JP5986187B2 - マクロ多孔性チタン化合物モノリスとその製造方法 - Google Patents
マクロ多孔性チタン化合物モノリスとその製造方法 Download PDFInfo
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Description
本発明のマクロ多孔性酸素欠損型酸化チタンモノリス(以下、酸素欠損モノリス)の製造方法では、前駆体であるマクロ多孔性二酸化チタンモノリス(以下、二酸化モノリス)と、チタン還元能を有する金属とを使用する。
(1)骨格内および/または骨格の表面に粒子が配置された二酸化モノリスに対して上記気相還元を実施することで、骨格内および/または骨格の表面に粒子が配置された酸素欠損モノリスを得る方法;
(2)骨格内および/または骨格の表面に粒子前駆体が配置された二酸化モノリスに対する上記気相還元の実施を経て、骨格内および/または骨格の表面に粒子が配置された酸素欠損モノリスを得る方法;および
(3)二酸化モノリスに対する上記気相還元の実施により酸素欠損モノリスを得た後に、得られた酸素欠損モノリスの骨格内および/または骨格の表面に粒子を配置する方法;を含む。(1)、(2)、(3)のいずれの方法も、カーボン粒子の配置および金属粒子の配置に適用できる。(1)の方法において、二酸化モノリス内にカーボン粒子を配置した場合においても、上記気相還元の進行により、カーボン粒子による二酸化モノリス骨格からの酸素の引き抜き(カーボン粒子の酸化)が抑えられる。このため、単相の酸素欠損モノリスを得ることができる。
本発明の酸素欠損モノリスは、単相の(単一の結晶相)の酸素欠損型酸化チタンから構成される骨格とマクロ孔との共連続構造を有し、酸素欠損型酸化チタンに基づく電子伝導性を有する。この共連続構造は、上述のように、マクロ孔の直径の均一性が高く、孤立孔を有さない。酸素欠損型酸化チタンは、例えば、式TinO2n−1(nは2,3,4または6)により示される酸化チタンである。電子伝導性の程度は、当該モノリスの骨格を構成する酸素欠損型酸化チタン自体の物性による。電気抵抗率は、例えば103Ω・cm以下であり、常温において103Ω・cm以下であることが好ましく、当該モノリスの骨格を構成する酸素欠損型酸化チタンの組成および温度域によっては、例えば102Ω・cm以下、10Ω・cm以下、1Ω・cm以下、さらには10−1Ω・cm以下となる。
本発明のマクロ多孔性酸窒化チタンモノリス(以下、酸窒化モノリス)の製造方法では、前駆体である二酸化モノリスまたは酸素欠損モノリスと、金属窒化物とを使用する。
本発明の酸窒化モノリスは、酸窒化チタンから構成される骨格とマクロ孔との共連続構造を有し、酸窒化チタンに基づく電子伝導性を有する。この共連続構造は、上述のように、マクロ孔の直径の均一性が高く、孤立孔を有さない。電子伝導性の程度は、当該モノリスの骨格を構成する酸窒化チタン自体の物性による。
本発明のマクロ多孔性窒化チタンモノリス(以下、窒化モノリス)の製造方法では、前駆体である二酸化モノリス、酸素欠損モノリスまたは酸窒化モノリスと、アンモニアとを使用する。
本発明の窒化モノリスは、窒化チタンから構成される骨格とマクロ孔との共連続構造を有し、窒化チタンに基づく電子伝導性を有する。この共連続構造は、上述のように、マクロ孔の直径の均一性が高く、孤立孔を有さない。電子伝導性の程度は、当該モノリスの骨格を構成する窒化チタン自体の物性による。
前駆体である二酸化モノリスを、George Hasegawa et al.文献に開示の方法に従って作製した。具体的には、以下の手順で作製した。
上記のように作製した二酸化モノリスAから酸素欠損モノリスを作製した。具体的には、以下の手順で作製した。
