CN109390598A - A kind of preparation method and applications of difunctional perofskite type oxide oxygen electrode catalyst - Google Patents
A kind of preparation method and applications of difunctional perofskite type oxide oxygen electrode catalyst Download PDFInfo
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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
- H01M4/9016—Oxides, hydroxides or oxygenated metallic salts
- H01M4/9025—Oxides specially used in fuel cell operating at high temperature, e.g. SOFC
- H01M4/9033—Complex oxides, optionally doped, of the type M1MeO3, M1 being an alkaline earth metal or a rare earth, Me being a metal, e.g. perovskites
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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
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Abstract
The present invention is a kind of preparation method and applications of difunctional perofskite type oxide oxygen electrode catalyst.Method includes the following steps: the aqueous solution of lanthanum nitrate, strontium nitrate, nickel nitrate and ferric nitrate is mixed, ethylene glycol then is added to it, then add it in citric acid solution, heating water bath is to 70~90 DEG C until at gel；Gelling temp is finally risen to 650~800 DEG C, keeps the temperature 6~9h；Finally obtain La1‑xSrxNi1‑yFeyO3Powder, i.e., difunctional perofskite type oxide oxygen electrode catalyst；The catalyst is used for the oxygen evolution reaction (OER) and oxygen reduction reaction (ORR) of catalytic fuel cell and electrolytic cell.Main component of the present invention from rich reserves transition metal raw material, it is cheap.
Description
Technical field
The present invention relates to a kind of metal-air cell catalyst, more specifically for be a kind of there is difunctional oxygen electricity to urge
Change active metal-air cell catalyst.
Background technique
Oxygen electro-catalysis, i.e. oxygen reduction reaction and oxygen evolution reaction play extremely important in oxygroup renewable energy technologies
Effect, such as rechargeable metal-air battery, regeneratable fuel cell and water decomposition.Therefore, the exploitation of oxygen catalytic material
These renewable energy technologies with commercial competitiveness are made to become most important.Commercialization hydrogen reduction (ORR) elctro-catalyst at present
Material is Pt/C, and the electrocatalyst materials for being used for oxygen evolution reaction (OER) are then metal oxide containing precious metals (IrO2, RuO2).Although
Pt/C and IrOx, RuO2Elctro-catalyst has low overpotential and high current density and high stability.But they are same
Belong to noble metal, limited resource and high cost limit the widespread commercial of these two types of elctro-catalysts.And these two types are urged
It is perishable under the anti-toxicity and high potential of agent also to limit the development of fuel cell.Therefore, the research of oxide enters
The visual field of people, such as transition metal oxide (such as CoOx/NiCoOx/CoFeOx) and the double oxyhydroxides (LDHs) of transition metal
(such as NiFeOx).Junheng Huang etc. passes through Cl-Intercalation and ultrasonic wave removing obtain the hydroxy cobalt oxide of nano-sheet
(CoOOH), compared to the iridium dioxide (IrO of standard2) its oxygen evolution reaction (OER) performance is 2.4 times high.It is living with high water oxygenization
Property, it is the ideal material of production cleaning, sustainable chemistry fuel.
But the research of single metal oxide is very comprehensive, and perofskite type oxide is moved due to its preferable oxygen
Shifting rate and widely available property (such as LaMO3), it is in the exploratory stage at present.Shao-Horn seminar obtains height by research
Imitate difunctional perovskite elctro-catalyst Ba0.5Sr0.5Co0.8Fe0.2O3-δ, performance has been more than active highest in alkaline medium
IrO2Catalyst, and demonstrate LaNiO3High inherent OER and ORR electro catalytic activity.Wu et al. uses ultrasonic wave by g-C3N4With
LaNiO3It is mixed to get g-C3N4-LaNiO3Composite material.They have found Ni high in composite material3+/Ni2+Ratio is adsorbable more
More hydroxyls, and then promote oxygen evolution reaction (OER).But these perovskite composite oxides only have single electrocatalysis
Can, far from the requirement for meeting metal-air cell and using.Therefore, it is high that base metal base, stability and catalytic performance are found
Difunctional oxygen electrocatalysis material, and develop it in the application of metal-air cell field, there is very important research to anticipate
Justice and application value, are the mains direction of studying of current electrocatalysis material.
