CN104752736A - Platinum-based catalyst having high catalytic activity and high durability and adopting porous carbon nano fiber as carrier and preparation method of platinum-based catalyst - Google Patents
Platinum-based catalyst having high catalytic activity and high durability and adopting porous carbon nano fiber as carrier and preparation method of platinum-based catalyst Download PDFInfo
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Abstract
The invention relates to a platinum-based catalyst having high catalytic activity and high durability and adopting porous carbon nano fibers as a carrier and a preparation method of the platinum-based catalyst, and particularly relates to a method of improving the catalytic activity and durability of a catalyst adopting a loose three-dimensional netted through structure composed of the porous carbon nano fibers as a carrier to load nano platinum particles and an application of the catalyst in a proton exchanging membrane fuel cell. According to the platinum-based catalyst adopting the porous carbon nano fibers as the carrier, the porous carbon nano fibers which are used as the carrier form a loose three-dimensional netted through structure, and metal platinum is loaded on the porous carbon nano fibers; the catalytic activity of the platinum-based catalyst adopting the porous carbon nano fibers as the carrier is as follows: the peak potential is 100mA ahead of that of a platinum-carbon catalyst, and the utilization rate of platinum reaches 80 percent; the durability of the platinum-based catalyst adopting the porous carbon nano fibers as the carrier is as follows: the ECSA retention rate after the fuel cell is circulated for 1000 times can reach 50 percent.
Description
Technical field
The invention belongs to catalyst technical field, relate to that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as platinum based catalyst of carrier and preparation method thereof and its application, the catalytic activity of used in proton exchange membrane fuel cell platinum carbon catalyst and the method for durability and application thereof is improved in particular to a kind of, specifically, that a kind of employing forms the catalyst of the loose three-dimensional netted structure run through as carrier loaded nano-platinum particle to improve the method for catalyst activity and durability and the application for Proton Exchange Membrane Fuel Cells thereof by porous carbon nanofiber.
Background technology
Proton Exchange Membrane Fuel Cells has outside clean pollution-free, the common feature that fuel cell has such as energy conversion rate is high due to it, also possess toggle speed fast, without electrolyte leakage and corrode the advantages such as low, become one of focus studied in world wide.Therefore at the society of showing great attention to environmental pollution and energy crisis, Proton Exchange Membrane Fuel Cells gets a good chance of using as follow-on novel battery, becomes the main force in energy field.
The core component membrane electrode assembly (MEA) of Proton Exchange Membrane Fuel Cells is electrochemical reaction place, and the performance of membrane electrode and its structure form close relationship, therefore improves film electrode structure composition significant to raising battery performance.Wherein as the catalyst of reaction electrode, price and lower activity, efficiency and the life-span of its costliness seriously govern performance and the development of fuel cell.Current research direction mainly contains two, reduces the consumption of the noble metal such as platinum, palladium, or to give precious metal alloys completely alternative, reduces the cost of catalyst and fuel cell with this, but the activity of the catalyst of the method reduction, reduce the performance of fuel cell.Another kind of scheme mainly through changing composition and the pattern of catalyst carrier, but because the load process of the preparation of carrier, catalyst is numerous and diverse, exist and pollute, and catalyst performance is unstable and fail commercialization.
Summary of the invention
Technical problem to be solved by this invention is to provide that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as platinum based catalyst of carrier and preparation method thereof and its application, particularly provide a kind of and improve the catalytic activity of used in proton exchange membrane fuel cell platinum carbon catalyst and the method for durability and application thereof, specifically, that a kind of employing forms the loose three-dimensional netted structure run through as carrier loaded platinum carbon catalyst to improve the method for platinum carbon catalyst catalytic activity and durability and the application for Proton Exchange Membrane Fuel Cells thereof by porous carbon nanofiber.