乾燥ゲルの焼成温度を800℃とした以外は上述した前駆体モノリスの作製方法に従って、二酸化モノリスBを得た。この二酸化モノリスBに対して、SEMによる観察、水銀圧入法による細孔分布測定、および骨格を構成する材料のXRD回折ピークの評価を行った。図7Aに、二酸化モノリスBの骨格を構成する材料のXRD回折ピークを示す。図7Aにおいて、「TiO2」と示されているものが、二酸化モノリスBに対する結果である。なお、図7Aにおいて、2つの破線のうち下方の破線はルチル型TiO2の理論上の回折ピーク、実線は二酸化モノリスBおよび当該モノリスを気相還元して得た酸素欠損モノリスに対して実際に測定された回折ピークである。これらの評価結果から、二酸化モノリスBがルチル型二酸化チタンから構成される骨格とマクロ孔との共連続構造を有するマクロ多孔性モノリスであること、二酸化モノリスAと同様に、二酸化モノリスBにおけるマクロ孔の直径の均一性が高いことが確認された。
上記のように作製した二酸化モノリスAから、酸窒化モノリスを作製した。具体的には、以下の手順で作製した。
上記のように作製した二酸化モノリスAから、窒化モノリスを作製した。具体的には、以下の手順で作製した。
カーボン粒子が骨格内および骨格の表面に配置された二酸化モノリスから、カーボン粒子が骨格内および骨格の表面に配置された酸素欠損モノリスを作製した。具体的には、以下の手順で作製した。
実施例6では、マクロ多孔性モノリスの電極としての使用を考慮し、電気化学的な当該モノリスの安定性、および当該モノリスの電極としての具体的な応用を確認した。実施例6における、マクロ多孔性モノリスにより構成される電極(以下、モノリス電極)の電気化学特性は、ポテンショスタット/ガルバノスタット(北斗電工社製、HSV−110)および三極式セルを用いて評価した。
白金粒子を担持させたTi4O7モノリス電極の硫酸電解液(濃度0.1mol/L)中におけるCV曲線を図19に示す。CVの評価は、白金担持モノリス電極を作用極に配置し、対極に白金線を、参照極にAg/AgCl参照電極(ALS社製)をそれぞれ使用して、三極式セルにおいて実施した。カットオフ電位は−0.7Vから2.0Vとした。図19に示すように、モノリスに担持された白金粒子による触媒作用により、およそ1.5V以上の電位で酸素の発生に起因する電流が、およそ−0.3V以下の電位で水素の発生に起因する電流が流れることが確認された。
白金を担持させたTi4O7モノリス電極のメタノール硫酸水溶液(メタノール濃度1.0mol/L、硫酸濃度0.1mol/L)中におけるリニアスイープボルタンメトリー(LSV)曲線を図20に示す。LSVの評価は、白金担持モノリス電極を作用極に配置し、対極に白金線を、参照極にAg/AgCl参照電極(ALS社製)をそれぞれ使用して、三極式セルにおいて実施した。走査は0.40Vから1.30Vまでとした。比較のために、白金担持前のTi4O7モノリスを参照極に使用した対比実験を併せて実施した。評価結果を図20に示す。図20において、実線が白金担持モノリス電極のLSV曲線を示し、点線が白金粒子を担持していないモノリス電極のLSV曲線を示す。
Claims (19)
- 単相の酸素欠損型酸化チタンから構成される骨格とマクロ孔との共連続構造を有し、
前記酸素欠損型酸化チタンに基づく電子伝導性を有するマクロ多孔性チタン化合物モノリス。 - 電気抵抗率が103Ω・cm以下である、請求項1に記載のマクロ多孔性チタン化合物モノリス。
- カーボン粒子および/または金属粒子が、前記骨格内および/または前記骨格の表面に配置されている、請求項1に記載のマクロ多孔性チタン化合物モノリス。
- 電極である、請求項1に記載のマクロ多孔性チタン化合物モノリス。
- 二酸化チタンから構成される骨格とマクロ孔との共連続構造を有するマクロ多孔性二酸化チタンモノリスと、チタン還元能を有する金属と、を容器に収容し、
