• Bulletin of the Korean Chemical Society
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• 제27권8호
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• pp.1121-1126
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• 2006

Methanol oxidation effect on carbon supported Pt was investigated as a function of Pt content in a sample which is closely correlated with Pt particle sizes. After prolonged methanol oxidation the Pt particle size did not change within the experimental error ranges. The $^{13}C$ chemical shift and linewidth of CO adsorbed on Pt show non-linear behavior simply due to the Pt particle size difference. The Pt size variation difference between this work and the previous reports of the particle growths is explained by the experimental temperature difference.

• 한국재료학회지
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• 제21권3호
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• pp.156-160
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• 2011

FePt nanoparticles suspension was synthesized by reduction of platinum acetylacetonate and decomposition of iron pentacarbonyl in the presence of oleic acid and oleyl amine. FePt nanoparticles were coated on a substrate by convective assembly from the suspension. To prevent the coalescence during the annealing of FePt nanoparticles double convective coatings were tried. First convective coating was for silica particle assembly on a silicon substrate and second one was for FePt nanoparticles on the previously coated silica layers. It was observed by scanning electron microscopy (SEM) that FePt nanoparticles were dispersed on the silica particle surface. After annealing at $700^{\circ}C$ for 30 minutes under nitrogen atmosphere, FePt nanoparticles on silica particles were maintained in a dispersed state with slight increase of particle size. On the contrary, FePt nanoparticles that were directly coated on silicon substrate showed severe particle growth after annealing due to the close-packing of nanoparticles during assembly. The size variation during annealing was also verified by X-ray diffractometer (XRD). It was suggested that pre-coating, which offered solvent flux oppose to the capillary force between FePt nanoparticles, was an effective method to prevent coalescence of nano-sized particles under high temperature annealing.

• 한국신재생에너지학회:학술대회논문집
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• 한국신재생에너지학회 2006년도 추계학술대회
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• pp.443-446
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• 2006

Carbon-supported Platinum (Pt) is the potential electro-catalyst material for anodic and cathodic reactions in fuel cell. Catalytic activity of the metal strongly depends on the particle shape, size and distribution of the metal in the porous supportive network. Conventional preparation techniques based on wet impregnation and chemical reduction of the metal precursors often do not provide adequate control of particle size and shape. We have proposed a novel route for preparing nano sized Pt colloidal particles in solution by oxidation of ethylene glycol. These Pt nano particles were deposited on large surface area carbon support. The process of nano Pt colloid formation involves the oxidation of solvent ethylene glycol to mainly glycolic acid and the presence of its anion glycolate depends on the solution pH. In the process of colloidal Pt formation glycolate actsas stabilizer for the Pt colloidal particle and prevents the agglomeration of colloidal Pt particles. These mono disperse Pt particles in carbon support are found uniformly distributed in nearly spherical shape and the size distribution was narrow for both supported and unsupported metals. The average diameter of the Pt nano particle was controlled in the range off to 3 nm by optimizing reaction parameters. Transmission electron microscopy, CV and RRDE experiments were used to compliment the results.

• Bulletin of the Korean Chemical Society
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• 제33권10호
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• pp.3331-3337
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• 2012

Ru-modified Pt nanoparticles of various sizes on platelet carbon nanofiber toward methanol oxidation were investigated in terms of particle size effect. The sizes of Pt nanoparticles, prepared by polyol method, were in the range of 1.5-7.5 nm and Ru was spontaneously deposited by contacting Pt nanoparticles with the Ru precursor solutions of 2 and 5 mM. The Ru-modified Pt nanoparticles were characterized using transmission electron microscopy, X-ray photoelectron spectroscopy and cyclic voltammetry. The methanol oxidation activities of Ru-modified Pt nanoparticles, measured using cyclic voltammetry and chronoamperometry, revealed that when the Pt particle size was less than 4.3 nm, the mass specific activity was fairly constant with an enhancement factor of more than 2 at 0.4 V. However, the surface area specific activity was maximized on Pt nanoparticles of 4.3 nm modified with 5 mM Ru precursor solution. The observations were discussed in terms of the enhancement of poison oxidation by Ru and the population variation of Pt atoms at vertices and edges of Pt nanoparticles due to selective deposition of Ru on the facets of (111) and (100).

• 전기화학회지
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• 제11권4호
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• pp.313-318
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• 2008

본 연구에서는 백금의 입자크기가 내구성과 활성에 미치는 영향을 고찰하였다. 상용 Pt/C의 열처리를 통해 백금 입자 크기를 $3.5{\sim}9\;nm$로 조절하였고, XRD와 TEM을 통해 이를 확인하였다. 촉매의 내구성 분석을 위해 가속 실험을 실시하였고, 촉매 활성 측정을 위해 산소환원반응 실험을 하였다. 백금의 입자크기를 증가시킬수록 내구성은 향상되었으나 촉매의 활성이 저하되었다. 즉 촉매의 내구성과 활성은 반비례관계가 성립된다는 것을 확인하였다. 그리고 저하된 촉매 활성과 내구성을 향상시키기 위해, 합금 촉매를 사용하였다.상용 Pt/C의 최대 전력 밀도는 약 $507.6\;mV/cm^2$ 이고, PtCo/C 합금촉매는 $585.8\;mV/cm^2$이었다. 전기화학적 표면적은 상용 Pt/C는 약 60%정도 감소하였고, PtCo/C 합금촉매는 약 24%정도의 감소율을 나타냈다. 따라서 백금의 입자 크기 조절과 합금화를 통해 백금의 내구성과 활성을 동시에 높일 수 있었다.

