JP2007290936A - 改質黒鉛、その改質黒鉛を用いる黒鉛層間化合物及び触媒並びにそれらの製造方法。 - Google Patents
改質黒鉛、その改質黒鉛を用いる黒鉛層間化合物及び触媒並びにそれらの製造方法。 Download PDFInfo
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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- Carbon And Carbon Compounds (AREA)
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- Electric Double-Layer Capacitors Or The Like (AREA)
- Inert Electrodes (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
【解決手段】比表面積が200〜1000m2/g 、ラマンスペクトルのDバンド(1350cm−1)とGバンド(1580cm−1)のピーク強度比であるR値が0.3〜0.7、およびX線回折法の(002)面のc軸方向の結晶子の大きさLc(002)が30nm以上であることを特徴とする改質黒鉛。前記改質黒鉛を用いる金属塩化物がインターカレートされてなる黒鉛層間化合物及び触媒並びにそれらの製造方法とする。
【選択図】なし
Description
本発明に係る改質黒鉛は、黒鉛粒子表面が高比表面積からなる黒鉛構造に改質された結果、比表面積が200〜1000m2/g 、ラマンスペクトルのDバンド(1350cm−1)とGバンド(1580cm−1)のピーク強度比であるR値が0.3〜0.7、およびX線回折法の(002)面のc軸方向の結晶子の大きさLc(002)が30nm以上であることを特徴とする。
〈改質黒鉛の調整方法1〉
粉砕原料粉として鱗片状天然黒鉛(粒径16μm)33gを容積450cm3のスチール製ポットに仕込み、振動ボールミル(SUS製ボール4.5mmφまたは1mmφ、振動振幅5mm、振動数1200Hz)で粉砕した。粉砕の条件は、10−3Torrの真空雰囲気中で、粉砕時間0.5〜96時間の範囲とした。さらに、粉砕生成物の一部は、窒素雰囲気中で1500℃の温度で1時間、焼成処理を行った。
粉砕原料粉として鱗片状天然黒鉛(粒径16μm)30gを容積450cm3のスチール製ポットに仕込み、遊星ボールミル(ジルコニア製ボール4mmφから0.2mmφ、自転400rpm、公転400rpm)で粉砕した。粉砕の条件は、10−3Torrの真空雰囲気中で、粉砕時間0.5〜24時間の範囲とした。
1)溶媒法による合成方法
原料粉である黒鉛を約5g、真空容器内に入れた後、真空ラインを用いて2×10-2Torr、80℃で24時間焼き出しを行った。次に、アルゴン雰囲気中グローブボックス内で黒鉛2.05g、インターカラントとしてH2PtCl6・6H2Oを2.89g(C:Ptのモル比=30:1とした)、溶媒としてSOCl2 25mlをナス形フラスコに入れた後、アルゴンガスを15ml/minで流しながら119時間撹拌を行った後オイルバスを設置し、アルゴンガス流量を30ml/minにし、80℃で7時間還流を行った。還流後トルエンで洗浄し、真空ラインで乾燥し試料とした。
黒鉛粒子の粒径は、レーザー回折式粒度分布計(日機装製MICROTRAC-3000EX)を用いて測定した。黒鉛微粒子の比表面積はQantachrom製Autosorb-1を用いて、BET多点法により算出した。また、黒鉛微粒子および合成した層間化合物の結晶構造はX線回折装置(Rigaku製Multiflex)を用いて測定した。さらに調整したサンプルの表面部分が黒鉛層間化合物を形成しているか確認するため、Renishow社製NRS-2100を用いラマン散乱分光分析を行った。
(粉体抵抗)
三菱化学製粉体抵抗計PD―51を用い、650kg/cm2加圧時の粉体抵抗を測定した。