It is of the present invention that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as platinum based catalyst of carrier and preparation method thereof and its application, with porous carbon nanofiber and commercialization platinum carbon catalyst blended, using porous carbon nanofiber and carbon black as composite carbon carrier, improve platinum carbon catalyst catalytic activity and durability.The active site utilizing porous carbon nanofiber blemish to provide makes platinum grain be moved by carbon blacksurface and be fixed on porous carbon nanofiber surface.The pore structure that porous carbon nanofiber is abundant, and suitable draw ratio, not only increase catalyst activity, more in electrode structure, define loose layer structure, improve the life-span of catalyst, and reduce the mass transfer polarization of membrane electrode, thus further increase the power generation performance of fuel cell.
Of the present invention a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, and the porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, and porous carbon nanofiber is supported with metal platinum; Described take porous carbon nanofiber as the catalytic activity of the platinum based catalyst of carrier: play a spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art; Described take porous carbon nanofiber as the durability of the platinum based catalyst of carrier: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.The hole on porous carbon nanofiber surface and defect provide more active sites, can improve the catalytic activity of Pt nanoparticle; Meanwhile, the hole on porous carbon nanofiber surface and defect energy anchored platinum particle, improve the durability of catalyst.
As preferred technical scheme:
What have high catalytic activity and high-durability as above take porous carbon nanofiber as the platinum based catalyst of carrier, described porous carbon nanofiber is also supported with carbon black, and on carbon black, load has metal platinum.The hole on porous carbon nanofiber surface and defect are conducive to the dispersion of Pt nanoparticle, obviously can improve the dispersiveness of Pt nanoparticle, and porous carbon nanofiber can also disperse carbon black pellet simultaneously, further increases the dispersiveness of platinum.Dispersed improvement makes more Pt nanoparticles come out, and effectively can improve platinum utilization.
What have high catalytic activity and high-durability as above take porous carbon nanofiber as the platinum based catalyst of carrier, and the average fibre diameter of described porous carbon nanofiber is 100 ~ 1000 nanometers, and aperture is 5 ~ 100 nanometers, and Fiber Aspect Ratio is 5 ~ 30.Because porous carbon nanofiber has certain draw ratio, can effectively avoid catalyst tightly packed, when building electrode, porous carbon nanofiber forms a loose three-dimensional netted structure run through in the electrodes, be conducive to reducing resistance to mass tranfer, be conducive to the eliminating of product simultaneously, avoid catalyst water logging inactivation.
What have high catalytic activity and high-durability as above take porous carbon nanofiber as the platinum based catalyst of carrier, and in the platinum based catalyst taking porous carbon nanofiber as carrier, the content of described platinum is 10wt% ~ 40wt%.
What have high catalytic activity and high-durability as above take porous carbon nanofiber as the platinum based catalyst of carrier, in the platinum based catalyst taking porous carbon nanofiber as carrier, and the content≤50wt% of described carbon black.
Present invention also offers that a kind of that have high catalytic activity and high-durability take porous carbon nanofiber as the preparation method of the platinum based catalyst of carrier, by porous carbon nanofiber and platinum carbon catalyst common distribution in dispersant, ultrasonic process post-drying, namely obtain with porous carbon nanofiber be carrier take porous carbon nanofiber as the platinum based catalyst of carrier.
Preparation method as above, described dispersant is isopropyl alcohol or methyl alcohol; In described platinum carbon catalyst, platinum content is 15wt% ~ 60wt%, and all the other are carbon black; Particle diameter 20 ~ the 40nm of described platinum carbon catalyst; Described ultrasonic process refers to the frequency ultrasound process 0.5 ~ 4 hour with 50 hertz; Described oven dry refer at 40 ~ 120 DEG C of temperature dry 6 ~ 12 hours.
Invention further provides that a kind of that have high catalytic activity and high-durability take porous carbon nanofiber as the preparation method of the platinum based catalyst of carrier, is by the method for electronation, platinum is reducing loaded on carbon carrier porous carbon nanofiber with the form of nano particle by the presoma of platinum.As according to document [Songli Wei, Dingcai Wu, Xuelong Shang, Ruowen Fu, Studieson the Structure and Electrochemical Performance of Pt/Carbon Aerogel Catalyst for DirectMethanol Fuel Cells, Energy & Fuels, 23 (2009) 908 – 911] described in method.Platinum reduces and is carried on carbon aerogels by spent glycol liquid phase reduction from chloroplatinic acid.
