CN102664274A - Preparation method of platinum and carbon composite nanometer material - Google Patents

Preparation method of platinum and carbon composite nanometer material Download PDF

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Publication number
CN102664274A
CN102664274A CN2012101316943A CN201210131694A CN102664274A CN 102664274 A CN102664274 A CN 102664274A CN 2012101316943 A CN2012101316943 A CN 2012101316943A CN 201210131694 A CN201210131694 A CN 201210131694A CN 102664274 A CN102664274 A CN 102664274A
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China
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platinum
preparation
organic solvent
carbon composite
chloroplatinic acid
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CN2012101316943A
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Chinese (zh)
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崔晓莉
宋鹏
张晓艳
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Fudan University
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Fudan University
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Priority to CN2012101316943A priority Critical patent/CN102664274A/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30Hydrogen technology
    • Y02E60/50Fuel cells

Abstract

The invention belongs to the technical field of a nanometer material, in particular relates to a preparation method of a platinum and carbon composite nanometer material. The preparation method comprises the following specific steps of adopting chloroplatinic acid as a raw material and utilizing organic solvent to prepare chloroplatinic acid solution; and then igniting the chloroplatinic acid solution with fire, reducing the chloroplatinic acid to simple substance platinum through the heat released in the burning process, making the solution disappear through the burning, directly producing carbon through the incomplete burning of the organic solvent, and finally forming the needed platinum and carbon composite nanometer material. The organic solvent can be any flammable organic solvent and is preferentially selected from methanol, ethanol, propyl alcohol or isopropyl alcohol, or normal hexane and benzene and the like, and the concentration of the prepared chloroplatinic acid solution is 10 to 50 mM. The preparation method is simple, no special equipment is required, no waste liquid is produced, the heat treatment process can be avoided, the platinum-carbon composite powder material can be directly obtained in one step, the energy conservation and emission reduction in the production process can be realized, and the preparation method is applicable to the industrialized production.

Description

The preparation method of a kind of platinum and carbon composite nano-material
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of method for preparing platinum and carbon composite nano-material.
Background technology
Since eighties of last century began nanometer technology flourish the nineties, the preparation of nano material was the important core content in nanometer science and technology field always.At present, preparation of nanomaterials research has become the active problem of a ten minutes of new material exploitation.The preparation of nano-powder material has many methods, like sol-gel process, coprecipitation method, atomizing thermolysis process etc.The straightforward procedure research of preparation nano material is new material exploitation and key in application problem.
The Pt/ carbon composite is at the electrode catalyst of fuel cell field extensive use, and its preparation has several different methods, like chemical reduction method, and hydrothermal method, solvent-thermal method, electrochemical reduction deposition technique etc.These method operating procedures are more loaded down with trivial details, manufacturing cycle is long, relates to discharging of waste liquid, need heat treatment to accomplish crystal transfer simultaneously, need specific heat treatment or electrochemical apparatus etc.
Summary of the invention
The object of the invention is to provide that a kind of technology is simple, the method for preparing Pt and carbon nano-composite material of no discharging of waste liquid.
The present invention utilizes organic substance to burn and in combustion process, discharges the characteristics of thermal discharge, directly accomplishes the crystal formation conversion of material.Organic imperfect combustion directly produces carbon, avoids the discharging of waste liquid, need not the last handling process of product, realizes energy-saving and emission-reduction, can directly prepare the nano composite material with specific crystal formation.With respect to " solvent thermal, hydro thermal method " method of preparation nano material, we are this new method called after " burning hot method ".
The method for preparing Pt and carbon nano-composite material that the present invention proposes is a raw material with the chloroplatinic acid, disposes platinum acid chloride solution with organic solvent earlier; Light with naked light then, along with the carrying out of combustion process, liberated heat makes the chloroplatinic acid thermal reduction change simple substance platinum, and solution disappears through burning, and the imperfect combustion of organic solvent directly produces carbon, finally forms required Pt and carbon nano-composite material.This material is the composite powder material of a kind of nano platinum particle and carbon.
Among the present invention, said organic solvent can use any organic solvent that can burn, and preferably, the used solvent of the present invention is methyl alcohol, ethanol, propyl alcohol or isopropyl alcohol, or n-hexane, benzene etc.
Among the present invention, the concentration of the platinum acid chloride solution of configuration is 10-50mM.
Among the present invention, in the composite powder material of Pt nanoparticle and carbon, the ratio of Pt nanoparticle and carbon can be regulated through the molar concentration of control chloroplatinic acid and the solvent of selective combustion.For example under the concentration conditions of identical chloroplatinic acid, be that carbon content in the composite material that obtains of solvent is higher than with ethanol with the propyl alcohol be the carbon content in the composite material of solvent.
Experiment shows that the composite powder material of Pt nanoparticle-carbon that the present invention is prepared has good electro catalytic activity, can be used for the electrode catalyst of fuel cell.
The preparation method of the composite powder material of Pt nanoparticle-carbon provided by the present invention compared with prior art, has the following advantages: method is very simple; Need not special installation; Do not have any waste liquid and produce, avoided heat treatment process, directly obtain platinum-carbon composite powder material; Realizing the energy-saving and emission-reduction of production process, is to be suitable for industrial preparation method.
Description of drawings
Fig. 1 is the inventive method process sketch map.Wherein, a representes solution, the composite material powder of platinum-carbon that b obtains after representing to burn.
The XPS figure of the Pt of the composite powder material of Pt nanoparticle-carbon that Fig. 2 the inventive method is prepared.
The XPS figure of the carbon of the composite powder material of Pt nanoparticle-carbon that Fig. 3 the inventive method is prepared.
The TEM figure of the composite powder material of Pt nanoparticle-carbon that Fig. 4 the inventive method is prepared.
The composite powder material electrode of Pt nanoparticle-carbon that Fig. 5 the present invention is prepared is at H 2SO 4Cyclic voltammogram in the solution.
The composite powder material electrode of Pt nanoparticle-carbon that Fig. 6 the present invention is prepared is at CH 3OH+H 2SO 4Cyclic voltammogram in the solution.
Embodiment
Below through embodiment the present invention is described further, but be not limited thereto.
Embodiment 1Prepare the absolute ethyl alcohol of 15 mM chloroplatinic acids and put into the 150mL beaker, light with match, liquid promptly takes fire from liquid level, obtains the sample of black after burning finishes.The XPS of working sample finds exist (Fig. 2) of simple substance Pt in the gained sample.Fig. 3 is the XPS spectrum of carbon in the sample, and working sample TEM surface topography can be found, the size of the Pt nano particle that this technology obtains is about 10 nm.(Fig. 4).
Embodiment 2The preparation of Pt/C sample is with embodiment 1.Take by weighing 0.5% the NAFION solution of Pt/C sample preparation 2mg/ml, ultrasonic dispersion soln is to evenly.Measure 10 μ l and drip and be coated in the glass-carbon electrode surface of handling, room temperature is placed dry, then at H 2SO 4Measure its cyclic voltammetric characteristic curve (Fig. 5) in the solution, show the existence of simple substance Pt in the sample.
Embodiment 3The preparation of Pt/C sample is with embodiment 1.Take by weighing 0.5% the NAFION solution of the prepared Pt/C sample of the present invention preparation 2mg/ml, ultrasonic dispersion soln is to evenly.Measure 20ul and drip and be coated in the glass-carbon electrode surface of handling, room temperature is placed dry, then at CH 3OH+H 2SO 4Measure its cyclic voltammetric characteristic curve in the solution, find that the gained sample is to CH 3The OH oxidation shows good electric catalyticing characteristic (Fig. 6).
Embodiment 4Prepare the aqueous isopropanol of 10 mM chloroplatinic acids and put into the 150mL beaker, light with match, liquid promptly takes fire from liquid level, obtains the sample of black after burning finishes.The XPS of working sample finds the existence of simple substance Pt in the gained sample, shows the generation of simple substance Pt.

