CN105070925B - The preparation and application of fuel-cell catalyst Pt CrN/ graphene complexes - Google Patents
The preparation and application of fuel-cell catalyst Pt CrN/ graphene complexes Download PDFInfo
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- CN105070925B CN105070925B CN201510564565.7A CN201510564565A CN105070925B CN 105070925 B CN105070925 B CN 105070925B CN 201510564565 A CN201510564565 A CN 201510564565A CN 105070925 B CN105070925 B CN 105070925B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 kind of preparation and application of fuel-cell catalyst Pt CrN/ graphene complexes.The preparation method includes：(1) CrN/ graphene complexes are made using graphite oxide and chromic salts；(2) Pt CrN/ graphene complexes are made using by platinum salt, solvent and CrN/ graphene complexes.Product prepared by the present invention has excellent anodic oxidation, cathodic oxygen reduction performance as fuel-cell catalyst.Technique is simple, and cost is low, and controllability is good, favorable repeatability, may be adapted to mass produce.The present invention solves the problem of costly present in the existing technology for preparing CrN/ Nano Carbon bodies, condition harshness, complex process.Fuel-cell catalyst Pt CrN/ graphene complexes prepared by the present invention can be applied to methanol, formic acid, ethanol electrooxidation and oxygen reduction reaction catalyst.
Description
Technical field
The invention belongs to the field of fuel-cell catalyst, and in particular to a kind of fuel-cell catalyst Pt-CrN/ graphite
The preparation and application of alkene complex.
Background technology
Fuel cell is a kind of TRT that the chemical energy of fuel is directly translated into electric energy.It is used as battery using fuel
Negative electrode active material, oxidation reaction occurs in negative pole；Positive active material of the oxygen as fuel cell, it is anti-that reduction occurs in positive pole
Should.By only having the electrolyte of ionic conductivity to separate between positive pole and negative pole, the oxidation reaction of such fuel and the reduction of oxygen
Reaction is to occur respectively in two places, and the energy difference between reactant and reaction product is with the potential difference of positive and negative electrode and flows through outer
The electric current of circuit discharges.It is that the positive and negative electrode of fuel cell does not include active matter in itself with general battery difference
Matter, simply play catalytic conversion, the required fuel (fossil fuel such as hydrogen or methane, natural gas, coal gas, methanol, ethanol, gasoline
Or bioenergy is reformed and produced) and oxygen (or air) constantly by extraneous input.Fuel cell is because of its efficient and environmentally friendly generating side
Formula, by as the substitute products of diesel-driven generator and gas turbine powered generator.Europe, the developed country of north America region competitively put into
Huge fund is developed and has achieved many important achievements.Fuel cell technology has developed into the practical stage, is especially led in national defence
Domain, its application is more and more extensive, such as fuel cell AIP (the Air Independent of German conventional submarine
Propulsion) system achieves the achievement to attract people's attention.Although fuel cell achieves one in reliability, durability etc.
Fixed progress, but to reach really practical, many deficiencies also be present.The use cost of fuel cell is of a relatively high at present
It is the principal element for limiting its large-scale application.Wherein, Pt a large amount of use causes its cost high in catalyst
Major reason.Therefore, how to find the fuel-cell catalyst of cheap, high activity and high stability has turned into current research heat
Point.
The content of the invention
In order to solve, existing fuel-cell catalyst prepares cost height, complex process, activity is low and leads to not really fire
Expect the commercialized problem of battery.It is compound that the primary and foremost purpose of the present invention is to provide for fuel-cell catalyst Pt-CrN/ graphenes
The preparation method of body, the preparation method technique is simple, cost is low, controllability is good, favorable repeatability, may be adapted to large-scale production property
The excellent anode of fuel cell oxidation of energy, the catalyst Pt-CrN/ graphene complexes of cathodic oxygen reduction.
The fuel-cell catalyst Pt-CrN/ graphenes obtained another object of the present invention is to provide above-mentioned preparation method
Complex.
It is yet a further object of the present invention to provide answering for above-mentioned fuel-cell catalyst Pt-CrN/ graphene complexes
With.
The object of the invention is achieved through the following technical solutions：
A kind of preparation method of fuel-cell catalyst Pt-CrN/ graphene complexes, comprises the following steps：
(1) preparation of CrN/ graphene complexes：Graphite oxide and chromic salts are added in solvent, ultrasound, stirring are complete
After dissolving, 4~12h is heated in 110~150 DEG C；After product is washed, drying, then under ammonification atmosphere, with 5~12 DEG C/
Min heating rate, it is warming up to 500~900 DEG C and is incubated 2~6h progress nitrogen treatment, CrN/ graphene complexes are made；
(2) preparation of Pt-CrN/ graphene complexes：Platinum salt is dissolved in solvent ethylene glycol, adds certain mass step
Suddenly the CrN/ graphene complexes prepared by (1), ultrasound, stirring it is uniformly dispersed, then 120~160 DEG C react 1~
3h；Product is washed, dried, obtains the fuel-cell catalyst Pt-CrN/ graphene complexes.
