CN101814607A - Preparation method of platinum/graphen catalyst for proton exchange membrane fuel cell - Google Patents
Preparation method of platinum/graphen catalyst for proton exchange membrane fuel cell Download PDFInfo
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Abstract
The invention discloses a preparation method of a platinum/graphen catalyst for a proton exchange membrane fuel cell. The platinum/graphen catalyst for the proton exchange membrane fuel cell is prepared by adopting graphen as a carrier, taking sodium borohydride or ethylene glycol as a reducing agent, and reducing oxidized graphite and chloroplatinic acid together, and the platinum loading capacity of the catalyst is between 10 and 60 weight percent. The catalyst has the initial electrochemical activity superficial area of 4.75 m<2>/g, and the performance attenuation of 18.4 percent in 3,000 times of cyclic volt-ampere tests. Compared with the conventional commercial catalyst platinum/XC-72 (having the attenuation of 44.5 percent) of E-TEK Company, the catalyst shows higher electrochemical stability.
Description
Technical field
The present invention relates to the method for preparing catalyst that a kind of fuel cell is used, particularly a kind of preparation method of used in proton exchange membrane fuel cell platinum/graphen catalyst.
Background technology
Advantages such as that Proton Exchange Membrane Fuel Cells (PEMFC) has is simple in structure, start-up time is short show good prospects for application in recent years.But PEMFC will reach real commercial applications also needs to solve problems such as catalyst cost and stability.Improve catalyst support structures, it is favourable that catalyst is improved stability.All kinds of conductive carbon materials are used as electro-catalyst carrier as carbosphere, multi-walled carbon nano-tubes, Single Walled Carbon Nanotube etc., in the hope of improving its stability.
That be most widely used at present is commodity conductive black XC-72, as U.S. Pat 3,857, adopt infusion process that the platinum ammino is closed ion load to XC-72 in 737, U.S. Pat 4,044,193 and Japan Patent JP99-47595 adopt the precipitation method that platinum oxygen gel is loaded on the XC-72, Chinese patent CN1915521A adopts solid phase method that platinum is carried on the XC-72, from report, find out, platinum/XC-72 the catalyst that is carried on this carrier has electrocatalysis characteristic preferably, but the stability of platinum/XC-72 catalyst is not reported.During rolling up 145 pages in 2007 172, Journal of Power Sources magazine reported present situation about platinum/C catalyst stability, to XC-72, carrier materials such as carbon nano-tube are discussed, think that the stability of carrier is great to the catalyst stability influence, article is pointed out, under the fuel battery operation environment (greater than 0.6 volt, room temperature and above operating temperature) obvious loss can appear in carbon carrier, this is owing to carbon carrier under this condition can generate carbon dioxide or carbon monoxide, the reunion of simultaneous metallic particles, catalyst activity can show very big decay, after 170 hours, platinum/C catalyst the decay of activity that with XC-72 is carrier is 80%, is that the platinum/C catalyst decay of activity of carrier is 30% with the carbon nano-tube.Therefore, the stability of catalyst be improved, more stable carrier need be selected for use.
Geim pointed out during the Science magazine was rolled up 1530 pages in 2009 324, and Graphene is to have the material with carbon element that is less than 10 layers of graphite molecule layer structure, and specific area is higher, and (the theoretical specific area of single-layer graphene can reach 2620m
2/ g), can provide more life to belong to load byte.Simultaneously, Graphene shows very strong quantum effect, has the good electron conducting power.Calculate to find that by first principle platinum bunch can stably be carried on the Graphene, and carbon monoxide or hydrogen can reduce at the energy of adsorption that life belongs on the platinum grain, are more conducive to the reaction in the fuel cell because of the existence of Graphene.Therefore, Graphene can be used as a good carbon carrier.
Be initial activity and the preparation method of the relevant report of the platinum/graphen catalyst instrument of reducing agent preparation at catalyst with sodium borohydride or ethylene glycol at present, catalyst stability does not still have investigation.The related content that does not also prepare in the patent about platinum/graphen catalyst.
Reported a kind of preparation method of platinum/graphen catalyst during The Journal of Physical Chemistry C magazine was rolled up 7990 pages in 2009 113, the researcher reduces when pH=2, obtains the 50wt% platinum/graphen catalyst.
The platinum/graphen catalyst of report needed under pH=10 reductase 12 4 hours in 846 pages of Electrochemistry Communications magazine 2009 11 volumes, and 40 ℃ of oven dry down, obtained the platinum/graphen catalyst of 45wt%.
2008 112 volumes of The Journal of Physical Chemistry C magazine have been reported the method that a kind of spent glycol method reduction prepares platinum/graphen catalyst for 19841 pages, are used for the methanol electro-oxidizing reaction.
