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- JP2012041581A5 JP2012041581A5 JP2010182053A JP2010182053A JP2012041581A5 JP 2012041581 A5 JP2012041581 A5 JP 2012041581A5 JP 2010182053 A JP2010182053 A JP 2010182053A JP 2010182053 A JP2010182053 A JP 2010182053A JP 2012041581 A5 JP2012041581 A5 JP 2012041581A5
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- 239000002245 particle Substances 0.000 description 15
- 239000007771 core particle Substances 0.000 description 11
- 239000002105 nanoparticle Substances 0.000 description 11
- 239000011258 core-shell material Substances 0.000 description 10
- 239000013078 crystal Substances 0.000 description 9
- 239000010419 fine particle Substances 0.000 description 9
- 239000006229 carbon black Substances 0.000 description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 6
- 229910052750 molybdenum Inorganic materials 0.000 description 6
- 239000011733 molybdenum Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 5
- 229910052721 tungsten Inorganic materials 0.000 description 5
- 239000010937 tungsten Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910001868 water Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000550 scanning electron microscopy energy dispersive X-ray spectroscopy Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000004841 transmission electron microscopy energy-dispersive X-ray spectroscopy Methods 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
Description
本発明におけるコアシェル型微粒子は、第１の材料によって面心立方（ｆｃｃ）結晶構造を有するコア粒子を形成し、第１の材料と異なる第２の材料によって面心立方（ｆｃｃ）結晶構造を有するシェル層をコア粒子の表面にエピタキシャル成長させることによって形成され、面心立方（ｆｃｃ）結晶構造の｛１１１｝結晶面を表面に有している。
本発明におけるコアシェル型微粒子（コアシェル型触媒）は、好ましくは、貴金属以外の第１の材料によって面心立方（ｆｃｃ）結晶構造を有するコア粒子を形成し、好ましくは、貴金属からなる第２の材料によって面心立方（ｆｃｃ）結晶構造を有するシェル層をコア粒子の表面にエピタキシャル成長させることによって形成され、面心立方（ｆｃｃ）結晶構造の｛１１１｝結晶面を触媒微粒子の表面に有している。
（シェル層の厚さ（白金原子積層数）の評価方法）
作製したコアシェル型微粒子のシェル層の平均厚さは、コア粒子の平均直径とコアシェル型微粒子の平均直径（シェル層の外側直径に等しい。）をそれぞれＳＥＭ像（Scanning Electron Microscope image）又はＴＥＭ像（Transmission Electron Microscope image）により評価し、コア粒子、コアシェル型微粒子の平均粒子径（平均直径）を求め、コア粒子の平均粒子径（平均直径）Ｒ1とコアシェル型微粒子の平均粒子径（平均直径）Ｒ2の差(（Ｒ2−Ｒ1）／２）により求められる。白金原子積層数は、白金層の平均厚さを白金の面間隔（ｄ111＝０．２２６５ｎｍ）で割ることにより求められる。なお、コア粒子とコアシェル型微粒子のそれぞれの平均粒子径（平均直径）は、粒子の短径及び長径の各方向について求められた粒子径の平均値とする。
作製したコアシェル型微粒子のシェル層の平均厚さは、コア粒子の平均直径とコアシェル型微粒子の平均直径（シェル層の外側直径に等しい。）をそれぞれＳＥＭ像（Scanning Electron Microscope image）又はＴＥＭ像（Transmission Electron Microscope image）により評価し、コア粒子、コアシェル型微粒子の平均粒子径（平均直径）を求め、コア粒子の平均粒子径（平均直径）Ｒ1とコアシェル型微粒子の平均粒子径（平均直径）Ｒ2の差(（Ｒ2−Ｒ1）／２）により求められる。白金原子積層数は、白金層の平均厚さを白金の面間隔（ｄ111＝０．２２６５ｎｍ）で割ることにより求められる。なお、コア粒子とコアシェル型微粒子のそれぞれの平均粒子径（平均直径）は、粒子の短径及び長径の各方向について求められた粒子径の平均値とする。
