CN103247805A - Non-noble metal electrocatalyst for fuel cell and preparation method thereof - Google Patents
Non-noble metal electrocatalyst for fuel cell and preparation method thereof Download PDFInfo
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- CN103247805A CN103247805A CN2013101701485A CN201310170148A CN103247805A CN 103247805 A CN103247805 A CN 103247805A CN 2013101701485 A CN2013101701485 A CN 2013101701485A CN 201310170148 A CN201310170148 A CN 201310170148A CN 103247805 A CN103247805 A CN 103247805A
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
Abstract
The invention discloses a non-noble metal electrocatalyst for a fuel cell and a preparation method thereof. The non-noble metal electrocatalyst is a Co-Mo/carrier alloy or an MoCo-N/carrier alloy. The preparation method of the non-noble metal electrocatalyst comprises the following steps of: (1) dispersing a molybdenum-containing precursor, a cobalt-containing precursor and a carrier into an ortho-xylene solution, reacting for 2.5-4.5 hours at 140 DEG C-155 DEG C in the presence of ortho-xylene serving as a solvent and a reducing agent, filtering, washing, and drying to obtain an MoCo/carrier alloy precursor; and (2) carrying out low-temperature heat treatment on the prepared MoCo/carrier alloy precursor in a reducing atmosphere to obtain a supported MoCo/carrier alloy and/or an MoCo-N/carrier alloy. The used alloy has good electrocatalysis activity, stability and methanol resistant property for oxygen reduction under an alkaline condition; the preparation process is simple and easy; and the non-noble metal electrocatalyst meets the requirements of the cathode electrocatalyst of a proton exchange membrane fuel cell.
Description
Technical field,
The invention belongs to the fuel cell material science and technology field, be specifically related to a kind of non-noble metal fuel cell oxygen reduction electrocatalyst and preparation method thereof.
Background technology
At present, the used commercial electrical catalyst of the oxygen reduction reaction of Proton Exchange Membrane Fuel Cells is the platinum based catalyst of expensive and anti-methyl alcohol poor performance, uses thereby hindered its scale.Therefore, cheap, the good stability of development, catalytic activity cathodic oxygen reduction eelctro-catalyst good, that have anti-methyl alcohol are significant for the large-scale commercial applications application of Proton Exchange Membrane Fuel Cells.
In recent years, the research of multiple non-platinum catalyst or non-precious metal catalyst had obtained bigger progress, mainly comprised N
4-macrocyclic compound (Fe-N
4And Co-N
4) (R.Bashyam, P.Zelenay.A Class of Non – Precious Metal Composite Catalysts for Fuel Cells.Nature, 2006,443:63-66.), nitrogen carbon compound (K.Gong, F.Du, Z.Xia, et al.Nitrogen – Doped Carbon Nanotube Arrays with High Electrocatalytic Activity for Oxygen Reduction.Science, 2009,323:760-764.), iron-based thing (D.H.Deng, L.Yu, X.H.Bao, et al.Encapsulated within Pod-like Carbon Nanotubes for OxygenReduction Reaction.Angew.Chem.Int.Ed.2013,52:371-375) and supported cobalt (Y.Liang, Y.Li, H.Wang, et al.Co
3O
4Nanocrystals on Graphene as a Synergistic Catalyst for Oxygen Reduction Reaction.Nature Mater., 2011,10:780-786.), manganese cobalt/cobalt oxide (F.Y.Cheng, J.Shen, B.Peng, Y.D.Pan, Z.L.Tao, J.Chen.Rapid room-temperature synthesis of nanocrystalline spinels as oxygen reduction and evolution electrocatalysts.Nature Chem, 2011,3,79-84.) etc.These non-platinum catalysts are compared can comparing favourably of having aspect the catalytic activity under alkali condition with current platinum based catalyst, but gap is arranged very also, especially under acid system, has more weak stability, and the research of electrocatalytic oxidation reducing property avtive spot is fuzzyyer, in addition this type of catalyst preparation process more complicated, severe reaction conditions.Therefore, develop the efficient eelctro-catalyst of novel high catalytic activity site, better stability to promoting that further developing of fuel cell studies plays crucial effects.
Summary of the invention
The object of the present invention is to provide a kind of used in proton exchange membrane fuel cell base metal Co-Mo eelctro-catalyst and preparation method thereof.It is simple that this legal system is equipped with technological operation, and controllability is strong.
Technical scheme of the present invention is as follows:
A kind of fuel cell base metal eelctro-catalyst, it is Co-Mo/ carrier alloy or MoCo-N/ carrier alloy.
