CN103247805B - A kind of Non-noble metal electrocatalyst for fuel cell and preparation method thereof - Google Patents
A kind of Non-noble metal electrocatalyst for fuel cell and preparation method thereof Download PDFInfo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The present invention disclose a kind of Non-noble metal electrocatalyst for fuel cell with and preparation method thereof.This eelctro-catalyst is Co-Mo/ carrier alloy or MoCo-N/ carrier alloy, its preparation method is: 1) by the presoma containing molybdenum, containing the presoma of cobalt and support dispersion in o-xylene solution, be that solvent and reducing agent react 2.5-4.5h under the condition of temperature control for 140-155 DEG C with ortho-xylene, filtration, washing and drying obtain the presoma of MoCo/ carrier alloy afterwards; 2) presoma of the MoCo/ carrier alloy of preparation is carried out Low Temperature Heat Treatment under reducing atmosphere, obtain support type MoCo/ carrier alloy and/or MoCo-N/ carrier alloy.Alloy of the present invention has good electro catalytic activity, stability and methanol tolerant performance to hydrogen reduction in the basic conditions, and preparation technology is simple and easy to do, is applicable to the requirement of fuel battery cathode with proton exchange film eelctro-catalyst.
Description
Technical field,
The invention belongs to 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 commercial electrocatalyst that the oxygen reduction reaction of Proton Exchange Membrane Fuel Cells is used is expensive and platinum based catalyst that is methanol tolerant poor performance, thus hinders its scale application.Therefore, develop cheap, good stability, catalytic activity are good, the cathodic oxygen reduction eelctro-catalyst with methanol tolerant is significant for the large-scale commercial application of Proton Exchange Membrane Fuel Cells.
In recent years, the research of multiple non-platinum catalyst or non-precious metal catalyst achieved greater advance, mainly comprised N
4-macrocyclic compound (Fe-N
4and Co-N
4) (R.Bashyam, P.Zelenay.AClassofNon – PreciousMetalCompositeCatalystsforFuelCells.Nature, 2006, 443:63-66.), nitrogen carbon compound (K.Gong, F.Du, Z.Xia, etal.Nitrogen – DopedCarbonNanotubeArrayswithHighElectrocatalyticActivit yforOxygenReduction.Science, 2009, 323:760-764.), iron-based compound (D.H.Deng, L.Yu, X.H.Bao, etal.EncapsulatedwithinPod-likeCarbonNanotubesforOxygenR eductionReaction.Angew.Chem.Int.Ed.2013, 52:371-375) and supported cobalt (Y.Liang, Y.Li, H.Wang, etal.Co
3o
4nanocrystalsonGrapheneasaSynergisticCatalystforOxygenRed uctionReaction.NatureMater., 2011,10:780-786.), manganese cobalt/cobalt oxide (F.Y.Cheng, J.Shen, B.Peng, Y.D.Pan, Z.L.Tao, J.Chen.Rapidroom-temperaturesynthesisofnanocrystallinesp inelsasoxygenreductionandevolutionelectrocatalysts.Natur eChem, 2011,3,79-84.) etc.What these non-platinum catalysts compared with current platinum based catalyst that catalytic activity aspect in the basic conditions has can compare favourably, but also there is gap very much, especially under acid system, there is more weak stability, and the research of electrocatalytic oxidation reducing property avtive spot is fuzzyyer, this type of catalyst preparation process more complicated, severe reaction conditions in addition.Therefore, the efficient electric catalyst of development of new high catalytic activity site, better stability plays vital effect to further developing of fuel cell studies of promotion.
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.This legal system is simple for technological operation, and controllability is strong.
Technical scheme of the present invention is as follows:
A kind of Non-noble metal electrocatalyst for fuel cell, 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) by the presoma containing molybdenum, containing the presoma of cobalt and support dispersion in o-xylene solution, be that solvent and reducing agent react 2.5-4.5h under the condition of temperature for 140-155 DEG C with ortho-xylene, filtration, washing and drying obtain the presoma of MoCo/ carrier alloy afterwards;
2) presoma of the MoCo/ carrier alloy of preparation is carried out Low Temperature Heat Treatment under reducing atmosphere, obtain support type MoCo/ carrier and/or MoCo-N/ carrier alloy.
