JP5620110B2 - 導電性ポリマー発泡体、その作製方法、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、およびその使用 Download PDFInfo
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- JP5620110B2 JP5620110B2 JP2009549094A JP2009549094A JP5620110B2 JP 5620110 B2 JP5620110 B2 JP 5620110B2 JP 2009549094 A JP2009549094 A JP 2009549094A JP 2009549094 A JP2009549094 A JP 2009549094A JP 5620110 B2 JP5620110 B2 JP 5620110B2
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Images
Classifications
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- 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
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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Description
この出願は、2007年2月6日に出願された米国出願番号60/888360の内容をすべて援用し、その利益を主張する。
本開示は、導電性ポリマー、その作製方法、およびそのポリマーを含む物品に関する。
本明細書には、ポリマー発泡体層であって、第一の表面および反対側の第二の表面と;前記ポリマー発泡体層の前記第一の表面および前記反対側の第二の表面の間にある複数のセルであって、前記第一の表面および前記反対側の第二の表面の間の前記ポリマー発泡体層の厚さが、前記複数のセルの平均高さの1.0〜1.5倍であるセルと;前記ポリマー発泡体層の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互いに孤立したチェーンへと整列された複数の磁性導電性粒子とを含む層が開示されている。
図1は、導電性ポリマー発泡体の一例の概観図である。
本発明者等は、意外にも、ポリマー発泡体において導電性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導電性を付与することが可能であることを発見した。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。発泡体中のセルの平均直径が発泡体層の厚さの平均に近づいたとき、即ち、発泡体層の厚さが発泡体中のセルの平均高さの1.0〜1.5倍であるときに、導電性の改善が達成されることがわかった。さらなる予期せぬ特徴では、ポリマー発泡体の物理的性質に実質的には悪影響を及ぼすことなく、このような導電性を実現することができる。したがって、一実施形態においては、導電性を有し、またそれらポリマー発泡体の圧縮性、可とう性、耐圧縮永久ひずみ性、セル均一性等のうちの1つまたは複数も実質的に保持するポリマー発泡体が製造される。これらの材料は、EMIおよび/またはRFIから守ることができる物品の形成における使用に特に適している。
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(すなわち、アルキレンまたはアリーレン基)であってよく、または式Q1−Z−Q1の基(Q1は、アルキレンまたはアリーレン基であり、Zは、−O−、−O−Q1−S、−CO−、−S−、−S−Q1−S−、−SO−、−SO2−、アルキレンまたはアリーレン)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シールド効果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3で得られた結果に基づいて、追加の発泡体セットを配合し、表4Aに示す試験を実施した。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。
表5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5に示すように70℃で発泡させ硬化させた。
Claims (29)
- ポリマー発泡体層であって、
第一の表面および反対側の第二の表面と;
前記ポリマー発泡体層の前記第一の表面および前記反対側の第二の表面の間にある複数のセルであって、前記第一の表面および前記反対側の第二の表面の間の前記ポリマー発泡体層の厚さが、前記複数のセルの平均高さの1.0〜1.5倍であるセルと;
前記ポリマー発泡体層の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互いに孤立したチェーンへと整列された複数の磁性導電性粒子と
を含む層。 - 前記粒子が、磁性と導電性の両者を備えた材料から形成されてなる請求項1に記載の層。
- 前記磁性導電性粒子が、ニッケル、コバルト、鉄、またはこれらの金属の少なくともひとつを含む組み合わせである請求項1に記載の層。
- 前記粒子が、ニッケル、またはニッケルと銀との組み合わせである請求項1に記載の層。
- 前記粒子が、ニッケル被覆鉄粒子、銀被覆ニッケル粒子、またはこれらの粒子の少なくともひとつを含む組み合わせである請求項1に記載の層。
- 前記ポリマー発泡体層が、前記磁性導電性粒子を含む発泡体用前駆体配合物を発泡させることにより得られ、前記磁性導電性粒子が、前記発泡前の発泡体用前駆体配合物の1〜30体積%の割合で配合されている請求項1に記載の層。
- 前記磁性導電性粒子の平均直径が、20〜300μmである請求項1に記載の層。
- 前記チェーンが、前記ポリマー発泡体層の前記第一の表面と前記第二の表面に対して本質的に垂直である請求項1に記載の層。
- 前記チェーンが、前記ポリマー層の前記第一と第二の表面に垂直な軸に対して、相対的に5〜45度の角度を有する請求項1に記載の層。
- 前記粒子が、前記ポリマー発泡体の表面から突出していない請求項1に記載の層。
- 前記ポリマー発泡体が、ポリウレタン発泡体、シリコーン発泡体、またはこれらの発泡体の少なくともひとつを含む組み合わせである請求項1に記載の層。
- 前記ポリマー発泡体層が、50dB以上の電磁気シールド能を有する請求項1に記載の層。
- 前記ポリマー発泡体層が、圧力689キロパスカルにおいて10 -3ohm−cm〜10 3ohm−cmの体積抵抗率を有する請求項1に記載の層。
- 前記ポリマー発泡体層が、ASTM1056に従って測定された25%撓みにおいて、0.007〜10.5kg/cm2の圧縮力撓み値を有する請求項1に記載の層。