The platinum/graphen catalyst of 954 pages of reports of 2009 11 volumes of Electrochemistry Communications magazine is the reducing agent preparation with the high-temperature hydrogen, at cyclic voltammetric test rear catalyst performance degradation is 37.6%, shows the stability that is better than commercial catalysts.
Summary of the invention
The objective of the invention is to prepare a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell, wherein the platinum carrying capacity is 10wt%-60wt%.This catalyst uses Graphene to be carrier, utilizes distinctive quantum effect of Graphene and two-dimentional ductility, to improve the stability of catalyst.By chloroplatinic acid and graphite oxide are carried out blend, use sodium borohydride or ethylene glycol to carry out coreduction as reducing agent, by regulating the activity of recovery time control catalyst, have the more catalyst of fuel batter with proton exchange film of high stability thereby prepare.
The preparation method of a kind of used in proton exchange membrane fuel cell platinum/graphen catalyst of the present invention is as follows, below all represents with mass parts:
A. sodium borohydride reduction method: get that graphite oxide is ultrasonic to be scattered in the graphite oxide dispersion liquid 1000-20000 part that forms 0.05wt%-1wt% in the deionized water, adding 2.66-15.93 part chloroplatinic acid mixes, making platinum carrying capacity in platinum/graphen catalyst is 10wt%-60wt%, regulate the pH value to 9-13 with the 0.5M-4M potassium hydroxide aqueous solution, add 160-640 part sodium borohydride and 5000-10000 part deionized water, reduced 1-18 hour, suction filtration then, and use deionized water wash, 60-100 ℃ dry 6-24 hour, obtain a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell;
Or B. reduction of ethylene glycol method: get the ultrasonic graphite oxide dispersion liquid 1000-20000 part that is scattered in formation 0.05wt%-1wt% in the ethylene glycol of graphite oxide, adding 2.66-15.93 part chloroplatinic acid mixes, making platinum carrying capacity in platinum/graphen catalyst is 10wt%-60wt%, regulate the pH value to 9-13 with 0.5M-4M potassium hydroxide ethylene glycol solution, 90-150 ℃ was reduced 3-12 hour down, suction filtration then, and use deionized water wash, with product 60-100 ℃ dry 6-24 hour, obtain a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell.
The raw material graphite oxide is according to 771 pages of reported in literature preparations of 1999 11 volumes of Chemistry ofMaterials magazine among the present invention, concrete preparation method is as follows: with 1 part of graphite dispersed with stirring in 80 parts of 98wt% concentrated sulfuric acids, adding 4.5 parts of potassium permanganate under 25 ℃ of water bath condition reacts, react after 5 days, add deionized water and 10 parts of 30wt% aqueous hydrogen peroxide solution cessation reactions, centrifugal then, and with deionized water wash 16 times, 80 ℃ of dryings obtained graphite oxide in 24 hours.
Among the preparation method of a kind of used in proton exchange membrane fuel cell platinum/graphen catalyst of the present invention, the employing Graphene is a carrier, utilize the distinctive quantum effect of Graphene to form electric negative center on the Graphene surface, in catalyst preparation process, adsorb platinum particles, make platinum particles can more stably be carried on carrier surface, be difficult for migration; Owing to the very big specific area of Graphene, the platinum particles of load is difficult for being in contact with one another reunion, can keep the catalytic activity of catalyst better simultaneously.A kind of used in proton exchange membrane fuel cell platinum/graphen catalyst for preparing among the present invention is 18.4% at 3000 cyclic voltammetrics test rear catalyst performance degradations, 44.5% is had better stability than what the commercial catalysts platinum/XC-72 of E-TEK company showed.
Description of drawings
Fig. 1 a kind of used in proton exchange membrane fuel cell platinum/graphen catalyst that to be embodiment 3 obtain with Comparative Examples 1 and the cyclic voltammogram of platinum/XC-72 catalyst.
Fig. 2 is that embodiment 3 contrasts with a kind of used in proton exchange membrane fuel cell platinum/graphen catalyst and the platinum/XC-72 catalyst performance decay that Comparative Examples 1 obtains.
Embodiment
The following examples help further to elaborate the present invention, and should not be interpreted as limiting the scope of the invention.