Further, step 1) the described presoma containing molybdenum and described be 1:1 containing the mol ratio of molybdenum and cobalt in the presoma of cobalt.
Further, step 1) described in state containing cobalt precursor to be acetylacetone cobalt, to be hexacarbonylmolybdenum containing molybdenum presoma, carrier is the carbon dust of XC-72 model or replaces with other carbon carriers (as carbon nano-tube, Graphene etc.).Carrier quality is determined according to the load capacity need preparing molybdenum in eelctro-catalyst, such as can carry out load by 20% load capacity of Mo.Ortho-xylene is solvent and reducing agent, need not regulate solution ph.
Further, step 1) adopt ultrasonic method to disperse.
Further, step 2) temperature of described Low Temperature Heat Treatment is 450-600 DEG C, the time is 1-6h.
Further, step 2) adopt the distribution be 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%; Ammonia is adopted to prepare MoCo-N/ carrier alloy as reducing atmosphere.
Co-Mo/ carrier alloy of the present invention and MoCo-N/ carrier alloy have good electro catalytic activity, stability and good methanol tolerant performance to hydrogen reduction in the basic conditions, are applicable 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.
Accompanying drawing explanation
Fig. 1 is the flow chart that " two step method " of the present invention prepares PEMFC eelctro-catalyst MoCo/ carrier, MoCo-N/ carrier alloy.
Fig. 2 is that the obtained PEMFC eelctro-catalyst MoCo-N/ carrier of embodiment 1 is at 0.1molL
-1electrochemistry cyclic voltammetry curve under KOH nitrogen, oxygen atmosphere.
Fig. 3 is that the obtained PEMFC eelctro-catalyst MoCo-N/ carrier of embodiment 1 is at 0.1molL
-1polarization curve under KOH oxygen atmosphere.
Fig. 4 is that the obtained PEMFC eelctro-catalyst MoCo-N/ carrier of embodiment 1 is at 0.1molL
-1kOH+1MCH
3electrochemistry cyclic voltammetry curve under OH nitrogen atmosphere.
Fig. 5 is that the obtained PEMFC eelctro-catalyst MoCo-N/ carrier of embodiment 1 is at 0.1molL
-1kOH+1MCH
3polarization curve under OH nitrogen atmosphere.
Fig. 6 is that the obtained PEMFC eelctro-catalyst MoCo-N/ carrier of embodiment 1 is at 0.1molL
-1chronoa mperometric plot under KOH oxygen atmosphere.
Fig. 7 is the X-ray diffractogram of the presoma of MoCo/ carrier alloy obtained in embodiment, and the reflux temperature that wherein a, b, c tri-curves are corresponding is respectively 155 DEG C, 145 DEG C, 140 DEG C.
Fig. 8 be PEMFC eelctro-catalyst MoCo/ carrier obtained in embodiment at the heat treated X-ray diffractogram of ammonia atmosphere, wherein reflux temperature is respectively 140 DEG C, 145 DEG C, 155 DEG C.
Fig. 9 is the X-ray diffractogram of PEMFC eelctro-catalyst MoCo/ carrier presoma under different return time obtained in embodiment, and the return time that wherein a, b, c tri-curves are corresponding is respectively 3.5h, 2.5h, 4.5h.
Figure 10 is that return time obtained in embodiment is respectively 3.5h, and under 2.5h, 4.5h, PEMFC eelctro-catalyst MoCo/ carrier is at the heat treated X-ray diffractogram of ammonia atmosphere.
Figure 11 is PEMFC eelctro-catalyst MoCo/ carrier heat treated X-ray diffractogram at different temperatures obtained in embodiment, and the heat treatment temperature that wherein a, b, c, d tetra-curves are corresponding is respectively 450 DEG C, 500 DEG C, 550 DEG C, 600 DEG C.