- 前記発泡体が、化学的および/または物理的にブローされた請求項1に記載の層。
- 前記第一の表面および前記反対側の第二の表面の間の前記ポリマー発泡体層の厚さが、前記複数のセルの平均高さの1.0〜1.3倍である請求項1に記載の層。
- 各カラムが、2〜12個の導電性粒子の独立したチェーンで構成されてなる請求項1に記載の層。
- 各カラムが、3〜8個の導電性粒子の独立したチェーンで構成されてなる請求項1に記載の層。
- ポリマー発泡体層を作製する方法であって、
第一の表面および反対側の第二の表面を持つ層を形成するステップであって、前記層が、
ポリマー発泡体前駆体組成物と
複数の磁性導電性粒子を含有するフィラー組成物と
を含むステップと;
前記発泡体前駆体組成物を発泡させて、前記層中に複数のセルを形成するステップと;
前記層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、有効な時間層に印加するステップと;
前記発泡された層を硬化するステップであって、前記硬化された層の厚さが、前記硬化された層中の前記複数のセルの平均高さの1.0〜1.5倍であるステップと
を含む方法。 - 前記印加される磁束密度が、100〜1500ガウスである請求項19に記載の方法。
- 前記磁場が、前記組成物の発泡の間印加される請求項19に記載の方法。
- 前記磁場が、前記層を硬化する前に印加される請求項19に記載の方法。
- 前記層を完全に硬化させる前に前記層を部分的に硬化させるステップであって、前記磁場が、前記層を部分的に硬化させた後に前記磁場が印加されるステップをさらに含む請求項19に記載の方法。
- 前記層を形成するステップが、第一のキャリア支持体の上に前記層をキャストするステップをさらに含む請求項19に記載の方法。
- 前記第一のキャリア支持体の反対側の前記層の上に、第二のキャリア支持体を配置するステップをさらに含む請求項24に記載の方法。
- シリコーン発泡体を作製する方法であって、
ハイドライド置換基を有するポリシロキサンポリマー、発泡剤、白金系触媒、および複数の磁性導電性粒子を含有する充填剤組成物を含有する混合物を押し出すステップと;
印加された磁場中で前記混合物をブローおよび硬化して、前記発泡体の第一の表面と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、前記発泡体の厚さが、前記硬化された層中の前記複数のセルの平均高さの1.0〜1.5倍であるステップと
を含む方法。 - ポリマー発泡体を作製する方法であって、
ハイドライド置換基を有するポリシロキサンポリマー、発泡剤、白金系触媒、および複数の磁性導電性粒子を含有する組成物を、モールドまたは連続被覆ラインに輸送および/またはキャストするステップと;
前記組成物を発泡させて、第一の表面および反対側の第二の表面を有する発泡体を得るステップと;
前記発泡体を磁場にさらして、前記発泡体の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、前記発泡体の厚さが、前記硬化された層中の前記複数のセルの平均高さの1.0〜1.5倍であるステップと
を含む方法。 - 請求項1に記載の発泡体層を含む物品。
- 電磁気シールド用のガスケット、接地パッド(grounding pad)、または電池接点用導電性バネ素材(battery contact conductive spring elements)の形状を有する請求項28に記載の物品。
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- 2008-02-06 CN CN2008800039841A patent/CN101600758B/zh not_active Expired - Fee Related
- 2008-02-06 WO PCT/US2008/001564 patent/WO2008097571A1/en active Application Filing
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- 2008-02-06 JP JP2009549093A patent/JP2010518227A/ja active Pending
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- 2008-02-06 GB GB0911839A patent/GB2458067B/en not_active Expired - Fee Related
- 2008-02-06 US US12/027,018 patent/US7815998B2/en not_active Expired - Fee Related
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Also Published As
Publication number | Publication date |
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CN101600758A (zh) | 2009-12-09 |
US7875345B1 (en) | 2011-01-25 |
DE112008000327T5 (de) | 2009-12-31 |
GB2458067A (en) | 2009-09-09 |
GB0911838D0 (en) | 2009-08-19 |
WO2008097570A2 (en) | 2008-08-14 |
GB2458067B (en) | 2011-10-05 |
GB2458066B (en) | 2011-10-05 |
CN101605842B (zh) | 2012-07-04 |
CN101600758B (zh) | 2012-07-04 |
WO2008097570A3 (en) | 2008-10-02 |
US20110006267A1 (en) | 2011-01-13 |
CN101605842A (zh) | 2009-12-16 |
GB0911839D0 (en) | 2009-08-19 |
US7815998B2 (en) | 2010-10-19 |
GB2458066A (en) | 2009-09-09 |
WO2008097571A1 (en) | 2008-08-14 |
DE112008000326T5 (de) | 2010-02-11 |
JP2010518228A (ja) | 2010-05-27 |
JP2010518227A (ja) | 2010-05-27 |
US20080213565A1 (en) | 2008-09-04 |
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