Claims (3)

1. the preparation method of platinum and carbon composite nano-material is characterized in that concrete steps are: be raw material with the chloroplatinic acid, dispose platinum acid chloride solution with organic solvent earlier; Light with naked light then, along with the carrying out of combustion process, liberated heat makes the chloroplatinic acid thermal reduction change simple substance platinum into, and solution disappears through burning, and the imperfect combustion of organic solvent directly produces carbon, finally forms required platinum and carbon composite nano-material.
2. the preparation method of platinum according to claim 1 and carbon composite nano-material is characterized in that said organic solvent is methyl alcohol, ethanol, propyl alcohol or isopropyl alcohol.
3. the preparation method of platinum according to claim 1 and carbon composite nano-material, the concentration that it is characterized in that the platinum acid chloride solution of said configuration is 10-50mM.
CN2012101316943A 2012-05-02 2012-05-02 Preparation method of platinum and carbon composite nanometer material Pending CN102664274A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20080039034A (en) * 2006-10-31 2008-05-07 삼성에스디아이 주식회사 Method of preparing catalyst for fuel cell
US20090104497A1 (en) * 2007-10-18 2009-04-23 Kabushiki Kaisha Toshiba Fuel electrode catalyst, method for producing fuel electrode catalyst, fuel cell, and method for producing fuel cell
CN101798110A (en) * 2010-04-08 2010-08-11 复旦大学 Preparation method of spherical nanometer titanium dioxide

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20080039034A (en) * 2006-10-31 2008-05-07 삼성에스디아이 주식회사 Method of preparing catalyst for fuel cell
US20090104497A1 (en) * 2007-10-18 2009-04-23 Kabushiki Kaisha Toshiba Fuel electrode catalyst, method for producing fuel electrode catalyst, fuel cell, and method for producing fuel cell
CN101798110A (en) * 2010-04-08 2010-08-11 复旦大学 Preparation method of spherical nanometer titanium dioxide

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
XIAOYAN ZHANG等: "Carbon-incorporated TiO2 microspheres: Facile flame assisted hydrolysis of tetrabutyl orthotitanate and photocatalytic hydrogen production", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》 *
XIAOYAN ZHANG等: "Carbon-incorporated TiO2 microspheres: Facile flame assisted hydrolysis of tetrabutyl orthotitanate and photocatalytic hydrogen production", 《INTERNATIONAL JOURNAL OF HYDROGEN ENERGY》, vol. 37, no. 2, 24 October 2011 (2011-10-24), pages 1356 - 1365 *

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Application publication date: 20120912