CN103259023B - A kind of hydrogen cell electrode material preparation method - Google Patents
A kind of hydrogen cell electrode material preparation method Download PDFInfo
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- CN103259023B CN103259023B CN201210450953.9A CN201210450953A CN103259023B CN 103259023 B CN103259023 B CN 103259023B CN 201210450953 A CN201210450953 A CN 201210450953A CN 103259023 B CN103259023 B CN 103259023B
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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
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The present invention relates to the preparation method of fuel cell electrode material, particularly in carbon paper surface growth CNT (CNT) and the method for load platinum (Pt).Comprise the following steps that: (1) deposits the catalyst of a layer growth CNT by the method for ion sputtering on carbon paper；(2) CNT is grown with plasma reinforced chemical vapour deposition at carbon paper surface；(3) method that grown the carbon paper ion sputtering of CNT is deposited platinum catalyst on the carbon nanotubes.
Description
Technical field
The present invention relates to the electrode material preparation method for fuel cell, particularly to one for Proton Exchange Membrane Fuel Cells
The platinum-carrying carbon nanotube of carbon fiber paper surface growth in situ and preparation method thereof.
Background technology
Fuel cell is the device that chemical energy is directly changed into low-voltage DC by fuel and oxidant generation electrochemical reaction.
Fuel cell is acknowledged as the cleaning of 21 century first-selection, efficient generation technology, and its development has become international energy with exploitation
The focus of area research, and whole electric automobile, submarine and the fast development of power generation industries will be promoted.
Up to the present, polytype fuel cell, wherein Proton Exchange Membrane Fuel Cells (PEMFC) have been researched and developed
It is after alkaline fuel cell, phosphoric acid type fuel cell, fused carbonate type fuel cell and SOFC
The 5th Replacing fuel battery.Owing to having used solid electrolyte polymeric membrane as electrolyte, there is energy transformation ratio high and low temperature
Start, electroless pond is revealed, corrosion-free, the high prominent advantage of life-span length, specific power.The research of PEMFC has become as all
Main flow in types of fuel cells research spring tide, is to be hopeful to realize business-like fuel cell the soonest.
CNT has the one-dimensional tubular graphene structure of uniqueness, and specific surface area is big, resistance is low, chemical stability is high, is to receive
The ideal carrier of rice catalyst.The noble metal nano particles with unique catalytic performance is supported on the surface of CNT, is formed
Noble metal nano particles/carbon mano-tube composite not only have the excellent properties of two kinds of nano materials concurrently, it is also possible to produce new spy
Property.Making catalyst carrier with CNT and can increase catalyst loadings, on carrier, dispersion and the active center of platinum are the most obvious
Improve.CNT mechanical strength is high, can form inierpeneirating network structure, improve the intensity of Catalytic Layer, favorably in Catalytic Layer
In improving the durability of membrane electrode fuel cell, and compared with traditional material with carbon element, the kinetics of electron transfer in CNT
Behavior is best.Therefore CNT has good application prospect in terms of fuel-cell catalyst carrier.
Patent " is directly grown CNT at carbon paper surface, then is urged in the supporting platinum-based nanometer of its carbon nano tube surface by CVD
The carbon nanotube electrode of agent and manufacture method thereof ", the patent No. 200710198794.7, it was also proposed that grow carbon nanometer at carbon paper surface
Managing and carry platinum and make fuel cell electrode material, its preparation method is that carbon paper is immersed in aqueous sulfuric acid pretreatment and is dried by (1)；
(2) carbon paper after processing is dipped in the electric spheroid aqueous solution of nickel, cobalt, iron compound or its mixture, is repeated ultrasonic
Ripple processes, and makes above-mentioned metal be evenly distributed on carbon paper surface；(3) it is passed through gas-phase carbon at the carbon paper surface being loaded with catalyst metals
Source, maintains suitable temperature and pressure, grows CNT；(4) from growth CNT remove nickel, cobalt, ferrum or its
Mixture metal, and CNT is carried out surface process；(5) on the carbon paper that grown CNT, gas phase platinum it is passed through
Electricity spheroid, keeps certain temperature and pressure, supporting platinum-based nanocatalyst.