Summary of the invention
The present invention is to solve expensive existing for existing oxygen electrode catalyst and shortage of resources and noble metal and urge
Agent only has the problems such as single catalytic performance, provides a kind of preparation of difunctional perofskite type oxide oxygen electrode catalyst
Method and its application.This method uses collosol and gel combination Low Temperature Solid-Phase sintering process, is co-doped with two steps synthesis calcium titanium using strontium and iron
Mine type oxide electrocatalyst.
The technical solution of the present invention is as follows:
A kind of preparation method of difunctional perofskite type oxide oxygen electrode catalyst, comprising the following steps:
Step 1: La is synthesized using sol-gal process1-xSrxNi1-yFeyO3Gel Precursor:
The aqueous solution of isometric lanthanum nitrate, strontium nitrate, nickel nitrate and ferric nitrate is respectively configured；
Wherein, the concentration of lanthanum nitrate hexahydrate is the lanthanum nitrate containing 0.1~0.9g in every 5ml deionized water；In other solution
The amount of substance abides by molar ratio lanthanum nitrate: strontium nitrate: nickel nitrate: ferric nitrate=(1-x): x:(1-y): y；0.2≦x≦0.6；
0.1≦y≦0.7；
Step 2: upper step being obtained into each metal ion salt solution and is mixed, the first mixed solution is obtained, second then is added to it
Glycol obtains the second mixed solution；The second mixed solution is added in citric acid solution again, it is molten that third mixing is obtained after stirring
Liquid；By third mixed solution heating water bath to 70~90 DEG C until at gel；Gelling temp is finally risen to 650~800 DEG C, is protected
6~9h of temperature；Finally obtain La1-xSrxNi1-yFeyO3Powder, i.e., difunctional perofskite type oxide oxygen electrode catalyst；
Wherein, molar ratio is (lanthanum nitrate+strontium nitrate+nickel nitrate+ferric nitrate): citric acid=1:1；The volume of ethylene glycol is
The 20~30% of first mixed solution；Citric acid solution is 0.9~1.1 times of the first mixed liquor volume；
The catalyst is the powdered object for being 100~200nm in partial size.
The application of the difunctional perofskite type oxide oxygen electrode catalyst, it is characterized in that being used for catalytic fuel cell
With the oxygen evolution reaction (OER) and oxygen reduction reaction (ORR) of electrolytic cell.
Substantive distinguishing features of the invention are as follows:
This method uses collosol and gel combination Low Temperature Solid-Phase sintering process, is co-doped with two steps synthesis Ca-Ti ore type oxygen using strontium and iron
Compound elctro-catalyst.Hydrolyze the ion salt solution of nickel nitrate, ferric nitrate, lanthanum nitrate and strontium nitrate at 70~90 DEG C,
And it is cross-linked with each other.Then the porous colloidal sol of formation is flashed into gel using heating water bath；Finally Low Temperature Solid-Phase is combined to be sintered
(650~800 DEG C) synthesis have the perofskite type oxide elctro-catalyst of nano-scale (100~200nm).With other method phases
Than easier, efficiently；Another object of the present invention is: with the conventional precious metal catalyst phase only with single catalytic performance
Than providing a kind of perofskite type oxide elctro-catalyst of non-noble metal double catalytic performances, i.e. oxygen evolution reaction (OER) and oxygen
Reduction reaction (ORR).
Compared with prior art, the invention has the benefit that
1, the perovskite type composite oxide catalyst prepared by the present invention has preferable difunctional electrocatalysis characteristic, oxygen
Gas reduction (ORR) catalytic performance is all improved with oxygen evolution (OER) catalytic performance；
2, the present invention is used as fuel cell and the efficient electrode catalyst of electrolytic cell, and main component is from rich reserves
Transition metal raw material, it is cheap, be ideal oxygen electrode catalyst material；
3, present invention process is simple, is easy to large-scale production, has it in metal-air cell field and potentially answers
Use prospect.
