JP5965395B2 - 複合体の調製法、得られる複合体及びその用途 - Google Patents
複合体の調製法、得られる複合体及びその用途 Download PDFInfo
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- JP5965395B2 JP5965395B2 JP2013517378A JP2013517378A JP5965395B2 JP 5965395 B2 JP5965395 B2 JP 5965395B2 JP 2013517378 A JP2013517378 A JP 2013517378A JP 2013517378 A JP2013517378 A JP 2013517378A JP 5965395 B2 JP5965395 B2 JP 5965395B2
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- 229910002601 GaN Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 101000617738 Homo sapiens Survival motor neuron protein Proteins 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 102100021947 Survival motor neuron protein Human genes 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
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- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 150000001449 anionic compounds Chemical class 0.000 description 1
- 125000003435 aroyl group Chemical group 0.000 description 1
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- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000002079 double walled nanotube Substances 0.000 description 1
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- ZOZZQPFBMNNPPO-UHFFFAOYSA-N ethyl-dimethyl-propylazanium Chemical compound CCC[N+](C)(C)CC ZOZZQPFBMNNPPO-UHFFFAOYSA-N 0.000 description 1
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- 229910052731 fluorine Inorganic materials 0.000 description 1
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- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
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- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
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- 229910001412 inorganic anion Inorganic materials 0.000 description 1
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- 229920000329 polyazepine Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
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- 150000003254 radicals Chemical class 0.000 description 1
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- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- MWNQXXOSWHCCOZ-UHFFFAOYSA-L sodium;oxido carbonate Chemical compound [Na+].[O-]OC([O-])=O MWNQXXOSWHCCOZ-UHFFFAOYSA-L 0.000 description 1
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- 241000894007 species Species 0.000 description 1
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- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- H01G11/22—Electrodes
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
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Description
−単壁ナノチューブ(SWNT)は、単一層のグラフェンのみが存在する場合に使用される;
−二重壁ナノチューブ(DWNT)は2層のグラフェンの存在するときに使用される;
−多重壁ナノチューブ(MWNT)は数層のグラフェンの存在するときに使用される。
a)電導性又は半導体性の伸張形状のナノ物体、とりわけ前記定義のものと当該伝導性ポリマーマトリックスのモノマー(類)前駆体(類)含有の溶液(以下溶液(S)と命名)とを接触させる工程;
b)当該ナノ物体をパルスガルバノスタットモードで分極し、その後に当該伝導性ポリマーマトリックスをナノ物体に電気化学的に析出させる工程。
−プラズマ処理などの物理的処理、とりわけ、酸素プラズマ、UV処理、X−線もしくはγ−線処理、電子及び重イオン照射処理;又は
−化学処理、例えば、アルコール性カリによる処理、強酸(HCl、H2SO4、HNO3、HClO4)での処理、水酸化ナトリウムでの処理、強酸化剤(KMnO4、K2Cr2O7、KClO3又はCrO3/塩酸、硫酸又は硝酸中)、オゾン処理及び酸素化気体(O2、H2Oなど)中での熱処理。
図1に図式化した本発明方法に使用する装置は、3つの電極をもつ電気化学セルを含んでなる。
先に説明したように、本発明による方法の不可欠の特徴は、溶液(S)中に存在するモノマーから得られるポリマーを析出させるための作用電極上での連続するガルバノスタットモードの使用である。
3.1.静電容量値に対する<ナノ構造化>効果の証明
サイクリックボルタンメトリー(CV)での検討を実施した(図3)。例えば、これらの検討では、ナノ複合体に相当する曲線下面積が、2つの他の曲線、すなわち、P3MTポリマーの曲線とCNT単独の曲線の面積の合計よりも大きいことを示すことができた。
カーペットの厚さに対する、EDXプローブによるイオウ元素の分布測定によって、P3MTポリマーが整列したチューブの全長に沿って存在することを証明し得た。逆に、連続的ガルバノスタットモードにおいては、該ポリマーが、パルスガルバノスタットモードを使用することの有益性を明瞭に示すカーペットの全長に沿って浸透していない。
静電容量は一定の電流密度で充電/放電サイクルを実施することにより測定した。図5は、J=10mA/cm2(図5A)及びJ=5mA/cm2(図5B)での2つの例を示すが、これらの値はしばしば電気化学貯蔵での応用に使用される。
P3MTに関して、析出量は、試料の可能性のあるリフトオフに大きな影響をもつ(本発明の特性の一つ)。
