CN103259023A - Preparation method of hydrogen cell electrode material - Google Patents
Preparation method of hydrogen cell electrode material Download PDFInfo
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- CN103259023A CN103259023A CN2012104509539A CN201210450953A CN103259023A CN 103259023 A CN103259023 A CN 103259023A CN 2012104509539 A CN2012104509539 A CN 2012104509539A CN 201210450953 A CN201210450953 A CN 201210450953A CN 103259023 A CN103259023 A CN 103259023A
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Abstract
The invention relates to a preparation method of fuel cell electrode material, especially relates to a method for growing carbon nanotube (CNT) on carbon paper surface and carrying platinum (Pt). The method comprises the following technology steps: (1) depositing a layer of catalyst for growing carbon nanotube on the carbon paper by an ion sputtering method; (2) growing carbon nanotube on the carbon paper surface by plasma-enhanced chemical vapor deposition; (3) depositing platinum catalyst on the carbon nanotube by the ion sputtering method with the carbon nanotube grown carbon paper.
Description
Technical field
The present invention relates to the electrode material preparation method for fuel cell, particularly a kind of carbon fiber paper surface in situ growth for Proton Exchange Membrane Fuel Cells carries platinum carbon nanometer tube and preparation method thereof.
Background technology
Fuel cell is the device that directly chemical energy is changed into low-voltage DC by fuel and oxidant generation electrochemical reaction.Fuel cell is acknowledged as the cleaning of 21 century first-selection, generation technology efficiently, and its development has become the focus of international energy area research with exploitation, and will promote the fast development of whole electric automobile, submarine and power generation industries.
Up to the present, researched and developed polytype fuel cell, wherein Proton Exchange Membrane Fuel Cells (PEMFC) be after alkaline fuel cell, phosphoric acid type fuel cell, fused carbonate type fuel cell and Solid Oxide Fuel Cell the 5th generation fuel cell.Owing to used the solid electrolyte polymeric membrane as electrolyte, had the startup of energy transformation ratio high and low temperature, the leakage of no electrolytic cell, long, the high outstanding advantage of specific power of no burn into life-span.The research of PEMFC has become the main flow in all types of fuel cells research spring tides, is to be hopeful the business-like fuel cell of the fastest realization.
Carbon nano-tube has unique one dimension tubular graphene structure, and specific area is big, resistance is low, chemical stability is high, is the ideal carrier of nanocatalyst.The noble metal nano particles that will have unique catalytic performance loads on the surface of carbon nano-tube, and the noble metal nano particles/carbon mano-tube composite of formation not only has the excellent properties of two kinds of nano materials concurrently, also may produce new characteristic.Making catalyst carrier with carbon nano-tube can increase catalyst loadings, and also obviously improve in the decentralization of platinum and activated centre on the carrier.Carbon nano-tube mechanical strength height can form inierpeneirating network structure in Catalytic Layer, improved the intensity of Catalytic Layer, is conducive to improve the durability of membrane electrode fuel cell, and compares with traditional material with carbon element, and the dynamic behavior that electronics shifts in the carbon nano-tube is best.Therefore carbon nano-tube has good application prospects aspect fuel-cell catalyst carrier.
Patent is " directly in carbon paper superficial growth carbon nano-tube, again by carbon nanotube electrode and the manufacture method thereof of CVD method at the supporting platinum-based nanocatalyst of its carbon nano tube surface ", the patent No. 200710198794.7, also propose in carbon paper superficial growth carbon nano-tube and carry platinum to make the fuel cell electrode material, its preparation method is that (1) is immersed in preliminary treatment and dry in the aqueous sulfuric acid with carbon paper; (2) carbon paper after will handling is dipped in the electric spheroid aqueous solution of nickel, cobalt, iron compound or its mixture, carries out ultrasonic wave repeatedly and handles, and makes above-mentioned metal be evenly distributed on the carbon paper surface; (3) there is the carbon paper surface of catalyst metals to feed the gas phase carbon source in load, keeps suitable temperature and pressure, carbon nano-tube; (4) from carbon nanotubes grown, remove nickel, cobalt, iron or its mixture metal, and carbon nano-tube is carried out surface treatment; (5) on the carbon paper of carbon nano-tube of having grown, feed gas phase platinum electricity spheroid, keep certain temperature and pressure, supporting platinum-based nanocatalyst.