Invention further provides a kind of monocell with porous carbon nanofiber obtained by the platinum based catalyst of carrier, be placed between anode and cathode flow-field plate by membrane electrode assembly and form, described membrane electrode assembly is sprayed at proton exchange membrane cathode side by the platinum based catalyst taking porous carbon nanofiber as carrier and anode-side obtains through hot pressing; Membrane electrode assembly resistance value is 200-500 ohm.
Monocell as above, the amount of described spraying is 0.2-0.8mg-Pt/cm
2; The temperature of described hot pressing is 50-150 DEG C.
Porous carbon nanofiber of the present invention provides the further dispersion of platinum, and can build loose catalyst layer mechanism when being applied to Proton Exchange Membrane Fuel Cells, is conducive to reducing resistance to mass tranfer.
Beneficial effect
1., by adding porous carbon nanofiber as composite carbon carrier, effectively raise catalyst activity, and oxygen reduction reaction speed, thus significantly improve catalyst use efficiency;
2. by adding porous carbon nanofiber as composite carbon carrier, can effectively build the catalyst layer with three-dimensional UNICOM structure, reducing the polarization of membrane electrode mass transfer, and catalyst granules is disperseed further, improve the power generation performance of fuel cell;
3. in the present invention, do not need to carry out extra load operation etc. to porous carbon nanofiber, therefore its technique is simple, easy to operate, is easy to commercialization;
4. porous carbon nanofiber of the present invention, with low cost, and preparation is simple, pollution-free.
5. the present invention is when building electrode, and porous carbon nanofiber forms the loose three-dimensional netted structure run through in the electrodes, is conducive to the eliminating of product, avoids catalyst water logging inactivation.
Accompanying drawing explanation
Fig. 1 is porous carbon nanofiber surface topography
Fig. 2 is porous carbon nanofiber cross-section morphology
Fig. 3 is that what obtained by chemical reduction method of the present invention take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 10%, Pt/PCNFs-10 surface topography
Fig. 4 is that what obtained by chemical reduction method of the present invention take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 40%, Pt/PCNFs-40 transmission electron microscope picture
Fig. 5 is that what obtained by chemical reduction method of the present invention take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 20%, Pt/PCNFs-20 transmission electron microscope picture
Fig. 6 is that what obtained by dispersion mixing method of the present invention take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 20%, Pt/PCNFs-20 transmission electron microscope picture
Fig. 7 take porous carbon nanofiber as the platinum based catalyst electrode surface pattern of carrier
Fig. 8 take porous carbon nanofiber as the platinum based catalyst electrode cross-section morphology of carrier
Fig. 9 take porous carbon nanofiber as the platinum based catalyst electrode cross-section morphology of carrier
Figure 10 different catalysts linear scan curve, wherein Pt/PCNFs-20 is that what obtained by dispersion mixing method of the present invention take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 20%; JM-20 is Johnson Matthey CorporationHiSPEC3000 platinum carbon catalyst; JM-40 is Johnson Matthey Corporation HiSPEC4000 platinum carbon catalyst.
Figure 11 different catalysts ECSA durability, wherein Pt/PCNFs-20 is that what obtained by chemical reduction method of the present invention take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 20%; Pt/Vulcan-20 is self-control platinum carbon catalyst, and platinum content is 20%; JM-20 is Johnson Matthey Corporation HiSPEC3000 platinum carbon catalyst.
Figure 12 monocell polarization curve, wherein Pt/PCNFs-20 is that what obtained by dispersion mixing method of the present invention take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 20%; JM-20 is Johnson Matthey Corporation HiSPEC3000 platinum carbon catalyst; JM-40 is Johnson Matthey Corporation HiSPEC4000 platinum carbon catalyst.