The detection method of the electro-chemical activity surface area of a kind of used in proton exchange membrane fuel cell platinum/graphen catalyst that the present invention obtains and stability is finished by carry out the cyclic voltammetric test in the standard three-electrode system.Adopt the platinum filament conduct to electrode, saturated calomel electrode (SCE) is as reference electrode, and the glass-carbon electrode of diameter 3mm is a work electrode, and electrolyte is the 0.5mol/L sulfuric acid solution.Test is carried out in CH50A (Shanghai occasion China company) system, and specific operation process is: accurately take by weighing the 5mg catalyst powder, add 50 μ l 5wt%
(Du Pont company) solution, ultrasonic being scattered in the 1ml deionized water.Pipetting 6 μ l drips in glass-carbon electrode surface, drying at room temperature.In immersing three electrode sulfuric acid system, feed earlier argon gas half an hour before the test, in 0.8V (SCE) interval, carry out repeatedly cyclic voltammetry scan at-0.2V with the sweep speed of 50mV/s, stable until curve, and be translated into numerical value with respect to standard hydrogen electrode (SHE).The electrochemical stability property testing is also finished in this three-electrode system.System is scanned up to stable, with the rate scanning of 50mV/s 3000 times.Each cyclic voltammetric data computation is obtained corresponding electro-chemical activity surface area.
Embodiment 1. sodium borohydride reduction methods
Get the ultrasonic graphite oxide dispersion liquid 2g that forms 0.45wt% in the deionized water that is scattered in of graphite oxide, add the 2.66mg chloroplatinic acid and mix, making platinum carrying capacity in platinum/graphen catalyst is 10wt%.Regulate pH value to 9 with the 0.5M potassium hydroxide aqueous solution, add 0.16g sodium borohydride and 5g deionized water, reduced 1 hour, suction filtration then, and use deionized water wash, 100 ℃ of dryings 6 hours obtain a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell.Its electro-chemical activity surface area the results are shown in table 1.
Embodiment 2. sodium borohydride reduction methods
Get the ultrasonic graphite oxide dispersion liquid 16g that forms 0.05wt% in the deionized water that is scattered in of graphite oxide, add the 5.31mg chloroplatinic acid and mix, making platinum carrying capacity in platinum/graphen catalyst is 20wt%.Regulate pH of mixed value to 10 with the 4M potassium hydroxide aqueous solution, add 0.64g sodium borohydride and 10g deionized water, reductase 12 hour, suction filtration then, and use deionized water wash, 60 ℃ of dryings 24 hours obtain a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell.Its electro-chemical activity surface area the results are shown in table 1.
Embodiment 3. sodium borohydride reduction methods
Get the ultrasonic graphite oxide dispersion liquid 10g that forms 0.08wt% in the deionized water that is scattered in of graphite oxide, add the 5.31mg chloroplatinic acid and mix, making platinum carrying capacity in platinum/graphen catalyst is 20wt%.Regulate pH value to 10 with the 1M potassium hydroxide aqueous solution, adding 0.4g sodium borohydride and 5g deionized water reduced 4 hours, suction filtration then, and use deionized water wash, and 80 ℃ of dryings 12 hours obtain a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell.Its electro-chemical activity surface area the results are shown in table 1, the electro-chemical activity cyclic voltammetric test result after initial electro-chemical activity and the circulation as shown in Figure 1, catalyst performance is decayed as shown in Figure 2.
Table 1 and Fig. 1 have illustrated the electro-chemical activity after platinum/XC-72 catalyst and the initial electro-chemical activity of platinum/graphen catalyst and 3000 circulations, and wherein, the initial value of platinum/XC-72 catalyst electro-chemical activity surface area is 54.94m
2/ g, the circulation back is 30.26m
2/ g, the initial value of platinum/graphen catalyst electro-chemical activity surface area is 47.54m
2/ g, the circulation back is 38.8m
2/ g, visible platinum/graphen catalyst has higher electro-chemical activity after circulation.
Initial electro-chemical activity surface area ratio platinum/the XC-72 catalyst is little though Fig. 2 has illustrated the prepared platinum/graphen catalyst of the present invention, but in 3000 cyclic voltammetric test operations, has higher stability, platinum/graphen catalyst instrument decay 18.4%, and platinum/XC-72 catalyst performance decays to 44.5%, illustrates that platinum/graphen catalyst more is applicable to Proton Exchange Membrane Fuel Cells.
Embodiment 4. sodium borohydride reduction methods
Get the ultrasonic graphite oxide dispersion liquid 12g that forms 0.05wt% in the deionized water that is scattered in of graphite oxide, add the 10.62mg chloroplatinic acid and mix, making platinum carrying capacity in platinum/graphen catalyst is 40wt%.Regulate pH value to 13 with the 1M potassium hydroxide aqueous solution, add 0.64g sodium borohydride and 5g deionized water, reduced 18 hours, suction filtration then, and use deionized water wash, 80 ℃ of dryings 12 hours obtain a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell.Its electro-chemical activity surface area the results are shown in table 1.
Embodiment 5. sodium borohydride reduction methods
Get the ultrasonic graphite oxide dispersion liquid 4g that forms 0.1wt% in the deionized water that is scattered in of graphite oxide, add the 15.93mg chloroplatinic acid and mix, making platinum carrying capacity in platinum/graphen catalyst is 60wt%.Regulate pH value to 10 with the 4M potassium hydroxide aqueous solution, add 0.64g sodium borohydride and 7.5g deionized water, reduced 4 hours, suction filtration then, and use deionized water wash, 80 ℃ of dryings 18 hours obtain a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell.Its electro-chemical activity surface area the results are shown in table 1.