This patent method is that (1) adopts the ion sputtering method at the catalyst of carbon fiber paper surface sputtering one deck nickel, iron or its mixture, feeds argon shield in the sputter procedure; (2) feed H on the carbon paper surface
2, keep suitable temperature and pressure, catalyst is fully reduced; (3) surface of the carbon paper after reduction is handled feeds the gas phase carbon source, keeps suitable temperature and pressure, carbon nano-tube under certain radio-frequency power and bias voltage; (4) will grow that the carbon paper of carbon nano-tube soaks and dry in hydrochloric acid solution, except metals such as de-iron, nickel; (5) will the grow carbon paper of carbon nano-tube carries out the sputter of platinum target ion, load platinum catalyst under argon gas atmosphere.This patent method of operation is simple, carbon paper need not preliminary treatment, owing to used means such as plasma enhancing and bias voltage in the carbon nano tube growth process, carbon nano tube growth density is big, uniform diameter, it is little that platinum grain is carried in ion sputtering, be evenly distributed in carbon nano tube surface, can obtain better catalytic performance.
Patent " low-platinum high active core-shell structure catalyst and preparation method thereof ", the patent No. 200910117488.5 cover platinum on the Metal Substrate kernel and form nucleocapsid structure, and are carried on carbon dust or the carbon nanotube carrier.Patent " carbon nano-tube is carried platinum electrode Preparation of catalysts method ", it is carrier that patent No. 02155255.X adopts carbon nano-tube, and the chloroplatinic acid reduce deposition is prepared the Pt/CNTs catalyst on carbon nano-tube.Patent " carbon nano-tube is carried the preparation method of the anti-CO electrode catalyst of platinum ruthenium ", the patent No. 02155256.8 are carrier with the carbon nano-tube, use in-situ chemical homogeneous deposition method, with Pt, Ru, the isoionic metastable state colloid of Sn reduce deposition on carbon nano-tube.Patent " a kind of preparation method of catalyst of carbon multi-wall nano tube loaded metal platinum nano particle of surface nitrile-group modification ", the patent No. 201010168318.2 adopts the multi-walled carbon nano-tubes of surface nitrile-group modification as carrier, be reducing agent with alcohol, with the chloroplatinic acid reduce deposition on carbon nano-tube.Patent " a kind of platinum/carbon nano-tube catalyst and method for making and application ", the patent No. 200910236390.1 are dipped in carbon nano-tube and stir dipping in the chloroplatinic acid aqueous solution, and grind dry back, adds thermal reduction with aqueous sodium formate solution, obtains the platinum/carbon nano-tube catalyst.Patent " a kind of fuel battery cathod catalyst that is applicable to the high stability of dynamic operation condition ", the patent No. 200910248845.1 is carried out preliminary treatment with commercially available carbon nano-tube, supports active component then, obtains the carbon nano-tube platinum catalyst.Patent " a kind of preparation method of carbon nano tube loaded cobalt-platinum alloy catalyst ", the patent No. 200810224481.9 is to contain cobalt.The carbon nano-tube work electrode of platinum base active matter precursor is negative electrode, is anode with the platinum electrode, is electrolyte with the solid phase electrolytic salt, and adopting pulse electrodeposition was to generate carbon nano tube loaded cobalt-platinum alloy catalyst originally.Patent " a kind of fuel battery cathode with proton exchange film Preparation of catalysts method ", the patent No. 200910085170.3 is distributed to carbon nano-tube in two book solution, adopts formic acid reducing process supporting Pt to generate catalyst.Patent " being used for carbon nano-tube platinum catalyst of fuel cell and preparation method thereof ", the patent No. 200410009870.1 is carried out preliminary treatment to carbon nano-tube earlier, adopts formaldehyde reduction method for preparing Pt/MWNTs catalyst then.This patent method is directly at carbon paper surface in situ carbon nano-tube, and adopts the ion sputtering method to prepare Pt nanoparticle in carbon nano tube surface, and the preparation method is different with above-mentioned patent.