触媒の機能性の評価の一つとしてチオフェンの水素化脱硫反応を行った。装置は常圧固定床流通式反応装置を用いた。触媒を反応管に0.1g充填し、前処理として500℃で1時間ヘリウム(He)処理をした。その後、水素還元を450℃で1時間行い反応に用いた。反応はモル比で、チオフェン:水素=1:30の混合ガスを装置内に導入することによって行い、反応温度は350℃とした。分析にはガスクロマトグラフ(FID)を用いた。
以上の結果を表1及び表2に示す。表1は、〈改質黒鉛の調整方法1〉により調整された試料の結果を示し、表2の試料9から11は、〈改質黒鉛の調整方法2〉により調整された試料の結果を示す。
Claims (9)
- 比表面積が200〜1000m2/g 、ラマンスペクトルのDバンド(1350cm−1)とGバンド(1580cm−1)のピーク強度比であるR値が0.3〜0.7、およびX線回折法の(002)面のc軸方向の結晶子の大きさLc(002)が30nm以上であることを特徴とする改質黒鉛。
- 比表面積が200〜1000m2/g 、ラマンスペクトルのDバンド(1350cm−1)とGバンド(1580cm−1)のピーク強度比であるR値が0.3〜0.7、およびX線回折法の(002)面のc軸方向の結晶子の大きさLc(002)が30nm以上である改質黒鉛に金属塩化物がインターカレートされてなることを特徴とする黒鉛層間化合物。
- X線回折法による回折角度(2θ)が21〜23.5°にピークを発現することを特徴とする請求項2記載の黒鉛層間化合物。
- X線回折法による回折角度(2θ)が5〜7°にピークを発現することを特徴とする請求項2記載の黒鉛層間化合物。
- ラマン分光スペクトルのピークが1600〜1610cm−1に発現することを特徴とする請求項2記載の黒鉛層間化合物。
- 比表面積が200〜1000m2/g 、ラマンスペクトルのDバンド(1350cm−1)とGバンド(1580cm−1)のピーク強度比であるR値が0.3〜0.7、およびX線回折法の(002)面のc軸方向の結晶子の大きさLc(002)が30nm以上である改質黒鉛の表面に触媒機能を備える金属が坦持されてなることを特徴とする触媒。
- 少なくとも真空雰囲気中、低酸素雰囲気中、減圧雰囲気中、窒素雰囲気中又は希ガス元素雰囲気中において、5mmφ以下の小質量粉砕媒体を用いて、乾式粉砕法により高結晶性粒子を含む黒鉛を粉砕することによって、黒鉛粒子の微細化を抑制しつつ黒鉛の表面改質を優先的に進行させることを特徴とする請求項1記載の改質黒鉛の製造方法。
- 前記改質黒鉛と金属塩化物を混合し、気相法または溶媒法により調整することを特徴とする請求項2〜5の何れかに記載の黒鉛層間化合物の製造方法。
- 請求項2〜5の何れかに記載の黒鉛層間化合物であって、触媒機能を備える金属からなる金属塩化物がインターカレートされた黒鉛層間化合物を用い、焼成による還元または化学的な還元により前記金属を黒鉛層間に析出させるとともに該金属を黒鉛エッジ部分または黒鉛表面に固着した状態で坦持させることを特徴とする触媒の製造方法。
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Cited By (9)
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JP2010205846A (ja) * | 2009-03-02 | 2010-09-16 | Asahi Kasei Corp | 非水系リチウム型蓄電素子 |
JP2015525184A (ja) * | 2012-05-21 | 2015-09-03 | イメリス グラファイト アンド カーボン スイッツァランド リミティド | 表面修飾カーボンハイブリッド粒子、その作製方法および応用 |
JP2015526264A (ja) * | 2012-05-18 | 2015-09-10 | ドゥー,インフワン | 粒子材料を乾式粉砕するプロセス |
JPWO2016063455A1 (ja) * | 2014-10-20 | 2017-06-29 | パナソニック株式会社 | 電極、燃料電池及び水処理装置 |
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