Embodiment
Below in conjunction with embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
It is of the present invention that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, wherein the content of platinum is 10wt%, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 100 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 5, porous carbon nanofiber is supported with metal platinum, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.
Embodiment 2
It is of the present invention that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, wherein the content of platinum is 40wt%, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 1000 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 30, porous carbon nanofiber is supported with metal platinum, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.
Embodiment 3
It is of the present invention that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, wherein the content of platinum is 20wt%, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 800 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 10, porous carbon nanofiber is supported with metal platinum, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.
Embodiment 4
It is of the present invention that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 100 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 30, porous carbon nanofiber is supported with metal platinum, also be supported with carbon black, and load has metal platinum on carbon black, in this platinum based catalyst, the content 50wt% of carbon black, the content of platinum is 40wt%, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.
Embodiment 5
It is of the present invention that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 1000 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 5, porous carbon nanofiber is supported with metal platinum, also be supported with carbon black, and load has metal platinum on carbon black, in this platinum based catalyst, the content 30wt% of carbon black, the content of platinum is 10wt%, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.
Embodiment 6
It is of the present invention that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 800 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 10, porous carbon nanofiber is supported with metal platinum, also be supported with carbon black, and load has metal platinum on carbon black, in this platinum based catalyst, the content 40wt% of carbon black, the content of platinum is 20wt%, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.
Embodiment 7
Monocell of the present invention, with porous carbon nanofiber obtained by the platinum based catalyst of carrier, be placed between anode and cathode flow-field plate by membrane electrode assembly and form, this porous carbon nanofiber is the platinum based catalyst of carrier, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, wherein the content of platinum is 10wt%, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 100 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 5, porous carbon nanofiber is supported with metal platinum, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art, membrane electrode assembly is sprayed at proton exchange membrane cathode side by the platinum based catalyst taking porous carbon nanofiber as carrier and anode-side obtains through hot pressing, and the amount of spraying is 0.2mg-Pt/cm
2, the temperature of hot pressing is 50 DEG C, membrane electrode assembly resistance value is 200 ohm.
Embodiment 8
Monocell of the present invention, with porous carbon nanofiber obtained by the platinum based catalyst of carrier, be placed between anode and cathode flow-field plate by membrane electrode assembly and form, this porous carbon nanofiber is the platinum based catalyst of carrier, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, wherein the content of platinum is 40wt%, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 1000 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 30, porous carbon nanofiber is supported with metal platinum, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art, membrane electrode assembly is sprayed at proton exchange membrane cathode side by the platinum based catalyst taking porous carbon nanofiber as carrier and anode-side obtains through hot pressing, and the amount of spraying is 0.8mg-Pt/cm
2, the temperature of hot pressing is 150 DEG C, membrane electrode assembly resistance value is 500 ohm.
Embodiment 9
Monocell of the present invention, with how empty carbon nano-fiber obtained by the platinum based catalyst of carrier, be placed between anode and cathode flow-field plate by membrane electrode assembly and form, it should be the platinum based catalyst of carrier with porous carbon nanofiber, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 1000 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 30, porous carbon nanofiber is supported with metal platinum, also be supported with carbon black, and load has metal platinum on carbon black, in this platinum based catalyst, the content of carbon black is 50wt%, the content of platinum is 10wt%, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art, this membrane electrode assembly is sprayed at proton exchange membrane cathode side by the platinum based catalyst taking porous carbon nanofiber as carrier and anode-side obtains through hot pressing, and the amount of spraying is 0.2mg-Pt/cm
2, the temperature of described hot pressing is 50 DEG C, membrane electrode assembly resistance value is 200 ohm.
Embodiment 10
Monocell of the present invention, with how empty carbon nano-fiber obtained by the platinum based catalyst of carrier, be placed between anode and cathode flow-field plate by membrane electrode assembly and form, the platinum based catalyst that should be carrier with how empty carbon nano-fiber, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 800 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 8, porous carbon nanofiber is supported with metal platinum, also be supported with carbon black, and load has metal platinum on carbon black, in this platinum based catalyst, the content 30wt% of carbon black, the content of platinum is 40wt%, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art, this membrane electrode assembly is sprayed at proton exchange membrane cathode side by the platinum based catalyst taking porous carbon nanofiber as carrier and anode-side obtains through hot pressing, and the amount of painting is 0.6mg-Pt/cm
2, the temperature of hot pressing is 100 DEG C, membrane electrode assembly resistance value is 300 ohm.