The present invention uses collosol and gel combination Low Temperature Solid-Phase sintering process, is co-doped with two steps synthesis Ca-Ti ore type oxygen using strontium and iron
Compound elctro-catalyst La1-xSrxNi1-yFeyO3.It is catalyzed with the reported at present conventional precious metal with the first catalytic performance
Agent RuO2It compares, with excellent difunctional electrocatalysis characteristic, i.e. oxygen evolution reaction (La0.4Sr0.6Ni0.5Fe0.5O3, 327mV@
10mA/cm2) can and RuO2(320mV@10mA/cm2) matched in excellence or beauty；With other perovskite oxide (LaNiO3) compare, oxygen is also
The take-off potential of original reaction can achieve 870mV, Ta Feier (Tafel) slope 81.05mV/dec, and limiting current density can reach
To 2.8mA/cm2, higher level is in compared to other perovskite oxides.Experimental results show that perovskite aoxidizes
The excellent catalytic performance of object derive from it first is that: the combination of sol-gal process and solid phase method.During colloidal sol becomes gel,
Heating water bath promotes Hydrolysis Reactions of Metal-ions and the abundant hole to be formed that is cross-linked with each other, in conjunction with subsequent Low Temperature Solid-Phase be sintered so that
To catalyst granules be not easy to grow up, in Nano grade (100~200nm) be more conducive to be catalyzed reaction generation；In addition, strontium
BO in perovskite is optimized with the codope of iron6High energy antibonding orbital (e of the transition metal in conjunction with oxygen in octahedrong) electronics
It is filled into 1.2.In addition, raw material sources used by the catalyst are in the transition metal of rich content, and it is cheap, it is ideal
Oxygen electrode catalyst material, effective solution precious metal catalyst agent content rare problem.In metal-air battery and fuel
The fields such as battery also have broad application prospects.
Detailed description of the invention
Fig. 1 is X-ray diffraction (XRD) figure of the perovskite oxide prepared in embodiment 2-6；
Fig. 2 is embodiment 2-6, oxygen evolution reaction (OER) polarization curve of the perovskite oxide prepared in 9；
Fig. 3 is X-ray diffraction (XRD) figure of the perovskite oxide prepared in embodiment 1,7-9；
Fig. 4 is oxygen evolution reaction (OER) polarization curve of the perovskite oxide prepared in embodiment 1,7-9；
Fig. 5 is X-ray diffraction (XRD) figure of the perovskite oxide prepared in embodiment 3,6,8,9；
Fig. 6 is oxygen evolution reaction (OER) polarization curve of the perovskite oxide prepared in embodiment 3,6,8,9；
Fig. 7 is oxygen reduction reaction (ORR) polarization curve of the perovskite oxide prepared in embodiment 3,8,9；
Fig. 8 is the perovskite oxide LaNiO prepared in embodiment 93Scanning figure (SEM)；
Fig. 9 is the LaNi of perovskite oxide prepared by embodiment 30.5Fe0.5O3Scanning figure (SEM)；
Figure 10 is the La of the perovskite oxide prepared in embodiment 80.4Sr0.6Ni0.5Fe0.5O3Scanning figure (SEM).
Specific embodiment
Technical solution of the present invention is further illustrated combined with specific embodiments below.