Figure 12 is PEMFC eelctro-catalyst MoCo-N/ carrier obtained in embodiment 5 X-ray diffractogram in the different heat treatment time.
Figure 13 is that PEMFC eelctro-catalyst MoCo/ carrier obtained in embodiment 6 is at the heat treated X-ray diffractogram of hydrogen atmosphere.
In Figure 14, a figure, b figure to be respectively in embodiment 6 and 1 transmission electron microscope picture after obtained PEMFC eelctro-catalyst MoCo/ carrier, MoCo-N/ support heat-tr eatment.
Embodiment
Embodiment 1:
The PEMFC (proton-exchangemembranefuelcells Proton Exchange Membrane Fuel Cells) of the present embodiment uses the building-up process of eelctro-catalyst see Fig. 1, is specially:
By 0.2mmol hexacarbonylmolybdenum (Mo (CO)
6) and 0.2mmol acetylacetone cobalt (Co (acac)
2) and 66mg carrier XC-72 to add volume be (volume of ortho-xylene does not limit, and ensures that this presoma and support dispersion are evenly) in the o-xylene solution of 150mL, make it be uniformly dispersed by ultrasonic.Under the condition being solvent and reducing agent with ortho-xylene, (to intensification stirring and refluxing " backflow " ensure under ortho-xylene and hexacarbonylmolybdenum boiling conditions, such one side hexacarbonylmolybdenum can reach the condition of cracking, ortho-xylene serves the effect of solvent and reducing agent on the other hand), temperature controls at 145 DEG C, obtains the presoma of support type after filtration after reaction 4.5h, washing, drying.The X-ray diffractogram of the presoma of gained is as shown in curve b in Fig. 7.
After the presoma of gained is ground, take ammonia as reducing atmosphere, after low temperature 550 DEG C of heat treatment 3h, obtain support type MoCo-N/ carrier alloy.Adopt inductively coupled plasma spectrum generator (ICP) to test the target product obtained, the content obtaining 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 as shown in c curve in Figure 11, and transmission electron microscope picture is as shown in b figure in Figure 14.From Figure 14, the support type MoCo-N/ carrier alloy of the transmission electron microscope picture display gained of b figure has narrower domain size distribution.
The MoCo-N/ carrier eelctro-catalyst of gained is made work electrode, adopts traditional three-electrode system, mercuric oxide electrode is reference electrode, and glass carbon plate, as auxiliary electrode, carries out electro-chemical test.Fig. 2 gives it at 0.1molL
-1cyclic voltammetry curve in KOH under saturated, the oxygen-saturated conditions of argon gas, sweep speed is 50mVs
-1.Its 0.1molL is given in Fig. 3
-1polarization curve under KOH oxygen atmosphere, sweep speed is 10mVs
-1, its rotating speed is followed successively by 400rpm, 900rpm, 1600rpm and 2500rpm from top to bottom.As can be seen from Fig. 2,3, the support type MoCo-N/ carrier eelctro-catalyst obtained shows good electrocatalytic oxidation reducing activity.Its 0.1molL is given in Fig. 4
-1kOH+1MCH
3cyclic voltammetry curve under OH oxygen atmosphere, sweep speed is 50mVs
-1.Its 0.1molL is given in Fig. 5
-1kOH+1MCH
3polarization curve under OH oxygen atmosphere, sweep speed is 10mVs
-1.As can be seen from Fig. 4,5, the support type MoCo-N/ carrier eelctro-catalyst obtained shows good methanol tolerant performance.Its 0.1molL is given in Fig. 6
-1chronoa mperometric plot under KOH oxygen atmosphere, current potential is-0.164V, and sweep time is 12h.As can be seen from Figure 6, heat treatment temperature is 500,550 DEG C and all shows good stability (in figure 500 DEG C and 550 DEG C of two curves substantially overlap).