Summary of the invention
The purpose of this invention is to provide a kind of catalyst good dispersion, used in proton exchange membrane fuel cell platinum/carbon nano-tube/carbon fiber paper electrode material that catalytic activity is high.
Another object of the present invention provides a kind of method of producing Proton Exchange Membrane Fuel Cells platinum/carbon nano-tube/carbon fiber paper electrode material in batches and being assembled into monocell.
Platinum/carbon nano-tube for fuel cell of the present invention/carbon fiber paper electrode material is to be carrier with the carbon fiber paper, in-situ growing carbon nano tube, and be carrier with the carbon nano-tube, the sputter platinum catalyst.Wherein, the diameter of carbon nano-tube is 20～40nm, and the diameter of platinum grain is 2～4nm, and platinum grain is dispersed in carbon nano tube surface.
Platinum/carbon nano-tube for fuel cell of the present invention/carbon fiber paper electrode preparation methods is earlier at carbon fiber paper surface sputtering nickel, iron catalyst, using plasma strengthens chemical vapour deposition technique (PECVD) in-situ growing carbon nano tube then, at carbon nano tube surface sputter platinum catalyst, this method may further comprise the steps at last:
(1) sputter nickel, iron catalyst: adopt the ion sputtering method at the catalyst film of carbon fiber paper surface sputtering one deck nickel or iron, feed argon shield in the sputter procedure;
(2) catalyst reduction: the carbon fiber paper that obtains after step (1) handled is at H
2Under the atmosphere, 200～1000 ℃ were reduced 0.5～5.0 hour;
(3) carbon nano-tube: the product that step (2) is obtained is at H
2And CH
4Under the atmosphere, handled 0.5～5 hour for 600～1000 ℃, make carbon fiber paper surface in situ carbon nanotubes grown, be cooled to back below 100 ℃ and take out;
(4) the resulting product of step (3) is soaked also drying in hydrochloric acid solution, except metals such as de-iron, nickel;
(5) the resulting product of step (4) is carried out the ion sputtering of Pt nanoparticle under argon gas atmosphere.
Adopt the method for the invention big in the epontic carbon nanotube density of carbon paper, be evenly distributed, be combined with carbon fiber paper firmly, caliber is 20～40nm, can realize the good dispersion of platinum grain, the platinum grain diameter is 2～4nm, shows catalytic performance preferably.
Utilize this method to prepare the fuel cell electrode material, avoided the dispersion steps of carbon nano-tube, operating process is simple, and carbon nano-tube and carbon fiber paper high base strength have been increased, improved the dispersiveness of platinum catalyst in carbon nano tube surface, improve the utilance of platinum catalyst, realized the batch process of proton exchange membrane fuel cell electrode material.
The shape characteristic of the used in proton exchange membrane fuel cell platinum/carbon nano-tube/carbon fiber paper electrode material of the inventive method preparation characterizes with ESEM (SEM).
Description of drawings
Fig. 1 is the stereoscan photograph of platinum/carbon nano-tube/carbon fiber paper.
Embodiment
Embodiment 1:
(1) sputter Raney nickel: adopt the ion sputtering method at carbon fiber paper surface sputtering one deck Raney nickel film, feed argon shield in the sputter procedure, the pressure of argon gas is 0.1～1MPa, and sputter pressure is 2～10 * 10
-1Pa, sputtering current are 1～10mA, and sputtering time is 5～60min;
(2) catalyst reduction: the carbon fiber paper that obtains after step (1) handled is at H
2Reduced H under the atmosphere 0.5～5 hour
2Pressure is 100～1000Pa, H
2Flow is 10～100sccm;
(3) product that step (2) is obtained is at H
2And CH
4Handled under the atmosphere 0.5～5 hour, and made carbon fiber paper surface in situ carbon nanotubes grown, be cooled to back below 100 ℃ and take out, the pressure of gas is 100～1000Pa, H
2Flow is 10～100sccm, CH
4Flow is 10～100sccm, and radio-frequency power is 0～200W, and back bias voltage is 0V;
(4) the resulting product of step (3) is soaked also drying in the 2mol/L hydrochloric acid solution, except metals such as de-iron, nickel;
(5) the resulting product of step (4) is carried out the ion sputtering of platinum grain under argon gas atmosphere, the pressure of argon gas is 0.1～1MPa, and sputter pressure is 2～10 * 10
-1Pa, sputtering current are 1～10mA, and sputtering time is 10～60s.