• 한국입자에어로졸학회지
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• 제8권2호
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• pp.83-88
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• 2012

The electrical wire explosion process in liquid media is promising for nano-sized metal and/or alloy particles. The hybrid Pt/Fe-Cr-Al and Pt/Ni-Cr-Fe nanoparticles for exhaust emission control system are synthesized by electrical wire explosion process in liquid media. The alloy powders have spherical shape and nanometer size. According to the wire component, while Pt/Fe-Cr-Al nanoparticles are shown the well dispersed Pt on the Fe-Cr-Al core particle, Pt/Ni-Cr-Fe nanoparticles are shown the partially separated Pt on the Ni-Cr-Fe core particle. Morphologies and component of two kinds of hybrid nano catalyst particles were characterized by transmission electron microscope and energy dispersive X-ray spectroscopy analysis.

• 한국자기공명학회논문지
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• 제6권1호
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• pp.38-44
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• 2002

60% Pt on Vulcan XC-72 with similar Pt sizes to fuel cell grade Pt black was investigated by $\^$13/C nuclear magnetic resonance spectroscopy (NMR), cyclic voltammery (CV), transmission electron microscopy (TEM). Experiments were carried out on electrochemically cleaned samples as well as as-received. The TEM and CV results showed that the average particle sizes were changed by cleaning. However, the chemical shift （$\delta$$\_$G/） of $\^$13/C of $\^$13/CO absorbed on Pt surfaces did not show any appreciable variation with particle size change as did in Pt black. These results indicate that a combination of different analytic techniques is essential to understand the properties of the metal particle catalysts and that the presence of carbon black support strongly influences the NMR data, probably through metal-support interaction.

• 한국분말재료학회지
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• 제19권1호
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• pp.60-66
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• 2012

In this study, Platinum(Pt) nanoparticles were synthesized by using polyol process which is one of the liquid phase reduction methods. Dihydrogen hexachloroplatinate (IV) hexahydrate $(H_2PtCl_6{\cdot}6H_2O)$, as a precursor, was dissolved in ethylene glycol and silver nitrate ($AgNO_3$) was added as metal salt for shape control of Pt particle. Also, polyvinylpyrrolidone (PVP), as capping agent, was added to reduce the size of particle and to separate the particles. The size of Pt nanoparticles was evaluated particle size analyzer (PSA). The size and morphology of Pt nanoparticles were observed by transmission electron microscopy (TEM) and high resolution TEM (HRTEM). Synthesized Pt nanoparticles were studied with varying time and temperature of polyol process. Pt nanoparticles have been successfully synthesized with controlled sizes in the range 5-10 and 20-40 nm with cube and multiple-cube shapes.

• 한국재료학회지
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• 제19권5호
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• pp.233-239
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• 2009

The electrocatalytic behavior of the PtCo catalyst supported on the multi-walled carbon nanotubes (MWNTs) has been evaluated and compared with commercial Pt/C catalyst in a polymer electrolyte membrane fuel cell(PEMFC). A PtCo/MWNTs electrocatalyst with a Pt:Co atomic ratio of 79:21 was synthesized and applied to a cathode of PEMFC. The structure and morphology of the synthesized PtCo/MWNTs electrocatalysts were characterized by X-ray diffraction and transmission electron microscopy. As a result of the X-ray studies, the crystal structure of a PtCo particle was determined to be a face-centered cubic(FCC) that was the same as the platinum structure. The particle size of PtCo in PtCo/MWNTs and Pt in Pt/C were 2.0 nm and 2.7 nm, respectively, which were calculated by Scherrer's formula from X-ray diffraction data. As a result we concluded that the specific surface activity of PtCo/MWNTs is superior to Pt/C's activity because of its smaller particle size. From the electrochemical impedance measurement, the membrane electrode assembly(MEA) fabricated with PtCo/MWNTs showed smaller anodic and cathodic activation losses than the MEA with Pt/C, although ohmic loss was the same as Pt/C. Finally, from the evaluation of cyclic voltammetry(CV), the unit cell using PtCo/MWNTs as the cathode electrocatalyst showed slightly higher fuel cell performance than the cell with a commercial Pt/C electrocatalyst.

• The Korean Journal of Ceramics
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• 제3권1호
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• pp.52-56
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• 1997

The Pt doped $TiO_2$ composite membranes were prepared by the sol-gel process. The Pt doped titania sol was peptized with hydrochloric acid in the pH range of 1.23 to 1.32 at 5$0^{\circ}C$. The average particle size of the Pt doped titania sol was shown to be below 15nm and well dispersed in the solution. XPS show the Pt elements continuous and homogeneous dispersed in the $TiO_2$ membrane. The mean particle size of the Pt doped $TiO_2$ composite membrane has smaller than that of the undoped $TiO_2$ composite membrane. The average pore size of the Pt doped $TiO_2$ composite membrane was increased from 58 to 193 $\AA$ with firing temperature changed from 550 to 85$0^{\circ}C$. It was observed that the Pt doped $TiO_2$ composite membranes showed crack-free and homogeneous microstructue as well as narrow particle size distribution up to above 75$0^{\circ}C$.