Embodiment 11
It is of the present invention that a kind of that have high catalytic activity and high-durability take porous carbon nanofiber as the preparation method of the platinum based catalyst of carrier, be 15wt% by porous carbon nanofiber and platinum content, all the other are that the platinum carbon catalyst common distribution of carbon black is in isopropyl alcohol dispersant, the wherein particle diameter 20 ~ 40nm of platinum carbon catalyst, then dry 6 hours at 40 DEG C of temperature after 0.5 hour with the frequency ultrasound process of 50 hertz, namely obtaining take porous carbon nanofiber as the platinum based catalyst of carrier, it should be the platinum based catalyst of carrier with porous carbon nanofiber, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 100 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 5, porous carbon nanofiber is supported with metal platinum, also be supported with carbon black, and load has metal platinum on carbon black, in this platinum based catalyst, the content 50wt% of carbon black, the content of platinum is 10wt%, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.
Embodiment 12
It is of the present invention that a kind of that have high catalytic activity and high-durability take porous carbon nanofiber as the preparation method of the platinum based catalyst of carrier, be 60wt% by porous carbon nanofiber and platinum content, all the other are that the platinum carbon catalyst common distribution of carbon black is in dispersant methyl alcohol, the wherein particle diameter 20 ~ 40nm of platinum carbon catalyst, then dry 12 hours at 120 DEG C of temperature after 4 hours with the frequency ultrasound process of 50 hertz, namely obtaining take porous carbon nanofiber as the platinum based catalyst of carrier, it should be the platinum based catalyst of carrier with porous carbon nanofiber, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 1000 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 30, porous carbon nanofiber is supported with metal platinum, also be supported with carbon black, and load has metal platinum on carbon black, in this platinum based catalyst, the content 30wt% of carbon black, the content of platinum is 40wt%, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.
Embodiment 13
It is of the present invention that a kind of that have high catalytic activity and high-durability take porous carbon nanofiber as the preparation method of the platinum based catalyst of carrier, be 20wt% by porous carbon nanofiber and platinum content, all the other are that the platinum carbon catalyst common distribution of carbon black is in dispersant methyl alcohol, wherein the particle diameter of platinum carbon catalyst is 20 ~ 40nm, then dry 10 hours at 80 DEG C of temperature after 2 hours with the frequency ultrasound process of 50 hertz, namely obtaining take porous carbon nanofiber as the platinum based catalyst of carrier, it should be the platinum based catalyst of carrier with porous carbon nanofiber, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 800 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 6, porous carbon nanofiber is supported with metal platinum, also be supported with carbon black, and on carbon black, load there is metal platinum, in this platinum based catalyst, the content 20wt% of carbon black, the content of platinum is 20wt%, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.Be different catalysts linear scan curve as shown in Figure 10, wherein the platinum based catalyst platinum content of Pt/PCNFs-20 to be obtained with porous carbon nanofiber be carrier is 20%; JM-20 is Johnson Matthey CorporationHiSPEC3000 platinum carbon catalyst; JM-40 is Johnson Matthey Corporation HiSPEC4000 platinum carbon catalyst.Be monocell polarization curve as shown in figure 12, wherein Pt/PCNFs-20 is that what obtained by dispersion mixing method of the present invention take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 20%; JM-20 is Johnson Matthey CorporationHiSPEC3000 platinum carbon catalyst; JM-40 is Johnson Matthey Corporation HiSPEC4000 platinum carbon catalyst.