Embodiment 2:
(1) sputter Raney nickel: adopt the ion sputtering method at carbon fiber paper surface sputtering one deck Raney nickel film, feed argon shield in the sputter procedure, the pressure of argon gas is 0.1～1MPa, and sputter pressure is 2～10 * 10
-1Pa, sputtering current are 1～10mA, and sputtering time is 5～60min;
(2) catalyst reduction: the carbon fiber paper that obtains after step (1) handled is at H
2Reduced H under the atmosphere 0.5～5 hour
2Pressure is 100～1000Pa, H
2Flow is 10～100sccm;
(3) product that step (2) is obtained is at H
2And CH
4Handled under the atmosphere 0.5～5 hour, and made carbon fiber paper surface in situ carbon nanotubes grown, be cooled to back below 100 ℃ and take out, the pressure of gas is 100～1000Pa, H
2Flow is 10～100sccm, CH
4Flow is 10～100sccm, and radio-frequency power is 0～200W, and back bias voltage is 25V;
(4) the resulting product of step (3) is soaked also drying in the 2mol/L hydrochloric acid solution, except metals such as de-iron, nickel;
(5) the resulting product of step (4) is carried out the ion sputtering of platinum grain under argon gas atmosphere, the pressure of argon gas is 0.1～1MPa, and sputter pressure is 2～10 * 10
-1Pa, sputtering current are 1～10mA, and sputtering time is 10～60s.
Embodiment 3:
(1) sputter iron catalyst: adopt the ion sputtering method at carbon fiber paper surface sputtering one deck iron catalyst film, feed argon shield in the sputter procedure, the pressure of argon gas is 0.1～1MPa, and sputter pressure is 2～10 * 10
-1Pa, sputtering current are 1～10mA, and sputtering time is 5～60min;
(2) catalyst reduction: the carbon fiber paper that obtains after step (1) handled is at H
2Reduced H under the atmosphere 0.5～5 hour
2Pressure is 100～1000Pa, H
2Flow is 10～100sccm;
(3) product that step (2) is obtained is at H
2And CH
4Handled under the atmosphere 0.5～5 hour, and made carbon fiber paper surface in situ carbon nanotubes grown, be cooled to back below 100 ℃ and take out, the pressure of gas is 100～1000Pa, H
2Flow is 10～100sccm, CH
4Flow is 10～100sccm, and radio-frequency power is 0～200W, and back bias voltage is 50V;
(4) the resulting product of step (3) is soaked also drying in the 2mol/L hydrochloric acid solution, except metals such as de-iron, nickel;
(5) the resulting product of step (4) is carried out the ion sputtering of platinum grain under argon gas atmosphere, the pressure of argon gas is 0.1～1MPa, and sputter pressure is 2～10 * 10
-1Pa, sputtering current are 1～10mA, and sputtering time is 10～60s.
Embodiment 4:
(1) sputter iron catalyst: adopt the ion sputtering method at carbon fiber paper surface sputtering one deck iron catalyst film, feed argon shield in the sputter procedure, the pressure of argon gas is 0.1～1MPa, and sputter pressure is 2～10 * 10
-1Pa, sputtering current are 1～10mA, and sputtering time is 5～60min;
(2) catalyst reduction: the carbon fiber paper that obtains after step (1) handled is at H
2Reduced H under the atmosphere 0.5～5 hour
2Pressure is 100～1000Pa, H
2Flow is 10～100sccm;
(3) product that step (2) is obtained is at H
2And CH
4Handled under the atmosphere 0.5～5 hour, and made carbon fiber paper surface in situ carbon nanotubes grown, be cooled to back below 100 ℃ and take out, the pressure of gas is 100～1000Pa, H
2Flow is 10～100sccm, CH
4Flow is 10～100sccm, and radio-frequency power is 0～200W, and back bias voltage is 75V;
(4) the resulting product of step (3) is soaked also drying in the 2mol/L hydrochloric acid solution, except metals such as de-iron, nickel;
(5) the resulting product of step (4) is carried out the ion sputtering of platinum grain under argon gas atmosphere, the pressure of argon gas is 0.1～1MPa, and sputter pressure is 2～10 * 10
-1Pa, sputtering current are 1～10mA, and sputtering time is 10～60s.