Chromic salts described in step (1) is Cr (NO3)3、Cr(ClO4)3、Cr2(SO4)3、CrCl3、K2Cr2O7、K2CrO4With
Na2CrO4In one kind.
Solvent described in step (1) is one kind or wherein several mixed by any ratio in water, methanol, ethanol and isopropanol
The mixture of conjunction.
The mass ratio of chromic salts and graphite oxide described in step (1) is 0.3:1~3:1, the mass ratio of solvent and chromic salts
For 20:1~100:1.
The power of supersound process described in step (1) is 60~110W, and mixing speed is 120~180 revs/min, is stirred
It is 2~5h to mix the time.
Ammonification atmosphere described in step (1) is ammonia, or ammonia is 1 according to volume ratio with nitrogen:1~2:1 it is mixed
Gas is closed, the gas flow of ammonification atmosphere is 80~130mL/min.
Platinum salt described in step (2) is one kind in chloroplatinic acid, potassium chloroplatinate and platinic sodium chloride.
The mass ratio of platinum salt and CrN/ graphene complexes described in step (2) is 0.15:1~0.5:1, can be preferred
For 0.15:1~0.4:1, or 0.15:1~0.3:1；The mass ratio of platinum salt and ethylene glycol is 0.0015:1~0.006:1.
The power of supersound process described in step (2) is 80~130W, and mixing speed is 150~210 revs/min, is stirred
It is 0.5~1h to mix the time.
Present invention also offers a kind of fuel-cell catalyst Pt-CrN/ graphenes obtained by above-mentioned preparation method are compound
Body.
Above-mentioned fuel-cell catalyst Pt-CrN/ graphene complexes can be applied to methanol, formic acid, ethanol electrooxidation and
Oxygen reduction reaction catalyst.
Compared with prior art, the present invention has advantages below and beneficial effect：
(1) technique of the invention is simple, and cost is low, and controllability is good, the method for favorable repeatability, suitable for large-scale production；
The present invention solves costly present in the existing technology for preparing CrN/ Nano Carbon bodies, condition harshness, complex process
The problem of.
(2) product prepared by the present invention has excellent anode of fuel cell oxidation and the moon as fuel-cell catalyst
Pole oxygen reduction catalytic activity.
Brief description of the drawings
Fig. 1 is the X-ray diffraction spectrogram of CrN/ graphene complexes prepared by specific embodiment 25.
Fig. 2 is the Raman spectrogram of CrN/ graphene complexes prepared by specific embodiment 25.
Embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.It should be noted that the combination of the technical characteristic or technical characteristic described in following embodiments is not construed as
Isolated, they can be mutually combined so as to reach superior technique effect.
Embodiment 1：
The preparation method of present embodiment fuel-cell catalyst Pt-CrN/ graphene complexes is completed by following step
's：
(1) preparation of CrN/ graphene complexes：By Cr (NO3)3It is added to the water with graphite oxide, wherein Cr (NO3)3
Mass ratio with graphite oxide is 0.3:1, the mass ratio of water and chromic salts is 100:1；Ultrasound, 180 under the conditions of power is 60W
Rev/min mixing speed under stirring 5h be completely dissolved after, then 110 DEG C heat 12h；After washing, drying, then in ammonia gas
Under atmosphere, ammonia flow 80mL/min, with 5 DEG C/min heating rate, it is warming up to 500 DEG C and is incubated 6h progress nitrogen treatment,
CrN/ graphene complexes are made；
(2) preparation of Pt-CrN/ graphene complexes：Potassium chloroplatinate is dissolved in solvent ethylene glycol, adds certain matter
The CrN/ graphene complexes prepared by step (1) are measured, wherein potassium chloroplatinate and the mass ratio of CrN/ graphene complexes is
0.15:1, the mass ratio of potassium chloroplatinate and ethylene glycol is 0.0015:1, under the conditions of power is 80W ultrasound, 150 revs/min
0.5h is stirred under mixing speed makes it be uniformly dispersed, and then reacts 3h at 120 DEG C；Washing, drying, have obtained Pt-CrN/ graphite
Alkene complex.The methanol electro-oxidizing-catalyzing activity of catalyst, its matter are tested using the cyclic voltammetry method of electrochemical workstation
Amount current density reaches 1500A/g Pt, is 7.5 times of business Pt/C catalyst.