Embodiment 14
It is of the present invention that a kind of that have high catalytic activity and high-durability take porous carbon nanofiber as the preparation method of the platinum based catalyst of carrier, by the method for electronation, platinum is reducing loaded on carbon carrier porous carbon nanofiber with the form of nano particle by the presoma of platinum, first the porous carbon fiber taking 80mg is placed in there-necked flask, the ethylene glycol ultrasonic disperse 1h adding 50ml forms the suspension dividing equally dispersion, slowly add a certain amount of chloroplatinic acid aqueous solution (making the platinum carrying capacity of platinum carbon catalyst be 15wt%) subsequently, continue ultrasonic 1h, stir 2h, by solution warms to 130 DEG C, N
2atmosphere protection backflow 3h, be cooled to room temperature, centrifugation goes out product, and with a large amount of washings several times, product is placed in vacuum drying oven 80 DEG C of vacuumize 12h, what must have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of content for 10wt% of carrier platinum, being illustrated in figure 3 obtained take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 10%, Pt/PCNFs-10 surface topography, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, this platinum based catalyst, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 100 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 5, porous carbon nanofiber is supported with metal platinum, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.
Embodiment 15
It is of the present invention that a kind of that have high catalytic activity and high-durability take porous carbon nanofiber as the preparation method of the platinum based catalyst of carrier, by the method for electronation, platinum is reducing loaded on carbon carrier porous carbon nanofiber with the form of nano particle by the presoma of platinum, first the porous carbon fiber taking 60mg is placed in there-necked flask, the sodium borohydride ultrasonic disperse 1h adding 60ml forms the suspension dividing equally dispersion, slowly add a certain amount of platinic sodium chloride aqueous solution (making the platinum carrying capacity of platinum carbon catalyst be 20wt%) subsequently, continue ultrasonic 2h, stir 2h, by solution warms to 130 DEG C, N
2atmosphere protection backflow 3h, be cooled to room temperature, centrifugation goes out product, and with a large amount of washings several times, product is placed in vacuum drying oven 80 DEG C of vacuumize 12h, what must have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of content for 20wt% of carrier platinum, being illustrated in figure 5 obtained take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 20%, Pt/PCNFs-20 transmission electron microscope picture, this platinum based catalyst, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 1000 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 30, porous carbon nanofiber is supported with metal platinum, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, far above 5% of prior art.Be different catalysts ECSA durability as shown in figure 11, wherein the platinum based catalyst platinum content of Pt/PCNFs-20 to be obtained with porous carbon nanofiber be carrier is 20%; Pt/Vulcan-20 is self-control platinum carbon catalyst, and platinum content is 20%; JM-20 is Johnson Matthey Corporation HiSPEC3000 platinum carbon catalyst.
Embodiment 16
It is of the present invention that a kind of that have high catalytic activity and high-durability take porous carbon nanofiber as the preparation method of the platinum based catalyst of carrier, by the method for electronation, platinum is reducing loaded on carbon carrier porous carbon nanofiber with the form of nano particle by the presoma of platinum, first the porous carbon fiber taking 30mg is placed in there-necked flask, the formic acid ultrasonic disperse 1h adding 80ml forms the suspension dividing equally dispersion, slowly add a certain amount of acetic acid platinum aqueous solution (making the platinum carrying capacity of platinum C catalyst be 60wt%) subsequently, continue ultrasonic 2h, stir 2h, by solution warms to 130 DEG C, N
2atmosphere protection backflow 3h, be cooled to room temperature, centrifugation goes out product, and with a large amount of washings several times, product is placed in vacuum drying oven 80 DEG C of vacuumize 12h, what must have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of content for 40wt% of carrier platinum, being illustrated in figure 4 obtained take porous carbon nanofiber as the platinum based catalyst platinum content of carrier is 40%, Pt/PCNFs-40 transmission electron microscope picture, the platinum based catalyst of what this had high catalytic activity and high-durability with porous carbon nanofiber is carrier, being illustrated in figure 7 with porous carbon nanofiber is the platinum based catalyst electrode surface pattern of carrier, being illustrated in figure 8 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, being illustrated in figure 9 with porous carbon nanofiber is the platinum based catalyst electrode cross-section morphology of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, Fig. 1 is porous carbon nanofiber surface topography, Fig. 2 is porous carbon nanofiber cross-section morphology, the average fibre diameter of porous carbon nanofiber is 800 nanometers, aperture is 5 ~ 100 nanometers, Fiber Aspect Ratio is 8, porous carbon nanofiber is supported with metal platinum, should be the catalytic activity of the platinum based catalyst of carrier with porous carbon nanofiber: play spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%, far above 45% of prior art, should be the durability of the platinum based catalyst of carrier with porous carbon nanofiber: after 1000 circulations, ECSA conservation rate reaches 50%, and far above 5% of prior art, in the platinum based catalyst taking porous carbon nanofiber as carrier, the content of platinum is 40wt%.