前記容器内を真空雰囲気または不活性ガス雰囲気とし、
前記モノリスおよび前記金属を加熱することで、前記金属を酸素ゲッターとして、前記モノリスを構成する二酸化チタンから酸素原子を奪う気相還元を行って、
酸素欠損型酸化チタンから構成される骨格と前記マクロ孔との共連続構造を有し、前記酸素欠損型酸化チタンに基づく電子伝導性を有するマクロ多孔性酸素欠損型酸化チタンモノリスを得る、マクロ多孔性チタン化合物モノリスの製造方法。 - 箔状の前記金属を前記容器に収容する請求項5に記載のマクロ多孔性チタン化合物モノリスの製造方法。
- 前記金属がジルコニウム(Zr)およびハフニウム(Hf)から選ばれる少なくとも1種である請求項5に記載のマクロ多孔性チタン化合物モノリスの製造方法。
- 前記加熱の温度が900〜1300℃である請求項7に記載のマクロ多孔性チタン化合物モノリスの製造方法。
- 前記マクロ多孔性二酸化チタンモノリスの骨格を構成する二酸化チタンがアナターゼ型である請求項5に記載のマクロ多孔性チタン化合物モノリスの製造方法。
- 酸窒化チタンから構成される骨格とマクロ孔との共連続構造を有し、
前記酸窒化チタンに基づく電子伝導性を有するマクロ多孔性チタン化合物モノリス。 - 二酸化チタンまたは酸素欠損型酸化チタンから構成される骨格とマクロ孔との共連続構造を有するマクロ多孔性チタン化合物モノリスと、金属窒化物と、を容器に収容し、
前記容器内を真空雰囲気または不活性ガス雰囲気とし、
前記モノリスおよび前記金属窒化物を加熱することで、前記金属窒化物を酸素ゲッターおよび窒素供給源として、前記モノリスを構成するチタン化合物から酸素原子を奪うとともに窒素原子を供給する気相還元を行って、
酸窒化チタンから構成される骨格と前記マクロ孔との共連続構造を有し、前記酸窒化チタンに基づく電子伝導性を有するマクロ多孔性酸窒化チタンモノリスを得る、マクロ多孔性チタン化合物モノリスの製造方法。 - 粉末状の前記金属窒化物を前記容器に収容する請求項11に記載のマクロ多孔性チタン化合物モノリスの製造方法。
- 前記金属窒化物が、窒化チタン、窒化ジルコニウムおよび窒化ハフニウムから選ばれる少なくとも1種である請求項11に記載のマクロ多孔性チタン化合物モノリスの製造方法。
- 前記加熱の温度が950〜1200℃である請求項13に記載のマクロ多孔性チタン化合物モノリスの製造方法。
- 二酸化チタンから構成される骨格と前記マクロ孔との共連続構造を有するマクロ多孔性二酸化チタンモノリスと、前記金属窒化物と、を前記容器に収容する請求項11に記載のマクロ多孔性チタン化合物モノリスの製造方法。
- 窒化チタンから構成される骨格とマクロ孔との共連続構造を有し、
前記窒化チタンに基づく電子伝導性を有するマクロ多孔性チタン化合物モノリス。 - 二酸化チタン、酸素欠損型酸化チタンまたは酸窒化チタンから構成される骨格とマクロ孔との共連続構造を有するマクロ多孔性チタン化合物モノリスを、アンモニアを含む雰囲気においてアンモニアの熱分解温度以上で熱処理して、前記モノリスを構成するチタン化合物から酸素原子を奪うとともに窒素原子を供給する気相還元を行って、
窒化チタンから構成される骨格と前記マクロ孔との共連続構造を有し、前記窒化チタンに基づく電子伝導性を有するマクロ多孔性窒化チタンモノリスを得る、マクロ多孔性チタン化合物モノリスの製造方法。 - 前記熱処理の温度が1000℃以上である請求項17に記載のマクロ多孔性チタン化合物モノリスの製造方法。
- 二酸化チタンから構成される骨格と前記マクロ孔との共連続構造を有するマクロ多孔性二酸化チタンモノリスを、アンモニアを含む雰囲気においてアンモニアの熱分解温度以上で熱処理する請求項17に記載のマクロ多孔性チタン化合物モノリスの製造方法。
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