This patent method is that (1) uses ion sputtering process to sputter one layer of nickel, ferrum or the catalyst of its mixture at carbon fiber paper surface,
Sputter procedure is passed through argon shield；(2) it is passed through H at carbon paper surface2, maintain suitable temperature and pressure, make catalyst be filled
Divide reduction；(3) carbon paper surface after reduction treatment is passed through gas phase carbon source, maintains suitable temperature and pressure, penetrates certain
Frequently CNT is grown under power and bias；(4) carbon paper that grown CNT soaked in hydrochloric acid solution and is dried, removing
The metal such as de-iron, nickel；(5) carbon paper that grown CNT being carried out platinum target ion sputtering under an argon atmosphere, Supported Pt Nanoparticles is urged
Agent.This patent operational approach is simple, and carbon paper, without pretreatment, strengthens owing to employing plasma in carbon nanotube growth process
And the means such as bias, growth density of carbon nanometer tube is big, uniform diameter, and it is little, in carbon nano tube surface that ion sputtering carries platinum grain
It is evenly distributed, more preferable catalytic performance can be obtained.
Patent " low-platinum high active core-shell structure catalyst and preparation method thereof ", platinum is covered by the patent No. 200910117488.5
Form nucleocapsid structure on Metal Substrate kernel, and be carried in carbon dust or carbon nanotube carrier." CNT carries platinum electrode and urges patent
The preparation method of agent ", patent No. 02155255.X uses CNT to be carrier, and chloroplatinic acid reduction is deposited on CNT
Upper preparation Pt/CNTs catalyst.Patent " preparation method of CNT load platinum ruthenium anti-CO electrode catalyst ", the patent No.
02155256.8 with CNT as carrier, uses in-situ chemical homogeneous precipitation method, by isoionic to Pt, Ru, Sn metastable state glue
Body reduction is deposited on CNT.Patent " the system of the catalyst of carbon multi-wall nano tube loaded metal platinum nano particle of a kind of surface nitrile-group modification
Preparation Method ", the patent No. 201010168318.2 use the multi-walled carbon nano-tubes of surface nitrile-group modification as carrier, with alcohol for reduction
Agent, deposits to chloroplatinic acid reduction on CNT.Patent " a kind of platinum/carbon nanotube catalyst and preparation method and application ", patent
CNT is dipped in chloroplatinic acid aqueous solution stirring dipping by numbers 200910236390.1, grinds after drying, uses aqueous sodium formate solution
Add thermal reduction, it is thus achieved that platinum/carbon nanotube catalyst.Patent " the fuel battery negative pole of a kind of high stability being applicable to dynamic operation condition
Catalyst ", commercially available CNT is carried out pretreatment by the patent No. 200910248845.1, then supports active component, it is thus achieved that
CNT platinum catalyst.Patent " preparation method of a kind of carbon nano tube loaded cobalt-platinum alloy catalyst ", the patent No.
200810224481.9 with containing cobalt.The CNT working electrode of platino active matter precursor is negative electrode, with platinum electrode as anode,
With Solid phase electrolysis salt as electrolyte, using pulse electrodeposition was to generate carbon nano tube loaded cobalt-platinum alloy catalyst originally.Patent " one
The preparation method of proton exchanging film fuel battery cathod catalyst ", CNT is distributed to by the patent No. 200910085170.3
In two book solution, formic acid reducing process supporting Pt is used to generate catalyst." CNT for fuel cell carries platinum and urges patent
Agent and preparation method thereof ", the patent No. 200410009870.1 first carries out pretreatment to CNT, then uses formaldehyde reduction
Method prepares Pt/MWNTs catalyst.This patent method is directly at carbon paper surface in-situ growing carbon nano tube, and uses ion to spatter
Method of penetrating prepares Pt nanoparticle in carbon nano tube surface, and preparation method is different from above-mentioned patent.
Summary of the invention
It is an object of the invention to provide a kind of catalyst dispersity good, the catalysis high used in proton exchange membrane fuel cell platinum/carbon of activity is received
Mitron/carbon fiber paper electrode material.
It is a further object to provide one and can be mass Proton Exchange Membrane Fuel Cells platinum/carbon nano-tube/carbon fiber paper
Electrode material the method being assembled into monocell.