Embodiment 2：Present embodiment is unlike embodiment 1：Chromic salts described in step (1) is Cr
(ClO4)3.The methanol electro-oxidizing-catalyzing activity of catalyst, its quality are tested using the cyclic voltammetry method of electrochemical workstation
Current density reaches 1200A/g Pt, is 6 times of business Pt/C catalyst.
Embodiment 3：Present embodiment is unlike embodiment 2：Chromic salts described in step (1) is Cr2
(SO4)3.The methanol electro-oxidizing-catalyzing activity of catalyst, its quality electricity are tested using the cyclic voltammetry method of electrochemical workstation
Current density reaches 1000A/g Pt, is 5 times of business Pt/C catalyst.
Embodiment 4：Present embodiment is unlike embodiment 3：Chromic salts described in step (1) is CrCl3。
The methanol electro-oxidizing-catalyzing activity of catalyst, its quality current density are tested using the cyclic voltammetry method of electrochemical workstation
Reach 1100A/g Pt, be 5.5 times of business Pt/C catalyst.
Embodiment 5：Present embodiment is unlike embodiment 4：Chromic salts described in step (1) is
K2Cr2O7.The methanol electro-oxidizing-catalyzing activity of catalyst, its quality are tested using the cyclic voltammetry method of electrochemical workstation
Current density reaches 1400A/g Pt, is 7 times of business Pt/C catalyst.
Embodiment 6：Present embodiment is unlike embodiment 5：Chromic salts described in step (1) is K2CrO4
In one kind.The methanol electro-oxidizing-catalyzing activity of catalyst, its matter are tested using the cyclic voltammetry method of electrochemical workstation
Amount current density reaches 1460A/g Pt, is 7.3 times of business Pt/C catalyst.
Embodiment 7：Present embodiment is unlike embodiment 6：Chromic salts described in step (1) is Na2CrO4
In one kind.The methanol electro-oxidizing-catalyzing activity of catalyst, its matter are tested using the cyclic voltammetry method of electrochemical workstation
Amount current density reaches 1420A/g Pt, is 7.1 times of business Pt/C catalyst.
Embodiment 8：Present embodiment is unlike embodiment 7：Solvent described in step (1) is methanol.
The methanol electro-oxidizing-catalyzing activity of catalyst, its quality current density are tested using the cyclic voltammetry method of electrochemical workstation
Reach 1240A/g Pt, be 6.2 times of business Pt/C catalyst.
Embodiment 9：Present embodiment is unlike embodiment 8：Solvent described in step (1) is ethanol.
The methanol electro-oxidizing-catalyzing activity of catalyst, its quality current density are tested using the cyclic voltammetry method of electrochemical workstation
Reach 1160A/g Pt, be 5.8 times of business Pt/C catalyst.
Embodiment 10：Present embodiment is unlike embodiment 9：Solvent described in step (1) is isopropyl
Alcohol.The methanol electro-oxidizing-catalyzing activity of catalyst, its quality electric current are tested using the cyclic voltammetry method of electrochemical workstation
Density reaches 1320A/g Pt, is 6.6 times of business Pt/C catalyst.
Embodiment 11：Present embodiment is unlike embodiment 10：Solvent described in step (1) is methanol
With the mixture of ethanol, the wherein mass ratio of methanol and ethanol is 1:1.Surveyed using the cyclic voltammetry method of electrochemical workstation
The methanol electro-oxidizing-catalyzing activity of catalyst is tried, its quality current density reaches 1560A/g Pt, is business Pt/C catalyst
7.8 again.
Embodiment 12：Present embodiment is unlike embodiment 11：Chromic salts and oxidation described in step (1)
The mass ratio of graphite is 1:1, the mass ratio of solvent and chromic salts is 50:1.Surveyed using the cyclic voltammetry method of electrochemical workstation
The methanol electro-oxidizing-catalyzing activity of catalyst is tried, its quality current density reaches 1180A/g Pt, is business Pt/C catalyst
5.9 again.
Embodiment 13：Present embodiment is unlike embodiment 12：Chromic salts and oxidation described in step (1)
The mass ratio of graphite is 2:1, the mass ratio of solvent and chromic salts is 70:1.Surveyed using the cyclic voltammetry method of electrochemical workstation
The methanol electro-oxidizing-catalyzing activity of catalyst is tried, its quality current density reaches 1280A/g Pt, is business Pt/C catalyst
6.4 again.