The preparation method of above-mentioned Co-Mo/ carrier alloy, MoCo-N/ carrier alloy is divided into following two steps:
1) will contain the presoma of molybdenum, the presoma that contains cobalt and carrier is scattered in the ortho-xylene solution, be that solvent and reducing agent are to react 2.5-4.5h under 140-155 ℃ the condition in temperature with the ortho-xylene, make the presoma of MoCo/ carrier alloy after filtration, washing and the drying;
2) presoma of MoCo/ carrier alloy with preparation carries out Low Temperature Heat Treatment under reducing atmosphere, obtains support type MoCo/ carrier and/or MoCo-N/ carrier alloy.
Further, the mol ratio of molybdenum and cobalt is 1:1 in the described presoma that contains molybdenum of step 1) and the described presoma that contains cobalt.
Further, step 1) is described states that to contain cobalt precursor be acetylacetone cobalt, and containing the molybdenum presoma is hexacarbonylmolybdenum, and carrier is the carbon dust of XC-72 model or replaces with other carbon carriers (as carbon nano-tube, Graphene etc.).The carrier quality prepares in the eelctro-catalyst load capacity of molybdenum according to need to be determined, such as carrying out load by 20% load capacity of Mo.Ortho-xylene is solvent and reducing agent, need not regulator solution pH value.
Further, step 1) adopts ultrasonic method to disperse.
Further, step 2) temperature of described Low Temperature Heat Treatment is 450-600 ℃, and the time is 1-6h.
Further, step 2) adopt the distribution of being made up of hydrogen and inert atmosphere (as argon gas etc.) to prepare MoCo/ carrier alloy as reducing atmosphere, wherein the volume content of hydrogen is 5%; Adopt ammonia to prepare MoCo-N/ carrier alloy as reducing atmosphere.
Co-Mo/ carrier alloy of the present invention and MoCo-N/ carrier alloy have preferably electro catalytic activity, stability and anti-methyl alcohol performance preferably to hydrogen reduction under alkali condition, be fit to the requirement of fuel battery cathode with proton exchange film eelctro-catalyst.Preparation technology of the present invention is simple to operate, and controllability is strong.
Description of drawings
Fig. 1 is the flow chart of " two step method " of the present invention preparation PEMFC eelctro-catalyst MoCo/ carrier, MoCo-N/ carrier alloy.
The PEMFC that Fig. 2 makes for embodiment 1 uses eelctro-catalyst MoCo-N/ carrier at 0.1mol L
-1Electrochemistry cyclic voltammetry curve under KOH nitrogen, the oxygen atmosphere.
The PEMFC that Fig. 3 makes for embodiment 1 uses eelctro-catalyst MoCo-N/ carrier at 0.1mol L
-1Polarization curve under the KOH oxygen atmosphere.
The PEMFC that Fig. 4 makes for embodiment 1 uses eelctro-catalyst MoCo-N/ carrier at 0.1mol L
-1KOH+1M CH
3Electrochemistry cyclic voltammetry curve under the OH nitrogen atmosphere.
The PEMFC that Fig. 5 makes for embodiment 1 uses eelctro-catalyst MoCo-N/ carrier at 0.1mol L
-1KOH+1M CH
3Polarization curve under the OH nitrogen atmosphere.
The PEMFC that Fig. 6 makes for embodiment 1 uses eelctro-catalyst MoCo-N/ carrier at 0.1mol L
-1Timing current curve under the KOH oxygen atmosphere.
Fig. 7 is the X-ray diffractogram of the presoma of the MoCo/ carrier alloy that makes among the embodiment, and a wherein, b, the reflux temperature of three curve correspondences of c are respectively 155 ℃, 145 ° C, 140 ℃.
Fig. 8 uses eelctro-catalyst MoCo/ carrier at the heat treated X-ray diffractogram of ammonia atmosphere for the PEMFC that makes among the embodiment, and wherein reflux temperature is respectively 140 ℃, 145 ℃, 155 ℃.
Fig. 9 is the PEMFC that makes among the embodiment X-ray diffractogram with eelctro-catalyst MoCo/ carrier presoma under different return times, a wherein, and b, the return time of three curve correspondences of c is respectively 3.5h, 2.5h, 4.5h.
Figure 10 is respectively 3.5h for the return time that makes among the embodiment, 2.5h, and PEMFC uses eelctro-catalyst MoCo/ carrier at the heat treated X-ray diffractogram of ammonia atmosphere under the 4.5h.