また、コア粒子、コアシェル型微粒子の粒径方向にＳＥＭ−ＥＤＸ（Scanning Electron Microscopy-Energy Dispersive X-ray Spectroscopy：走査型電子顕微鏡エネルギー分散型Ｘ線分析法）、又は、ＴＥＭ−ＥＤＸ（Transmission Electron Microscopy-Energy Dispersive X-ray Spectroscopy：透過型電子顕微鏡エネルギー分散型Ｘ線分析法）によるライン分析によって、コア粒子とコアシェル型微粒子のそれぞれの平均粒子径（平均直径）を求めこれらより、シェル層の白金層の平均厚さ（白金原子積層数）を求めることができる。なお、コア粒子とコアシェル型微粒子のそれぞれの平均粒子径（平均直径）は、粒子の短径及び長径の各方向について求められた粒子径の平均値とする。
図１に示すように、空気又は酸素３５が、流路をもつ空気又は酸素供給部（セパレータ）６０の入口２６ｂから通路２７ｂへと流され、ガス拡散層２４ｂを通って、ガス拡散層２４ｂによって保持された触媒電極２２ｂに到達し、図１の下方に示すカソード反応に従って、触媒電極２２ｂ上で水素イオン、電子、酸素が反応し、水が生成され、水を含む排ガス２９ｂが出口２８ｂら排出される。図１の下方に示すように全反応は、メタノールと酸素から電気エネルギーを取り出して水と二酸化炭素を排出するというメタノールの燃焼反応となる。
このカーボンブラックに担持されたタングステンナノ粒子を５０ｍＬのアセトンに加え、よく撹拌して分散させた後、遠心分離器を用いて沈降させ、上澄み液を除去しカーボンブラックに担持されたタングステンナノ粒子を洗浄した。この洗浄処理を合計５回繰返すことにより、カーボンブラックに担持されたタングステンナノ粒子を精製した。最後に、カーボンブラックに担持されたタングステンナノ粒子に窒素気流をあてて乾燥させた。ＴＥＭ観察像から求めたタングステンナノ粒子の平均粒子径（平均直径）は１．４ｎｍ（標準偏差は±０．３ｎｍ）であった。
このカーボンブラックに担持されたモリブデンナノ粒子を５０ｍＬのアセトンに加え、よく撹拌して分散させた後、遠心分離器を用いて沈降させ、上澄み液を除去しカーボンブラックに担持されたモリブデンナノ粒子を洗浄した。この洗浄処理を合計５回繰返すことにより、カーボンブラックに担持されたモリブデンナノ粒子を精製した。最後に、カーボンブラックに担持されたモリブデンナノ粒子に窒素気流をあてて乾燥させた。ＴＥＭ観察像から求めたモリブデンナノ粒子の平均粒子径（平均直径）は１．８ｎｍ（標準偏差は±０．３ｎｍ）であった。
S. Iijima et al.," Structure Instability of Ultrafine Particles of Metals ", Phys. Rev. Lett., 56, 616-619 (1986) （Fig.1〜Fig.3）
O. Kitakami et al.," Size effect on the crystal phase of cobalt fine particles ", Phys. Rev. B, 56, 13849-13854 (1997) （Experiment, Resultand Discussion）
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010182053A JP2012041581A (ja) | 2010-08-17 | 2010-08-17 | コアシェル型微粒子及びこれを用いた機能デバイス |
| US13/196,093 US8361924B2 (en) | 2010-08-17 | 2011-08-02 | Fine particles of core-shell structure and functional device incorporated therewith |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2010182053A JP2012041581A (ja) | 2010-08-17 | 2010-08-17 | コアシェル型微粒子及びこれを用いた機能デバイス |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JP2012041581A JP2012041581A (ja) | 2012-03-01 |
| JP2012041581A5 true JP2012041581A5 (ja) | 2013-08-22 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2010182053A Ceased JP2012041581A (ja) | 2010-08-17 | 2010-08-17 | コアシェル型微粒子及びこれを用いた機能デバイス |
Country Status (2)
| Country | Link |
|---|---|
| US (1) | US8361924B2 (ja) |
| JP (1) | JP2012041581A (ja) |
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2010
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2011
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