Embodiment 14：Present embodiment is unlike embodiment 13：Supersound process described in step (1)
Power is 90W, and mixing speed is 140 revs/min.The first of catalyst is tested using the cyclic voltammetry method of electrochemical workstation
Alcohol electro-oxidizing-catalyzing activity, its quality current density reach 1160A/g Pt, are 5.8 times of business Pt/C catalyst.
Embodiment 15：Present embodiment is unlike embodiment 14：Supersound process described in step (1)
Power is 110W, and mixing speed is 150 revs/min.Catalyst is tested using the cyclic voltammetry method of electrochemical workstation
Methanol electro-oxidizing-catalyzing activity, its quality current density reach 1220A/g Pt, are 6.1 times of business Pt/C catalyst.
Embodiment 16：Present embodiment is unlike embodiment 15：Ammonia gas stream described in step (1)
Measure as 100mL/min.The methanol electro-oxidizing-catalyzing activity of catalyst is tested using the cyclic voltammetry method of electrochemical workstation,
Its quality current density reaches 1260A/g Pt, is 6.3 times of business Pt/C catalyst.
Embodiment 17：Present embodiment is unlike embodiment 16：Ammonia gas stream described in step (1)
Measure as 120mL/min.The methanol electro-oxidizing-catalyzing activity of catalyst is tested using the cyclic voltammetry method of electrochemical workstation,
Its quality current density reaches 1700A/g Pt, is 8.5 times of business Pt/C catalyst.
Embodiment 18：Present embodiment is unlike embodiment 17：Platinum salt described in step (2) is chlorine platinum
Acid.The methanol electro-oxidizing-catalyzing activity of catalyst, its quality electric current are tested using the cyclic voltammetry method of electrochemical workstation
Density reaches 1420A/g Pt, is 7.1 times of business Pt/C catalyst.
Embodiment 19：Present embodiment is unlike embodiment 18：Platinum salt described in step (2) is chlorine platinum
Sour sodium.The methanol electro-oxidizing-catalyzing activity of catalyst, its quality electricity are tested using the cyclic voltammetry method of electrochemical workstation
Current density reaches 1060A/g Pt, is 5.3 times of business Pt/C catalyst.
Embodiment 20：Present embodiment is unlike embodiment 19：Platinum salt and CrN/ described in step (2)
The mass ratio of graphene complex is 0.3:1, the mass ratio of platinum salt and ethylene glycol is 0.002:1.Using electrochemical workstation
The methanol electro-oxidizing-catalyzing activity of cyclic voltammetry method test catalyst, its quality current density reach 1180A/g Pt, are
5.9 times of business Pt/C catalyst.
Embodiment 21：Present embodiment is unlike embodiment 20：Platinum salt and CrN/ described in step (2)
The mass ratio of graphene complex is 0.4:1, the mass ratio of platinum salt and ethylene glycol is 0.003:1.
Embodiment 22：Present embodiment is unlike embodiment 21：Supersound process described in step (2)
Power is 120W, and mixing speed is 160 revs/min.Catalyst is tested using the cyclic voltammetry method of electrochemical workstation
Methanol electro-oxidizing-catalyzing activity, its quality current density reach 1240A/g Pt, are 6.2 times of business Pt/C catalyst.
Embodiment 23：Present embodiment is unlike embodiment 22：Supersound process described in step (2)
Power is 110W, and mixing speed is 170 revs/min.Catalyst is tested using the cyclic voltammetry method of electrochemical workstation
Methanol electro-oxidizing-catalyzing activity, its quality current density reach 1360A/g Pt, are 6.8 times of business Pt/C catalyst.
Embodiment 24：Present embodiment is unlike embodiment 23：Supersound process described in step (2)
Power is 120W, and mixing speed is 200 revs/min.Catalyst is tested using the cyclic voltammetry method of electrochemical workstation
Methanol electro-oxidizing-catalyzing activity, its quality current density reach 1540A/g Pt, are 7.7 times of business Pt/C catalyst.
Embodiment 25：
The preparation method of present embodiment fuel-cell catalyst Pt-CrN/ graphene complexes is completed by following step
's：
(1), the preparation of CrN/ graphene complexes：By K2Cr2O7It is added to the water with graphite oxide, wherein K2Cr2O7With
The mass ratio of graphite oxide is 3:1, the mass ratio of water and chromic salts is 20:1；Power be 110W under the conditions of ultrasound, 120 revs/min
After stirring 2h is completely dissolved under the mixing speed of clock, then in 150 DEG C of heating 4h；After washing, drying, then under ammonia atmosphere,
Ammonia flow is 130mL/min, with 12 DEG C/min heating rate, is warming up to 900 DEG C and is incubated 2h progress nitrogen treatment, be made
CrN/ graphene complexes；
(2), the preparation of Pt-CrN/ graphene complexes：Potassium chloroplatinate is dissolved in solvent ethylene glycol, adds certain matter
The CrN/ graphene complexes prepared by step (1) are measured, wherein potassium chloroplatinate and the mass ratio of CrN/ graphene complexes is
0.25:1, the mass ratio of chloroplatinic acid and ethylene glycol is 0.003:1, under the conditions of power is 130W ultrasound, 210 revs/min stir
Mixing stirring 1h under speed makes it be uniformly dispersed, and then reacts 1h at 160 DEG C；Washing, drying, have obtained Pt-CrN/ graphenes and have answered
It is fit.