Figure 11 for the PEMFC that makes among the embodiment with eelctro-catalyst MoCo/ carrier heat treated X-ray diffractogram under different temperatures, a wherein, b, c, the heat treatment temperature of four curve correspondences of d is respectively 450 ℃, 500 ℃, 550 ℃, 600 ℃.
Figure 12 is the PEMFC that makes among the embodiment 5 X-ray diffractogram of eelctro-catalyst MoCo-N/ carrier in the different heat treatment time.
Figure 13 uses eelctro-catalyst MoCo/ carrier at the heat treated X-ray diffractogram of hydrogen atmosphere for the PEMFC that makes among the embodiment 6.
Figure 14 a, b are respectively the transmission electron microscope picture after the PEMFC that makes in embodiment 6 and 1 eelctro-catalyst MoCo/ carrier, the heat treatment of MoCo-N/ carrier.
Embodiment
Embodiment 1:
The PEMFC(proton-exchange membrane fuel cells Proton Exchange Membrane Fuel Cells of present embodiment) building-up process of using eelctro-catalyst is specially referring to Fig. 1:
With 0.2mmol hexacarbonylmolybdenum (Mo (CO)
6) and 0.2mmol acetylacetone cobalt (Co (acac)
2) and 66mg carrier XC-72 add in the ortho-xylene solution that volume is 150mL (volume of ortho-xylene is unqualified, guarantee this presoma and carrier are uniformly dispersed get final product), by ultrasonic it is uniformly dispersed.Be under the condition of solvent and reducing agent with the ortho-xylene, (" backflow " is to guarantee under ortho-xylene and hexacarbonylmolybdenum boiling point condition to the intensification stirring and refluxing, hexacarbonylmolybdenum can reach the condition of cracking so on the one hand, ortho-xylene has played the effect of solvent and reducing agent on the other hand), temperature control obtains the presoma of support type at 145 ℃ after filtration behind the reaction 4.5h, washing, the drying.The X-ray diffractogram of the presoma of gained is shown in curve b among Fig. 7.
After the presoma grinding with gained, be reducing atmosphere with the ammonia, behind 550 ℃ of heat treatment 3h of low temperature, obtain support type MoCo-N/ carrier alloy.Adopt inductively coupled plasma spectrum generator (ICP) to test the target product that obtains, the content that obtains Mo, Co is respectively 5.42 μ g/mL, 6.25 μ g/mL, so its Mo:Co proportion of composing is about 3:2, its composition can be written as: Co
3Mo
2N.Its X-ray diffraction photo is shown in Figure 11 c, and the transmission electron microscope picture is shown in Figure 13 b.Show that from the transmission electron microscope picture of Figure 13 b the support type MoCo-N/ carrier alloy of gained has narrower particle diameter and distributes.
The MoCo-N/ carrier eelctro-catalyst of gained is made work electrode, adopt traditional three-electrode system, mercuric oxide electrode is reference electrode, and the glass carbon plate carries out electro-chemical test as auxiliary electrode.Fig. 2 has provided it at 0.1mol L
-1Cyclic voltammetry curve among the KOH under saturated, the oxygen-saturated conditions of argon gas, sweep speed is 50mV s
-1Provided its 0.1mol L among Fig. 3
-1Polarization curve under the KOH oxygen atmosphere, sweep speed are 10mV s
-1, its rotating speed is followed successively by 400rpm, 900rpm, 1600rpm and 2500rpm from top to bottom.As can be seen, resulting support type MoCo-N/ carrier eelctro-catalyst shows electrocatalytic oxidation reducing activity preferably from Fig. 2,3.Provided its 0.1mol L among Fig. 4
-1KOH+1M CH
3Cyclic voltammetry curve under the OH oxygen atmosphere, sweep speed are 50mV s
-1Provided its 0.1mol L among Fig. 5
-1KOH+1M CH
3Polarization curve under the OH oxygen atmosphere, sweep speed are 10mV s
-1As can be seen, resulting support type MoCo-N/ carrier eelctro-catalyst shows anti-methyl alcohol performance preferably from Fig. 4,5.Provided its 0.1mol L among Fig. 6
-1Timing current curve under the KOH oxygen atmosphere, current potential are-0.164V that be 12h sweep time.As can be seen from Figure 6, heat treatment temperature is 500,550 ℃ and all shows preferably stability (among the figure 500 ℃ and 550 ℃ of two curves overlap substantially).