検討したパラメータは以下のとおりであった:
−電流密度:このものは伝導性ポリマーの析出物の割合に、また従って、その質に影響をもつ。
−パルス回数:これは所定の密度に対して析出物の厚さを制御する。
−パルスの形状:静止時間は析出物の質に対する効果的な影響因子であり得る。
パルスに適用される電流密度は材料の性質にとって重要な因子である。検討は3種の異なる電流密度:2;3;4mA/cm2で、同じパルス回数と1つの同じ印加電荷量を用いて実施した。
図7に示すように、2mA/cm2で析出させた層(図7A)は、4mA/cm2で析出させた層(図7B)と対照的に、高密度かつ均一である。図7A及び7Bを大きく拡大した図面が、それぞれ図7C及び7Dであり、図7Dの試料の表面にうねりを明示している。重合の動力学は4mA/cm2でより急速であるため、より多孔性の構造が得られる。
これら2つのパラメータは互いに分離することが困難である。異なる合成法に由来するもののみならず、1つの同じ合成法に由来する試料も、CNTの合成に使用されるチューブ状石英反応器中の異なる点に位置するので、それぞれが異なるCNTの長さを有する、
静止時間:
十分な静止時間での電解重合に際し、到達する電位は、最初は低下し、次いで合成を通じて略一定のままとなる。到達した電位は電極で生成させたポリマーの酸化電位の特性である(図11A)。
パルス時間の影響に関しては、これを図12及び13にて説明する。
その他のモノマーを用いて、CNTの長いカーペットから、その上に相当するポリマーを析出させることにより、本発明によるナノ複合体を調製した。
これらのポリマーは以下のとおりであった:
式:
式:
式:
式:
式:
Claims (13)
- 電導性又は半導体性の伸張形状ナノ物体及び電導性ポリマーマトリックスを含んでなり、当該電導性又は半導体性の伸長形状ナノ物体が、ナノ物体を整列させたカーペットの形状である複合材料の調製方法であって、パルスガルバノスタット法により、当該ナノ物体上に当該マトリックスを電気化学的に析出させることからなる工程を含んでなる方法。
- 当該電導性又は半導体性の伸張形状ナノ物体が、ナノファイバー、ナノチューブ及びナノワイヤーから選択されることを特徴とする請求項1記載の方法。
- 当該電導性又は半導体性の伸長形状ナノ物体が、炭素、ケイ素、金、銀、タンタル、ニッケル、白金、銅、モリブデン、パラジウム、鋼鉄、ステンレス鋼、亜鉛、窒化ホウ素、酸化亜鉛、酸化マンガン、窒化ガリウム、窒化ケイ素、二硫化タングステン、二硫化モリブデン、リン化インジウム、セレン化タングステン、セレン化モリブデン、二酸化チタン、二酸化ケイ素、三酸化モリブデン、及びそれらの混合物からなる群より選択される材料にあることを特徴とする請求項1又は2に記載の方法。
- 当該電導性ポリマーマトリックスが、ポリフルオレン、ポリピレン、ポリアズレン、ポリナフタレン、ポリピロール、ポリカルバゾール、ポリインドール、ポリアゼピン、ポリアニリン、ポリチオフェン、ポリ(p−フェニレンスルフィド)、ポリアセチレン及びポリ(p−フェニレンビニレン)から選択される1種(又はそれ以上)の(コ)ポリマー(類)から形成されることを特徴とする請求項1〜3のいずれかに記載の方法。
- 該パルスガルバノスタット法においては、定電流密度が10〜100秒間の継続時間の期間(ton)加えられることを特徴とする請求項1〜4のいずれかに記載の方法。
- 該パルスガルバノスタット法においては、各静止期間(toff)の継続時間の、定電流密度の各適用期間(ton)の継続時間に対する比が、2以上であることを特徴とする請求項1〜5のいずれかに記載の方法。
- 当該方法が、
a)電導性又は半導体性の伸張形状のナノ物体と当該伝導性ポリマーマトリックスのモノマー(類)前駆体(類)含有の溶液(以下溶液(S)と命名)とを接触させる工程;
b)当該ナノ物体をパルスガルバノスタットモードで分極し、その後に当該伝導性ポリマーマトリックスを当該ナノ物体に電気化学的に析出させる工程;
を含んでなることを特徴とする請求項1〜6のいずれかに記載の方法。 - 当該工程(a)に先立って、電導性又は半導体性の伸張形状のナノ物体を酸化処理に付すことを特徴とする請求項7記載の方法。
- 当該溶液(S)が、純粋なプロトン性もしくは非プロトン性溶媒の形状;溶媒としてプロトン性もしくは非プロトン性溶媒を含む電解液の形状;又はイオン性液体の形状であることを特徴とする請求項7又は8に記載の方法。
- 当該複合材料において、当該電導性もしくは半導体性の伸長形状のナノ物体が、伝導性ポリマーマトリックスで含浸された、整列したナノ物体のカーペットの形状であり、当該ナノ物体がカーペット形状のカーボンナノチューブであり、それらの長さが200μmを超えることを特徴とする請求項1〜9のいずれかに記載の方法。
- 当該複合材料が自立性であり、かつ柔軟性であることを特徴とする請求項10記載の方法。
- 当該複合材料が、スーパーコンデンサ又はバッテリーの正極/負極、光電装置用の電極及び電気化学センサ用の電極からなる群より選択される電極に使用されることを特徴とする、請求項10又は11に記載の方法。
- 当該複合材料がCO 2 貯蔵用の材料に使用されることを特徴とする、請求項10又は11に記載の方法。
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US8518405B2 (en) | 2009-10-08 | 2013-08-27 | The University Of North Carolina At Charlotte | Tumor specific antibodies and uses therefor |
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FR2980982B1 (fr) | 2011-10-07 | 2014-10-24 | Commissariat Energie Atomique | Dispositif comprenant un materiau composite presentant des nanotubes soumis a un champ electrique et ses utilisations |
JP6476627B2 (ja) * | 2013-07-24 | 2019-03-06 | 三菱ケミカル株式会社 | 非水系二次電池負極用活物質並びにそれを用いた負極及び非水系二次電池 |
FR3018046A1 (fr) | 2014-02-28 | 2015-09-04 | Commissariat Energie Atomique | Procede de preparation d'une suspension contenant des nanotubes de carbone et suspension stable ainsi obtenue |
US11554181B2 (en) | 2014-09-05 | 2023-01-17 | The University Of North Carolina At Charlotte | Tumor specific antibody conjugates and uses therefor |
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FR3064812B1 (fr) | 2017-04-03 | 2022-06-24 | Nawatechnologies | Procede de fabrication de condensateurs electrochimiques |
FR3068823B1 (fr) | 2017-07-07 | 2020-01-24 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Procede de preparation d'une electrode comprenant un support, des nanotubes de carbone alignes et un oxyde metallique depose par voie reductrice, ladite electrode et ses utilisations. |
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