Fig. 1 is the X-ray diffraction spectrogram of CrN/ graphene complexes prepared by specific embodiment 25.By that can be seen in figure
Go out obvious CrN characteristic diffraction peaks, illustrate that CrN crystallinity is higher.
Fig. 2 is the Raman spectrogram of CrN/ graphene complexes prepared by specific embodiment 25.D- bands and G- bands in figure
Two peaks are the characteristic peaks of graphene, it was demonstrated that the presence of graphene in complex, therefore illustrate that we are successfully prepared CrN/
Graphene complex.As that can prepare Pt-CrN/ graphene complexes after carrier loaded Pt, this material has excellent
Methanol electro-oxidizing performance.The methanol electro-oxidizing-catalyzing that catalyst is tested using the cyclic voltammetry method of electrochemical workstation is lived
Property, its quality current density reaches 1300A/g Pt, is 6.5 times of business Pt/C catalyst.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (7)
1. a kind of preparation method of fuel-cell catalyst Pt-CrN/ graphene complexes, it is characterised in that including following step
Suddenly：
(1) graphite oxide and chromic salts are added in solvent, ultrasound, stirring be completely dissolved after, in 110~150 DEG C heat 4~
12h；After product is washed, drying, then under ammonification atmosphere, with 5~12 DEG C/min heating rate, 500~900 are warming up to
DEG C and be incubated 2~6h and carry out nitrogen treatment, CrN/ graphene complexes are made；The power of described supersound process be 60~
110W, mixing speed are 120~180 revs/min, and mixing time is 2~5h；Described chromic salts and the mass ratio of graphite oxide are
0.3:1~3:1, the mass ratio of solvent and chromic salts is 20:1~100:1；Described solvent is in water, methanol, ethanol and isopropanol
One kind or wherein several mixtures being mixed by any ratio；
(2) platinum salt is dissolved in solvent ethylene glycol, adds the CrN/ graphene complexes prepared by certain mass step (1),
Ultrasound, stirring make it be uniformly dispersed, and then react 1~3h at 120~160 DEG C；Product is washed, dried, obtains the fuel
Cell catalyst Pt-CrN/ graphene complexes；The mass ratio of described platinum salt and CrN/ graphene complexes is 0.15:1~
0.5:1, the mass ratio of platinum salt and ethylene glycol is 0.0015:1~0.006:1.
2. the preparation method of fuel-cell catalyst Pt-CrN/ graphene complexes according to claim 1, its feature exist
In the chromic salts described in step (1) is Cr (NO3)3、Cr(ClO4)3、Cr2(SO4)3、CrCl3、K2Cr2O7、K2CrO4And Na2CrO4
In one kind.
3. the preparation method of fuel-cell catalyst Pt-CrN/ graphene complexes according to claim 1, its feature exist
In the ammonification atmosphere described in step (1) is ammonia, or ammonia is 1 according to volume ratio with nitrogen:1~2:1 gaseous mixture
Body, the gas flow of ammonification atmosphere is 80~130mL/min.
4. the preparation method of fuel-cell catalyst Pt-CrN/ graphene complexes according to claim 1, its feature exist
In the platinum salt described in step (2) is one kind in chloroplatinic acid, potassium chloroplatinate and platinic sodium chloride.
5. the preparation method of fuel-cell catalyst Pt-CrN/ graphene complexes according to claim 1, its feature exist
In the power of the supersound process described in step (2) is 80~130W, and mixing speed is 150~210 revs/min, mixing time
For 0.5~1h.
6. a kind of fuel-cell catalyst Pt-CrN/ graphene complexes, it is characterised in that it is by any one of claim 1 to 5
The preparation method of described fuel-cell catalyst Pt-CrN/ graphene complexes obtains.
7. electricity of the fuel-cell catalyst Pt-CrN/ graphene complexes as methanol, formic acid and ethanol described in claim 6
Oxidation or the application of oxygen reduction reaction catalyst.
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