The platinum/carbon nano-tube for fuel cell of the present invention/carbon fiber paper electrode material is with carbon fiber paper as carrier, growth in situ
CNT, and with CNT as carrier, sputter platinum catalyst.Wherein, a diameter of the 20 of CNT～40nm, platinum
A diameter of the 2～4nm of grain, platinum grain is dispersed in carbon nano tube surface.
The preparation method of the platinum/carbon nano-tube for fuel cell of the present invention/carbon fiber paper electrode material is first at carbon fiber paper table
Face sputtering nickel, iron catalyst, then using plasma strengthens chemical vapour deposition technique (PECVD) in-situ growing carbon nano tube,
Finally sputtering platinum catalyst in carbon nano tube surface, the method comprises the following steps:
(1) sputtering nickel, iron catalyst: use ion sputtering process to sputter one layer of nickel or the catalyst film of ferrum at carbon fiber paper surface,
Sputter procedure is passed through argon shield；
(2) catalyst reduction: the carbon fiber paper obtained after step (1) being processed is at H2Under atmosphere, 200～1000 DEG C of reduction
0.5～5.0 hour；
(3) growth CNT: product step (2) obtained is at H2And CH4Under atmosphere, 600～1000 DEG C process 0.5～5
Hour, prepare the CNT of carbon fiber paper surface growth in situ, take out after being cooled to less than 100 DEG C；
(4) product obtained by step (3) soaked in hydrochloric acid solution and is dried, removing the metal such as ferrum, nickel；
(5) product obtained by step (4) is carried out under an argon atmosphere the ion sputtering of Pt nanoparticle.
The carbon nanotube density using the method for the invention to grow at carbon paper surface is big, is evenly distributed, is combined jail with carbon fiber paper
Gu, caliber is 20～40nm, it is possible to realize the good dispersion of platinum grain, platinum grain a diameter of 2～4nm, shows preferably
Catalytic performance.
Utilizing the method to prepare fuel cell electrode material, avoid the dispersion steps of CNT, operating process is simple, and
Increase the bond strength of CNT and carbon fiber paper matrix, improve the platinum catalyst dispersibility in carbon nano tube surface, carry
The high utilization rate of platinum catalyst, it is achieved that the batch production of proton exchange membrane fuel cell electrode material.
The shape characteristic of used in proton exchange membrane fuel cell platinum/carbon nano-tube/carbon fiber paper electrode material prepared by the inventive method is used
Scanning electron microscope (SEM) characterizes.
Accompanying drawing explanation
Fig. 1 is the stereoscan photograph of platinum/carbon nano-tube/carbon fiber paper.
Detailed description of the invention
Embodiment 1:
(1) sputtering Raney nickel: use ion sputtering process to sputter one layer of Raney nickel thin film, sputter procedure at carbon fiber paper surface
In be passed through argon shield, the pressure of argon is 0.1～1MPa, and sputtering pressure is 2～10 × 10-1Pa, sputtering current is 1～10mA,
Sputtering time is 5～60min；
(2) catalyst reduction: the carbon fiber paper obtained after step (1) being processed is at H2Reduce 0.5～5 hour under atmosphere, H2
Pressure is 100～1000Pa, H2Flow is 10～100sccm；
(3) product step (2) obtained is at H2And CH4Process 0.5～5 hour under atmosphere, prepare carbon fiber paper surface former
The CNT of position growth, takes out after being cooled to less than 100 DEG C, and the pressure of gas is 100～1000Pa, H2Flow is
10～100sccm, CH4Flow is 10～100sccm, and radio-frequency power is 0～200W, and back bias voltage is 0V；
(4) product obtained by step (3) soaked in 2mol/L hydrochloric acid solution and is dried, removing the metal such as ferrum, nickel；
(5) product obtained by step (4) carries out the ion sputtering of platinum grain under an argon atmosphere, and the pressure of argon is
0.1～1MPa, sputtering pressure is 2～10 × 10-1Pa, sputtering current is 1～10mA, and sputtering time is 10～60s.