Embodiment 2:
Building-up process is specially referring to Fig. 1:
With 0.2mmol hexacarbonylmolybdenum (Mo (CO)
6) and 0.2mmol acetylacetone cobalt (Co (acac)
2) and 66mg carrier XC-72 to add volume be in the ortho-xylene solution of 150mL, be under the condition of solvent and reducing agent with the ortho-xylene, the intensification stirring and refluxing, temperature is controlled respectively at 140 ℃, 145 ℃, 155 ℃, obtains the presoma of support type after filtration behind the reaction 4.5h, washing, the drying.The X-ray diffractogram of the presoma of gained as shown in Figure 7, a wherein, b, three curves of c corresponding reflux temperature respectively are 155 ℃, 145 ℃, 140 ℃.
After the presoma grinding with gained under the different reflux temperatures, be reducing atmosphere with the ammonia, behind 550 ℃ of heat treatment 3h of low temperature, obtain support type MoCo-N/ carrier alloy.Its X-ray diffraction photo as shown in Figure 8.Show that from Fig. 7,8 X-ray diffractogram the support type MoCo/ support precursor of gained and target product all change little with reaction temperature.
Embodiment 3:
Building-up process is specially referring to Fig. 1:
With 0.2mmol hexacarbonylmolybdenum (Mo (CO)
6) and 0.2mmol acetylacetone cobalt (Co (acac)
2) and 66mg carrier XC-72 to add volume be in the ortho-xylene solution of 150mL, be under the condition of solvent and reducing agent with the ortho-xylene, the intensification stirring and refluxing, temperature control is at 145 ℃, reaction time is distributed as 2.5h, 3.5h 4.5h obtains the presoma of support type after filtration, washing, the drying.Fig. 9 is the PEMFC that makes with the X-ray diffractogram of eelctro-catalyst MoCo/ carrier presoma under different return times, and a wherein, b, three curves of c corresponding return time respectively are 3.5h, 2.5h, 4.5h.
After the presoma grinding with gained under the different return times, be reducing atmosphere with the ammonia, behind 550 ℃ of heat treatment 3h of low temperature, obtain support type MoCo-N/ carrier alloy.Its X-ray diffraction photo as shown in figure 10.Show that from Fig. 9,10 X-ray diffractogram the support type MoCo/ support precursor of gained and target product all change little with the reaction time.Comprehensive embodiment 2,3 as seen, reaction temperature, time all do not have too big influence to this target product, are conducive to simple operations, controlledly synthesis.
Embodiment 4:
Building-up process is specially referring to Fig. 1:
With 0.2mmol hexacarbonylmolybdenum (Mo (CO)
6) and 0.2mmol acetylacetone cobalt (Co (acac)
2) and 66mg carrier XC-72 to add volume be in the ortho-xylene solution of 150mL, be under the condition of solvent and reducing agent with the ortho-xylene, the intensification stirring and refluxing, temperature is controlled at 145 ℃, obtains the presoma of support type after filtration behind the reaction 4.5h, washing, the drying.The X-ray diffractogram of the presoma of gained is shown in the b curve among Fig. 7.
After the presoma grinding with gained, be reducing atmosphere with the ammonia, be distributed in 450 ℃ of low temperature, 500 ℃, 550 ℃, obtain support type MoCo-N/ carrier alloy behind 600 ℃ of heat treatment 3h.Its X-ray diffraction photo such as Figure 11 a, b, c, shown in the d, from the X-ray diffractogram demonstration of Figure 11, when heat treatment temperature rose to 600 ℃, its diffraction maximum had the trend of narrowing down, and illustrated that the product particle diameter becomes big, and particle diameter is crossed the application requirements that senior general does not meet eelctro-catalyst; And control in the time of 450,500,550 ℃ when heat treatment temperature, the support type MoCo-N/ carrier diffraction maximum of gained does not all have significant change, meets the application requirements of eelctro-catalyst.
Embodiment 5:
Building-up process is specially referring to Fig. 1:
With 0.2mmol hexacarbonylmolybdenum (Mo (CO)
6) and 0.2mmol acetylacetone cobalt (Co (acac)
2) and 66mg carrier XC-72 to add volume be in the ortho-xylene solution of 150mL, be under the condition of solvent and reducing agent with the ortho-xylene, the intensification stirring and refluxing, temperature is controlled at 145 ℃, obtains the presoma of support type after filtration behind the reaction 4.5h, washing, the drying.The X-ray diffractogram of the presoma of gained is shown in the b curve among Fig. 7.