The preparation of bi-functional oxygen electrode catalyst
Embodiment 1:
The present embodiment perovskite catalysts for bifunctional oxygen electrode, prepares as follows:
(1) La is synthesized using sol-gal process1-xSrxNi1-yFeyO3；
A: using deionized water as solvent, citric acid and ethylene glycol are respectively complexing agent, thickener, prepare citric acid, second two
The mixed solution of alcohol and soluble metallic salt；
A1: 5ml deionized water and 0.6928g La (NO are added in 20ml beaker3)2·6H2O (i.e. 1.6mmol), obtains La
(NO3)2Solution；
A2: 5ml deionized water and 0.29081gNi (NO are added in 20ml beaker3)2·6H2O obtains Ni (NO3)2Solution
(1mmol Ni(NO3)2·6H2O)；
A3: 5ml deionized water and 0.4040g Fe (NO are added in 20ml beaker3)3·9H2O (i.e. 1mmol Fe
(NO3)3·9H2O), Fe (NO is obtained3)3Solution；
A4: 5ml deionized water and 0.08465g Sr (NO are added in 20ml beaker3)2·4H2O (i.e. 0.4mmol Sr
(NO3)2·4H2O), obtain Sr (NO3)2Solution；
A5: 20ml deionized water and 0.84056g citric acid (i.e. 4mmol) are added in 50ml beaker, it is molten to obtain citric acid
Liquid；
A6: above-mentioned solution and 5ml ethylene glycol are added sequentially in citric acid solution, stirring 30 minutes to be uniformly mixed,
It gets a uniform mixture；
B: mixed solution is formed into transparent colloid, then by transparent adhesive tape to holding temperature 6h after 85 DEG C using heating water bath
Body is dried into xerogel for 120 DEG C in an oven；
C: gel powder grinding is placed in Muffle furnace at powder by grinding xerogel, by Muffle in-furnace temperature with 5 DEG C/
The rate of min is warming up to 750 DEG C, closes Muffle furnace after constant temperature 10h, and sample is taken out when Muffle furnace is naturally cooling to room temperature, will
Sample after being grinded with a mortar to get arrive perovskite composite oxide La0.8Sr0.2Ni0.5Fe0.5O3。
Following means of testing: X-ray diffraction spectrum (cloth has been carried out to prepared perovskite catalysts for bifunctional oxygen electrode
Luke (D8advance)), transmission electron microscope (Flied emission transmission electron microscope (Tecnai G2F20)), scanning electron microscope (scanning electricity
Sub- microscope (Hitachi, Japan, S-4800)), electrochemical workstation (CHI750E type), Pine electrochemical workstation；
Embodiment 2: by the La (NO of step a1 in embodiment 13)2·6H2O is 2mmol, and quality is 0.86604g；A2's
Ni(NO3)2·6H2O is 1.4mmol, and quality is 0.4071g；Fe (the NO of a33)3·9H2O is 0.6mmol, and quality is
0.2424g, no a4 step；
Embodiment 3: by the La (NO of step a1 in embodiment 13)2·6H2O is 2mmol, and quality is 0.86604g；A2's
Ni(NO3)2·6H2O is 1mmol, and quality is 0.29081g；Fe (the NO of a33)3·9H2O is 1mmol, and quality is
0.404g, no a4 step；
Embodiment 4: by the La (NO of step a1 in embodiment 13)2·6H2O is 2mmol, and quality is 0.86604g；A2's
Ni(NO3)2·6H2O is 0.6mmol, and quality is 0.1745g；Fe (the NO of a33)3·9H2O is 1.4mmol, and quality is
0.5656g, no a4 step；
Embodiment 5: by the La (NO of step a1 in embodiment 13)2·6H2O is 2mmol, and quality is 0.86604g；A2's
Ni(NO3)2·6H2O is 0.2mmol, and quality is 0.05816g；Fe (the NO of a33)3·9H2O is 1.8mmol, and quality is
0.7272g, no a4 step；
That is embodiment 2,3,4,5 that obtain is comparative sample LaNi1-yFeyO3。
Embodiment 6: by the La (NO of step a1 in embodiment 13)2·6H2O is 2mmol, and quality is 0.86604g；A3's
Fe(NO3)3·9H2O is 2mmol, and quality is 0.808g, no a2, a4 step；
That i.e. the present embodiment obtains is contrast sample LaFeO3。
Embodiment 7: by the La (NO of step a1 in embodiment 13)2·6H2O is 1.2mmol, and quality is 0.5196g；a2
Ni (NO3)2·6H2O is 1mmol, and quality is 0.29081g；Fe (the NO of a33)3·9H2O is 1mmol, and quality is
Sr (the NO of 0.404g, a43)2·4H2O is 0.8mmol, and quality is 0.1693g；
That i.e. the present embodiment obtains is perovskite composite oxide La0.6Sr0.4Ni0.5Fe0.5O3。
