続的に前記発泡体の橋渡しをする互いに孤立したチェーンへと前記磁性導電性粒子を整列させるステップと;
前記硬化発泡体の前記第一および/または第二の表面を、前記互いに孤立したチェーンの端部を少なくとも部分的に露出させるのに十分な量を取り除いて、60ポンド/平方インチの圧力で約10-3ohm−cm〜約103ohm−cmの体積抵抗率を有する前記シリコーン発泡複合体を得るステップと
を含む方法。 - 前記磁性導電性粒子が高アスペクト比粒子であり、前記互いに孤立したカラムが、前記第一の表面と前記反対側の第二の表面とに間で本質的に連続的に前記層の橋渡しをする請求項1〜16のいずれかに記載の方法。
- 第一の表面および反対側の第二の表面を有するポリマー発泡体と、
前記発泡体の前記第一の表面と前記反対側の第二の表面との間で互いに孤立したチェーンへと整列された導電性磁性粒子と
を備えるポリマー発泡複合体であって;
前記発泡体が、
約1〜約125ポンド/立方フィートの密度と、
60ポンド/平方インチの圧力で約10-3ohm−cm〜約103ohm−cmの体積抵抗率と
を有するポリマー発泡複合体。 - 前記セルが、約65〜約1000マイクロメートルの平均直径を有する請求項18に記載のポリマー発泡複合体。
- 前記第一および第二の表面における前記互いに孤立したチェーンの端部が、少なくとも部分的に露出している請求項18〜19のいずれかに記載のポリマー発泡複合体。
- 前記ポリマー発泡複合体が、その第一の表面上に接触して配置されている導電性層を有する請求項18〜20のいずれかに記載のポリマー発泡複合体。
- 前記磁性導電性粒子が高アスペクト比粒子であり、前記互いに孤立したカラムが、前記第一の表面と前記反対側の第二の表面との間で本質的に連続的に前記層の橋渡しをする請求項18〜22のいずれかに記載のポリマー発泡複合体。
- 前記高アスペクト比粒子が、約2〜約100の長さ対幅比を有する請求項22に記載のポリマー発泡複合体。
- 前記互いに孤立したカラムのそれぞれが、1〜5個の磁性導電性高アスペクト比粒子の孤立したチェーンからなる請求項22〜23のいずれかに記載のポリマー発泡複合体。
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US12/404,566 US20090226696A1 (en) | 2008-02-06 | 2009-03-16 | Conductive Polymer Foams, Method of Manufacture, And Uses Thereof |
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- 2009-07-27 DE DE200910034901 patent/DE102009034901A1/de not_active Withdrawn
- 2009-07-30 GB GB0913320A patent/GB2462356B/en not_active Expired - Fee Related
- 2009-08-04 JP JP2009181437A patent/JP5619388B2/ja not_active Expired - Fee Related
- 2009-08-04 CN CN2009101590537A patent/CN101643550B/zh not_active Expired - Fee Related
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2011144298A (ja) * | 2010-01-15 | 2011-07-28 | Fujifilm Corp | アゾ顔料の製造方法、顔料分散物、着色組成物、インクジェット記録用インクの調製方法、カラーフィルター用着色組成物及びカラーフィルター |
JP2016205923A (ja) * | 2015-04-20 | 2016-12-08 | 東洋ゴム工業株式会社 | 変形検出センサおよびその製造方法 |
KR101670788B1 (ko) | 2015-07-21 | 2016-10-31 | 한국생산기술연구원 | 족압 수집용 인솔 |
WO2018079655A1 (ja) * | 2016-10-27 | 2018-05-03 | 株式会社エンプラス | 異方導電性シート及びその製造方法 |
US10720398B2 (en) | 2016-10-27 | 2020-07-21 | Enplas Corporation | Anisotropic conductive sheet and method for manufacturing the same |
Also Published As
Publication number | Publication date |
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JP5619388B2 (ja) | 2014-11-05 |
GB2462356A (en) | 2010-02-10 |
US20090226696A1 (en) | 2009-09-10 |
GB2462356B (en) | 2013-03-27 |
DE102009034901A1 (de) | 2010-03-25 |
GB0913320D0 (en) | 2009-09-02 |
CN101643550B (zh) | 2013-03-20 |
CN101643550A (zh) | 2010-02-10 |
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