Embodiment 2:
(1) sputtering Raney nickel: use ion sputtering process to sputter one layer of Raney nickel thin film, sputter procedure at carbon fiber paper surface
In be passed through argon shield, the pressure of argon is 0.1～1MPa, and sputtering pressure is 2～10 × 10-1Pa, sputtering current is 1～10mA,
Sputtering time is 5～60min；
(2) catalyst reduction: the carbon fiber paper obtained after step (1) being processed is at H2Reduce 0.5～5 hour under atmosphere, H2
Pressure is 100～1000Pa, H2Flow is 10～100sccm；
(3) product step (2) obtained is at H2And CH4Process 0.5～5 hour under atmosphere, prepare carbon fiber paper surface former
The CNT of position growth, takes out after being cooled to less than 100 DEG C, and the pressure of gas is 100～1000Pa, H2Flow is
10～100sccm, CH4Flow is 10～100sccm, and radio-frequency power is 0～200W, and back bias voltage is 25V；
(4) product obtained by step (3) soaked in 2mol/L hydrochloric acid solution and is dried, removing the metal such as ferrum, nickel；
(5) product obtained by step (4) carries out the ion sputtering of platinum grain under an argon atmosphere, and the pressure of argon is
0.1～1MPa, sputtering pressure is 2～10 × 10-1Pa, sputtering current is 1～10mA, and sputtering time is 10～60s.
Embodiment 3:
(1) sputtering iron catalyst: use ion sputtering process to sputter one layer of iron catalyst thin film, sputter procedure at carbon fiber paper surface
In be passed through argon shield, the pressure of argon is 0.1～1MPa, and sputtering pressure is 2～10 × 10-1Pa, sputtering current is 1～10mA,
Sputtering time is 5～60min；
(2) catalyst reduction: the carbon fiber paper obtained after step (1) being processed is at H2Reduce 0.5～5 hour under atmosphere, H2
Pressure is 100～1000Pa, H2Flow is 10～100sccm；
(3) product step (2) obtained is at H2And CH4Process 0.5～5 hour under atmosphere, prepare carbon fiber paper surface former
The CNT of position growth, takes out after being cooled to less than 100 DEG C, and the pressure of gas is 100～1000Pa, H2Flow is
10～100sccm, CH4Flow is 10～100sccm, and radio-frequency power is 0～200W, and back bias voltage is 50V；
(4) product obtained by step (3) soaked in 2mol/L hydrochloric acid solution and is dried, removing the metal such as ferrum, nickel；
(5) product obtained by step (4) carries out the ion sputtering of platinum grain under an argon atmosphere, and the pressure of argon is
0.1～1MPa, sputtering pressure is 2～10 × 10-1Pa, sputtering current is 1～10mA, and sputtering time is 10～60s.
Embodiment 4:
(1) sputtering iron catalyst: use ion sputtering process to sputter one layer of iron catalyst thin film, sputter procedure at carbon fiber paper surface
In be passed through argon shield, the pressure of argon is 0.1～1MPa, and sputtering pressure is 2～10 × 10-1Pa, sputtering current is 1～10mA,
Sputtering time is 5～60min；
(2) catalyst reduction: the carbon fiber paper obtained after step (1) being processed is at H2Reduce 0.5～5 hour under atmosphere, H2
Pressure is 100～1000Pa, H2Flow is 10～100sccm；
(3) product step (2) obtained is at H2And CH4Process 0.5～5 hour under atmosphere, prepare carbon fiber paper surface former
The CNT of position growth, takes out after being cooled to less than 100 DEG C, and the pressure of gas is 100～1000Pa, H2Flow is
10～100sccm, CH4Flow is 10～100sccm, and radio-frequency power is 0～200W, and back bias voltage is 75V；
(4) product obtained by step (3) soaked in 2mol/L hydrochloric acid solution and is dried, removing the metal such as ferrum, nickel；
(5) product obtained by step (4) carries out the ion sputtering of platinum grain under an argon atmosphere, and the pressure of argon is
0.1～1MPa, sputtering pressure is 2～10 × 10-1Pa, sputtering current is 1～10mA, and sputtering time is 10～60s.