Embodiment 2:
Building-up process, see Fig. 1, is specially:
By 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 o-xylene solution of 150mL, under the condition being solvent and reducing agent with ortho-xylene, intensification stirring and refluxing, temperature controls at 140 DEG C, 145 DEG C, 155 DEG C respectively, obtains the presoma of support type after filtration after reaction 4.5h, washing, drying.As shown in Figure 7, the reflux temperature that wherein a, b, c tri-curves are corresponding is respectively 155 DEG C, 145 DEG C, 140 DEG C to the X-ray diffractogram of the presoma of gained.
After the presoma of gained under different reflux temperature is ground, take ammonia as reducing atmosphere, after low temperature 550 DEG C of heat treatment 3h, obtain support type MoCo-N/ carrier alloy.Its X-ray diffraction photo as shown in Figure 8.From Fig. 7,8 the X-ray diffractogram display support type MoCo/ support precursor of gained and target product all little with reaction temperature change.
Embodiment 3:
Building-up process, see Fig. 1, is specially:
By 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 o-xylene solution of 150mL, under the condition being solvent and reducing agent with ortho-xylene, intensification stirring and refluxing, temperature controls at 145 DEG C, reaction time is distributed as 2.5h, 3.5h, 4.5h, obtain the presoma of support type after filtration, washing, drying.Fig. 9 is the X-ray diffractogram of obtained PEMFC eelctro-catalyst MoCo/ carrier presoma under different return time, and the return time that wherein a, b, c tri-curves are corresponding is respectively 3.5h, 2.5h, 4.5h.
After the presoma of gained under different return time is ground, take ammonia as reducing atmosphere, after low temperature 550 DEG C of heat treatment 3h, obtain support type MoCo-N/ carrier alloy.Its X-ray diffraction photo as shown in Figure 10.From Fig. 9,10 the X-ray diffractogram display support type MoCo/ support precursor of gained and target product all little with reaction time change.Integrated embodiment 2,3 visible, reaction temperature, time all on this target product without too large impact, be conducive to simple operations, controlledly synthesis.
Embodiment 4:
Building-up process, see Fig. 1, is specially:
By 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 o-xylene solution of 150mL, under the condition being solvent and reducing agent with ortho-xylene, intensification stirring and refluxing, temperature controls at 145 DEG C, obtains the presoma of support type after filtration after reaction 4.5h, washing, drying.The X-ray diffractogram of the presoma of gained is as shown in the b curve in Fig. 7.
After the presoma of gained is ground, be reducing atmosphere with ammonia, be distributed in low temperature 450 DEG C, 500 DEG C, 550 DEG C, after 600 DEG C of heat treatment 3h, obtain support type MoCo-N/ carrier alloy.Its X-ray diffraction photo is as a, b, c in Figure 11, shown in d tetra-curves, show from the X-ray diffractogram of Figure 11, when heat treatment temperature rises to 600 DEG C, its diffraction maximum has the trend that narrows, and illustrate that particle size becomes large, particle diameter crosses the application requirement that senior general does not meet eelctro-catalyst; And when heat treatment temperature controls 450, when 500,550 DEG C, the support type MoCo-N/ carrier diffraction maximum of gained does not all have significant change, meets the application requirement of eelctro-catalyst.
Embodiment 5:
Building-up process, see Fig. 1, is specially:
By 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 o-xylene solution of 150mL, under the condition being solvent and reducing agent with ortho-xylene, intensification stirring and refluxing, temperature controls at 145 DEG C, obtains the presoma of support type after filtration after reaction 4.5h, washing, drying.The X-ray diffractogram of the presoma of gained is as shown in the b curve in Fig. 7.
After being ground by the presoma of gained, take ammonia as reducing atmosphere, be 550 DEG C in temperature, heat treatment time is respectively 1h, after 3h, 6h, obtains support type MoCo-N/ carrier alloy.Its X-ray diffraction photo as shown in figure 12, shows from the X-ray diffractogram of Figure 12, and when heat treatment time is in 1 ~ 6 hours window, its XRD, all less than too large change, illustrates that the length of heat treatment time is to the formation of its target product not too large change.