Claims (9)
1. platinum/carbon nano-tube/carbon fiber paper electrode material that is used for fuel cell is characterized in that: be carrier with the carbon fiber paper, and in-situ growing carbon nano tube, and be carrier with the carbon nano-tube, be catalyst with platinum, platinum grain is dispersed in the surface of carbon nano-tube uniformly.
2. catalyst according to claim 1, it is characterized in that: the diameter of described carbon nano-tube is 20～40nm, the diameter of platinum grain is 2～4nm.
3. one kind according to each described platinum/carbon nano-tube for fuel cell/carbon fiber paper electrode preparation methods of claim 1～2, it is characterized in that this method may further comprise the steps:
(1) adopts the ion sputtering method at the catalyst film of carbon fiber paper surface sputtering one deck nickel or iron, feed argon shield in the sputter procedure;
(2) carbon fiber paper that obtains after step (1) is handled is at H
2Under the atmosphere, 200～1000 ℃ were reduced 0.5～5.0 hour;
(3) product that step (2) is obtained is at H
2And CH
4Under the atmosphere, handled 0.5～5 hour for 600～1000 ℃, make carbon fiber paper surface in situ carbon nanotubes grown, be cooled to back below 100 ℃ and take out;
(4) product that step (3) is obtained soaks in hydrochloric acid solution and is dry, except metals such as de-iron, nickel;
(5) the resulting product of step (4) is carried out the ion sputtering of platinum grain under argon gas atmosphere;
4. method according to claim 3 is characterized in that, sputter pressure is 2～10 * 10 in the described step (1)
-1Pa, sputtering current are 1～10mA, and sputtering time is 5～60min.
5. method according to claim 3 is characterized in that, H in the described step (2)
2Pressure is 100～1000Pa, H
2Flow is 10～100sccm.
6. method according to claim 3 is characterized in that, the pressure of gas is 100～1000Pa in the described step (3), H
2Flow is 10～100sccm, CH
4Flow is 10～100sccm, and radio-frequency power is 0～200W, and back bias voltage is 0～100V.
7. method according to claim 3 is characterized in that, the concentration of hydrochloric acid is 2mol/L in the described step (4), soak time 12～24 hours, 100～120 ℃ of baking temperatures, 1～2 hour drying time.
8. method according to claim 3 is characterized in that, sputter pressure is 2～10 * 10 in the described step (5)
-1Pa, sputtering current are 1～10mA, and sputtering time is 10～60s.
9. method according to claim 3 is characterized in that, the pressure of argon gas is 0.1～1MPa.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106158063A (en) * | 2015-04-23 | 2016-11-23 | 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 |
| 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 |
| EP3474356A1 (en) * | 2017-10-20 | 2019-04-24 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Multilayer structure incorporating a carbon nanotube mat as the scattering layer in a pemfc |
| CN111342061A (en) * | 2018-12-18 | 2020-06-26 | 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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| 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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Patent Citations (2)
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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 |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106158063A (en) * | 2015-04-23 | 2016-11-23 | 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 |
| 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 |
| EP3474356A1 (en) * | 2017-10-20 | 2019-04-24 | Commissariat à l'Energie Atomique et aux Energies Alternatives | Multilayer structure incorporating a carbon nanotube mat as the scattering layer in a pemfc |
| FR3072608A1 (en) * | 2017-10-20 | 2019-04-26 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | MULTILAYER STRUCTURE INTEGRATING CARBON NANOTUBE MATS AS A DIFFUSION LAYER IN PEMFC |
| US11271220B2 (en) | 2017-10-20 | 2022-03-08 | Commissariat A L'energie Atomique Et Aux Energies Alternatives | Multilayer structure incorporating a mat of carbon nanotubes as 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 |
| CN111342061A (en) * | 2018-12-18 | 2020-06-26 | 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 |
| 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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| CN103259023B (en) | 2016-09-14 |
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