Claims (7)
1. the preparation method for the platinum/carbon nano-tube/carbon fiber paper electrode material of fuel cell, with carbon fiber paper as carrier, in-situ growing carbon nano tube, and with CNT as carrier, with platinum as catalyst, platinum grain is uniformly dispersed in the surface of CNT, it is characterized in that, the method comprises the following steps:
(1) use ion sputtering process at carbon fiber paper surface one layer of nickel of sputtering or the catalyst film of ferrum, sputter procedure is passed through argon shield；
(2) carbon fiber paper obtained after step (1) being processed is at H2Under atmosphere, 200 DEG C are reduced 5.0 hours；
(3) product step (2) obtained is at H2And CH4Under atmosphere, 600～1000 DEG C process 0.5～5 hour, and using plasma strengthens chemical vapour deposition technique PECVD and prepares the CNT of carbon fiber paper surface growth in situ, takes out after being cooled to less than 100 DEG C；The pressure of gas is 100～1000Pa, H2Flow is 10～100sccm, CH4Flow is 10～100sccm, and radio-frequency power is 0～200W, and back bias voltage is 0～100V；
(4) product that step (3) obtains soaked in hydrochloric acid solution and is dried, removing ferrum, nickel metal；
(5) product obtained by step (4) is carried out under an argon atmosphere the ion sputtering of platinum grain.
The preparation method of the platinum/carbon nano-tube for fuel cell the most according to claim 1/carbon fiber paper electrode material, is characterized in that: a diameter of the 20 of described CNT～40nm, a diameter of the 2 of platinum grain～4nm.
Method the most according to claim 1, is characterized in that, in described step (1), sputtering pressure is 2 × 10-1～10 × 10-1Pa, sputtering current is 1～10mA, and sputtering time is 5～60min.
Method the most according to claim 1, is characterized in that, H in described step (2)2Pressure is 100～1000Pa, H2Flow is 10～100sccm.
Method the most according to claim 1, is characterized in that, in described step (4), the concentration of hydrochloric acid is 2mol/L, soak time 12～24 hours, baking temperature 100～120 DEG C, drying time 1～2 hours.
Method the most according to claim 1, is characterized in that, in described step (5), sputtering pressure is 2 × 10-1～10 × 10-1Pa, sputtering current is 1～10mA, and sputtering time is 10～60s.
Method the most according to claim 1, is characterized in that, the pressure of argon is 0.1～1MPa.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106158063B (en) * | 2015-04-23 | 2018-01-19 | 中国科学院苏州纳米技术与纳米仿生研究所 | Carbon nanotube paper, its activation method and application for chemical electric power source electrode material |
| FR3072608B1 (en) * | 2017-10-20 | 2021-04-02 | Commissariat Energie Atomique | MULTI-LAYER STRUCTURE INTEGRATING A CARBON NANOTUBES MAT AS A DIFFUSION LAYER IN A PEMFC |
| CN108335916A (en) * | 2017-12-20 | 2018-07-27 | 肇庆市华师大光电产业研究院 | A kind of multi-walled carbon nanotube@X combination electrodes and its preparation method and application |
| CN109273730A (en) * | 2018-08-09 | 2019-01-25 | 浙江润涞科技服务有限公司 | A kind of preparation method of hydrogen cell electrode material |
| CN111342061B (en) * | 2018-12-18 | 2021-08-31 | 中国科学院大连化学物理研究所 | Core-shell fiber structure electrode and preparation method and application thereof |
| CN112916865A (en) * | 2021-01-22 | 2021-06-08 | 北京化工大学 | Method for preparing carbon nano tube loaded metal monoatomic by flame reduction |
| CN114695904A (en) * | 2022-04-21 | 2022-07-01 | 浙江理工大学 | Preparation and application of self-supporting nitrogen-doped carbon nanotube-loaded platinum nano cluster |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1472135A (en) * | 2002-07-29 | 2004-02-04 | ����Sdi��ʽ���� | Carbon nanometer for fuel battery, its preparing method and fuel battery therewith |
| CN101515648A (en) * | 2009-03-19 | 2009-08-26 | 同济大学 | Novel membrane electrode component available for fuel cell, preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1472135A (en) * | 2002-07-29 | 2004-02-04 | ����Sdi��ʽ���� | Carbon nanometer for fuel battery, its preparing method and fuel battery therewith |
| CN101515648A (en) * | 2009-03-19 | 2009-08-26 | 同济大学 | Novel membrane electrode component available for fuel cell, preparation method and application thereof |
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