Claims (10)
1. one kind what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, it is characterized in that: described take porous carbon nanofiber as the platinum based catalyst of carrier, porous carbon nanofiber as carrier forms the loose three-dimensional netted structure run through, and porous carbon nanofiber is supported with metal platinum; Described take porous carbon nanofiber as the catalytic activity of the platinum based catalyst of carrier: play a spike potential and shift to an earlier date 100 millivolts than platinum carbon catalyst, platinum utilization reaches 80%; Described take porous carbon nanofiber as the durability of the platinum based catalyst of carrier: after 1000 circulations, ECSA conservation rate reaches 50%.
2. according to claim 1 a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, it is characterized in that described porous carbon nanofiber is also supported with carbon black, and on carbon black, load having metal platinum.
It is 3. according to claim 1 and 2 that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, it is characterized in that, the average fibre diameter of described porous carbon nanofiber is 100 ~ 1000 nanometers, aperture is 5 ~ 100 nanometers, and Fiber Aspect Ratio is 5 ~ 30.
It is 4. according to claim 1 and 2 that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, it is characterized in that, in the platinum based catalyst taking porous carbon nanofiber as carrier, the content of described platinum is 10wt% ~ 40wt%.
It is 5. according to claim 2 that a kind of what have high catalytic activity and high-durability take porous carbon nanofiber as the platinum based catalyst of carrier, it is characterized in that, in the platinum based catalyst taking porous carbon nanofiber as carrier, the content≤50wt% of described carbon black.
6. one kind that have high catalytic activity and high-durability take porous carbon nanofiber as the preparation method of the platinum based catalyst of carrier, it is characterized in that: by porous carbon nanofiber and platinum carbon catalyst common distribution in dispersant, ultrasonic process post-drying, namely obtain with porous carbon nanofiber be carrier take porous carbon nanofiber as the platinum based catalyst of carrier.
7. preparation method according to claim 6, is characterized in that, described dispersant is isopropyl alcohol or methyl alcohol; In described platinum carbon catalyst, platinum content is 15wt% ~ 60wt%, and all the other are carbon black; Particle diameter 20 ~ the 40nm of described platinum carbon catalyst; Described ultrasonic process refers to the frequency ultrasound process 0.5 ~ 4 hour with 50 hertz; Described oven dry refer at 40 ~ 120 DEG C of temperature dry 6 ~ 12 hours.
8. that have high catalytic activity and high-durability take porous carbon nanofiber as the preparation method of the platinum based catalyst of carrier, it is characterized in that: be by the method for electronation, platinum is reducing loaded on carbon carrier porous carbon nanofiber with the form of nano particle by the presoma of platinum.
9. the monocell with porous carbon nanofiber obtained by the platinum based catalyst of carrier, be placed between anode and cathode flow-field plate by membrane electrode assembly and form, it is characterized in that: described membrane electrode assembly is sprayed at proton exchange membrane cathode side by the platinum based catalyst taking porous carbon nanofiber as carrier and anode-side obtains through hot pressing; Membrane electrode assembly resistance value is 200-500 ohm.
10. monocell according to claim 9, is characterized in that, the amount of described spraying is 0.2-0.8mg-Pt/cm
2; The temperature of described hot pressing is 50-150 DEG C.
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