Embodiment 6:
Building-up process, see Fig. 1, is specially:
By 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 o-xylene solution of 150mL, under the condition being solvent and reducing agent with ortho-xylene, intensification stirring and refluxing, temperature controls at 145 DEG C, obtains the presoma of support type after filtration after reaction 4.5h, washing, drying.The X-ray diffractogram of the presoma of gained is as shown in the b curve in Fig. 7.
After the presoma of gained is ground, adopt the hydrogen+argon gas of volume 5% as reducing atmosphere, after low temperature 500 DEG C of heat treatment 3h, obtain support type MoCo/ carrier alloy.Inductively coupled plasma spectrum generator (ICP) is adopted to test, the content obtaining 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, as shown in figure 13, transmission electron microscope picture is as shown in a figure in Figure 14 for its X-ray diffraction photo.From Figure 14, the support type MoCo/ carrier alloy of the transmission electron microscope picture display gained of a figure has narrower domain size distribution.
Above embodiment is only in order to illustrate technical scheme of the present invention but not to be limited; those of ordinary skill in the art can modify to technical scheme of the present invention or equivalent replacement; and not departing from the spirit and scope of the present invention, protection scope of the present invention should be as the criterion with described in claim.
Claims (7)
1. a Non-noble metal electrocatalyst for fuel cell, is characterized in that, this eelctro-catalyst is MoCo/ carrier alloy or MoCo-N/ carrier alloy, adopts and is prepared from the following method:
1) by the presoma hexacarbonylmolybdenum containing molybdenum, containing the presoma acetylacetone cobalt of cobalt and support dispersion in o-xylene solution, be that solvent and reducing agent react 2.5-4.5h under the condition of temperature for 140-155 DEG C with ortho-xylene, filtration, washing and drying obtain the presoma of MoCo/ carrier alloy afterwards;
2) presoma of the MoCo/ carrier alloy of preparation is carried out Low Temperature Heat Treatment under reducing atmosphere, obtain support type MoCo/ carrier alloy and/or MoCo-N/ carrier alloy; Adopt the distribution be made up of hydrogen and inert atmosphere to prepare described MoCo/ carrier alloy as reducing atmosphere, adopt ammonia to prepare described MoCo-N/ carrier alloy as reducing atmosphere.
2. prepare a method for Non-noble metal electrocatalyst for fuel cell described in claim 1, its step comprises:
1) by the presoma hexacarbonylmolybdenum containing molybdenum, containing the presoma acetylacetone cobalt of cobalt and support dispersion in o-xylene solution, be that solvent and reducing agent react 2.5-4.5h under the condition of temperature for 140-155 DEG C with ortho-xylene, filtration, washing and drying obtain the presoma of MoCo/ carrier alloy afterwards;
2) presoma of the MoCo/ carrier alloy of preparation is carried out Low Temperature Heat Treatment under reducing atmosphere, obtain support type MoCo/ carrier alloy and/or MoCo-N/ carrier alloy; Adopt the distribution be made up of hydrogen and inert atmosphere to prepare described MoCo/ carrier alloy as reducing atmosphere, adopt ammonia to prepare described MoCo-N/ carrier alloy as reducing atmosphere.
3. method as claimed in claim 2, is characterized in that: the described presoma containing molybdenum and the described mol ratio containing molybdenum and cobalt in the presoma of cobalt are 1:1.
4. method as claimed in claim 2, is characterized in that: described carrier is the one in XC-72, carbon nano-tube, Graphene.
5. method as claimed in claim 2, is characterized in that: adopt ultrasonic method by the presoma containing molybdenum, the presoma containing cobalt and support dispersion in o-xylene solution.
6. method as claimed in claim 2, is characterized in that: the temperature of described Low Temperature Heat Treatment is 450-600 DEG C, and the time is 1-6h.
7. method as claimed in claim 2, is characterized in that: in described distribution, the volume content of hydrogen is 5%.
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