Embodiment 6. reduction of ethylene glycol methods
Get the ultrasonic graphite oxide dispersion liquid 16g that forms 0.05wt% in the ethylene glycol that is scattered in of graphite oxide, add the 5.31mg chloroplatinic acid and mix, making platinum carrying capacity in platinum/graphen catalyst is 20wt%.Regulate pH value to 9 with 0.5M potassium hydroxide ethylene glycol solution, 90 ℃ were reduced 3 hours down, and suction filtration then, and use deionized water wash with 100 ℃ of dryings of product 6 hours, obtains a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell.Its electro-chemical activity surface area the results are shown in table 1.
Embodiment 7. reduction of ethylene glycol methods
Get the ultrasonic graphite oxide dispersion liquid 1g that forms 0.4wt% in the ethylene glycol that is scattered in of graphite oxide, add the 15.93mg chloroplatinic acid and mix, making platinum carrying capacity in platinum/graphen catalyst is 60%.Regulate pH value to 13 with 4M potassium hydroxide ethylene glycol solution, 150 ℃ were reduced 12 hours down, and suction filtration then, and use deionized water wash with 80 ℃ of dryings of product 24 hours, obtains a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell.Its electro-chemical activity surface area the results are shown in table 1.
Comparative Examples 1
The catalyst that uses in the Comparative Examples is the commercial platinum/C catalyst of E-TEK company, its carrier is XC-72, the platinum carrying capacity is 20wt%, the electro-chemical activity surface area that uses above-mentioned method of testing to obtain the results are shown in table 1, electro-chemical activity cyclic voltammetric test result after initial electro-chemical activity and the circulation as shown in Figure 1, catalyst performance is decayed as shown in Figure 2.
Table 1
| Embodiment | Carrier | Platinum carrying capacity (wt%) | Reducing agent | PH value | Recovery time (h) | Electro-chemical activity surface area (m 2/g) |
| ??1 | Graphene | ??10 | Sodium borohydride | ??9 | ??1 | ??7.6 |
| ??2 | Graphene | ??20 | Sodium borohydride | ??10 | ??2 | ??11.8 |
| Embodiment | Carrier | Platinum carrying capacity (wt%) | Reducing agent | PH value | Recovery time (h) | Electro-chemical activity surface area (m 2/g) |
| ?3 | Graphene | ??20 | Sodium borohydride | ??10 | ??4 | ??47.5 |
| ?4 | Graphene | ??40 | Sodium borohydride | ??13 | ??18 | ??50.8 |
| ?5 | Graphene | ??60 | Sodium borohydride | ??10 | ??4 | ??62.4 |
| ?6 | Graphene | ??20 | Ethylene glycol | ??9 | ??3 | ??13.8 |
| ?7 | Graphene | ??40 | Ethylene glycol | ??13 | ??12 | ??45.3 |
| Comparative Examples 1 | ??XC-72 | ??20 | ??- | ??- | ??- | ??54.5 |
Claims (1)
1. the preparation method of a used in proton exchange membrane fuel cell platinum/graphen catalyst is characterized in that the preparation method is as follows, below all represents with mass parts:
A. sodium borohydride reduction method: get that graphite oxide is ultrasonic to be scattered in the graphite oxide dispersion liquid 1000-20000 part that forms 0.05wt%-1wt% in the deionized water, adding 2.66-15.93 part chloroplatinic acid mixes, making platinum carrying capacity in platinum/graphen catalyst is 10wt%-60wt%, regulate the pH value to 9-13 with the 0.5M-4M potassium hydroxide aqueous solution, add 160-640 part sodium borohydride and 5000-10000 part deionized water, reduced 1-18 hour, suction filtration then, and use deionized water wash, 60-100 ℃ dry 6-24 hour, obtain a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell;
Or B. reduction of ethylene glycol method: get the ultrasonic graphite oxide dispersion liquid 1000-20000 part that is scattered in formation 0.05wt%-1wt% in the ethylene glycol of graphite oxide, adding 2.66-15.93 part chloroplatinic acid mixes, making platinum carrying capacity in platinum/graphen catalyst is 10wt%-60wt%, regulate the pH value to 9-13 with 0.5M-4M potassium hydroxide ethylene glycol solution, 90-150 ℃ was reduced 3-12 hour down, suction filtration then, and use deionized water wash, with product 60-100 ℃ dry 6-24 hour, obtain a kind of platinum/graphen catalyst of used in proton exchange membrane fuel cell.
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