After the presoma grinding with gained, being reducing atmosphere with the ammonia, is 550 ℃ in temperature, and heat treatment time is respectively 1h, and 3h behind the 6h, obtains support type MoCo-N/ carrier alloy.Its X-ray diffraction photo shows from the X-ray diffractogram of Figure 12 as shown in figure 12, when heat treatment time in 1～6 hour scope, its XRD is all less than too big variation, the length that heat treatment time is described to the formation of its target product less than too big variation.
Embodiment 6:
Building-up process is specially referring to Fig. 1:
With 0.2mmol hexacarbonylmolybdenum (Mo (CO)
6) and 0.2mmol acetylacetone cobalt (Co (acac)
2) and 66mg carrier XC-72 to add volume be in the ortho-xylene solution of 150mL, be under the condition of solvent and reducing agent with the ortho-xylene, the intensification stirring and refluxing, temperature is controlled at 145 ℃, obtains the presoma of support type after filtration behind the reaction 4.5h, washing, the drying.The X-ray diffractogram of the presoma of gained is shown in the b curve among Fig. 7.
After the presoma grinding with gained, adopt the hydrogen+argon gas of volume 5% as reducing atmosphere, behind 500 ℃ of heat treatment 3h of low temperature, obtain support type MoCo/ carrier alloy.Adopt inductively coupled plasma spectrum generator (ICP) to test, the content that obtains Mo, Co is respectively 5.57 μ g/mL, 6.78 μ g/mL, so its Mo:Co proportion of composing is about 1.3:1, its X-ray diffraction photo as shown in figure 12, the transmission electron microscope picture is shown in Figure 13 a.Show that from the transmission electron microscope picture of Figure 13 the support type MoCo/ carrier alloy of gained has narrower particle diameter and distributes.
Above embodiment is only in order to technical scheme of the present invention to be described but not limit it; those of ordinary skill in the art can make amendment or is equal to replacement technical scheme of the present invention; and not breaking away from the spirit and scope of the present invention, protection scope of the present invention should be as the criterion so that claim is described.
Claims (10)
1. a fuel cell base metal eelctro-catalyst is characterized in that, this eelctro-catalyst is Co-Mo/ carrier alloy or MoCo-N/ carrier alloy.
2. one kind prepares the method that the described fuel cell of claim 1 is used the base metal eelctro-catalyst, and its step comprises:
1) will contain the presoma of molybdenum, the presoma that contains cobalt and carrier is scattered in the ortho-xylene solution, be that solvent and reducing agent are to react 2.5-4.5h under 140-155 ℃ the condition in temperature with the ortho-xylene, make the presoma of MoCo/ carrier alloy after filtration, washing and the drying;
2) presoma of MoCo/ carrier alloy with preparation carries out Low Temperature Heat Treatment under reducing atmosphere, obtains support type MoCo/ carrier alloy and/or MoCo-N/ carrier alloy.
3. method as claimed in claim 2 is characterized in that: the mol ratio of molybdenum and cobalt is 1:1 in the described presoma that contains molybdenum and the described presoma that contains cobalt.
4. method as claimed in claim 2, it is characterized in that: the described cobalt precursor that contains is acetylacetone cobalt, the described molybdenum presoma that contains is hexacarbonylmolybdenum; Described carrier is a kind of in XC-72, carbon nano-tube, the Graphene.
5. method as claimed in claim 2 is characterized in that: adopt ultrasonic method will contain the presoma of molybdenum, the presoma that contains cobalt and carrier and be scattered in the ortho-xylene solution.
6. method as claimed in claim 2, it is characterized in that: the temperature of described Low Temperature Heat Treatment is 450-600 ℃, the time is 1-6h.
7. method as claimed in claim 2 is characterized in that: adopt the distribution of being made up of hydrogen and inert atmosphere to prepare described MoCo/ carrier alloy as reducing atmosphere.
8. method as claimed in claim 7, it is characterized in that: the volume content of hydrogen is 5% in the described distribution.
9. method as claimed in claim 2 is characterized in that: adopt ammonia to prepare described MoCo-N/ carrier alloy as reducing atmosphere.
10. according to the Co-Mo/ carrier alloy of each preparation in the claim 2 to 9 or the MoCo-N/ carrier alloy battery eelctro-catalyst that acts as a fuel.
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| WO2016124161A1 (en) * | 2015-02-02 | 2016-08-11 | 北京大学 | Pt/α-moc1-x supported catalyst, and synthesis and uses thereof |
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