Embodiment 8: by the La (NO of step a1 in embodiment 13)2·6H2O is 0.8mmol, and quality is 0.3464g；a2
Ni (NO3)2·6H2O is 1mmol, and quality is 0.29081g；Fe (the NO of a33)3·9H2O is 1mmol, and quality is
Sr (the NO of 0.404g, a43)2·4H2O is 1.2mmol, and quality is 0.2540g；
That i.e. the present embodiment obtains is perovskite composite oxide La0.4Sr0.6Ni0.5Fe0.5O3。
Embodiment 9: by the La (NO of step a1 in embodiment 13)2·6H2O is 2mmol, and quality is 0.86604g；A2's
Ni(NO3)2·6H2O is 2mmol, and quality is 0.58162g；Without a3, a4 step；
That i.e. the present embodiment obtains is contrast sample LaNiO3。
Test result: as seen from Figure 1, it can be seen that as the doping of Fe increases, LaNi1-yFeyO3Peak position by
It gradually deviates to the left, and crystallinity increases therewith.It is compared with standard cadmium ferrite PDF card, main strong peak is corresponding accurate, thus can be with
Find out and adulterates successfully.The LaNiO synthesized as can be seen from Figure 8 simultaneously3Made of the little particle of mainly 400~500nm is reunited
Bulky grain, and be evenly distributed；The LaNi after Fe is adulterated as can be seen from Figure 90.5Fe0.5O3The bulky grain of reunion has fragmentation to become smaller,
The surface area of catalyst is increased, catalysis is conducive to.Fig. 2 can be seen that the doping variation with Fe, and OER performance also occurs first therewith
The trend of reduction after increase, compared to LaNiO3, LaNi0.5Fe0.5O3Show higher current density and lower 10mA/cm2
Overpotential.For this purpose, we have selected the Fe amount of mixing up for 0.5 optimum condition as experiment.This also illustrates Fe introducings can be very
LaNiO is improved in big degree3Catalytic activity.This experiment is the mode based on doping, similar with Fe doping, and Fig. 3 is in calcium titanium
The double-perovskite X-ray diffractogram (XRD) of A, mine doping Sr can still obtain after the introducing that similarly can be seen that Sr in figure
Obtain the double-perovskite La of pure object phase1-xSrxNi0.5Fe0.5O3.And as can be seen from Figure 10: compared to LaNiO3With
LaNi0.5Fe0.5O3, La0.4Sr0.6Ni0.5Fe0.5O3Particle it is smaller, and it is uniformly many to be distributed more other two type oxides,
Particle size is distributed in 100~200nm, and specific surface area is bigger, and catalytic activity is higher, is more favorable for the generation of catalytic process.It is logical
Crossing the available optimal Sr doping of comparison oxygen evolution reaction (OER) performance is 0.6.It, can be with from Fig. 5 after the above results are summarized
Find out that codope makes the double-perovskite La obtained0.4Sr0.6Ni0.5Fe0.5O3Diffraction peak energy and standard cadmium ferrite (LaFeO3) and nickel acid
Lanthanum (LaNiO3) PDF card is corresponding accurate, thus codope does not destroy perovskite crystal structure.Fig. 6 and Fig. 7 is analysis respectively
Oxygen reacts the polarization curve of (OER) and oxygen reduction reaction (ORR), and Dependence Results show double-perovskite La0.4Sr0.6Ni0.5Fe0.5O3
With better than nickel acid lanthanum (LaNiO3) and cadmium ferrite (LaFeO3) oxygen evolution reaction (OER) and oxygen reduction reaction (ORR) performance.
In OER catalytic process, double-perovskite oxide La0.4Sr0.6Ni0.5Fe0.5O3Reaching current density is 10mA/cm2Current potential only
For 327mV, limiting current density can achieve 140mA/cm2；In ORR catalytic process, take-off potential can achieve 870mV,
Tafel slope drops to 81.05mV/dec, and limiting current density can achieve 2.8mA/cm2.Compared to other perovskite oxides
In higher level.
(explanation: OER test is completed on CHI750E electrochemical workstation, and catalyst is coated on glassy carbon electrode
As working electrode, lead to half an hour O before test in the electrolyte of 1M KOH2To oxygen saturation, then in lower throughput
Lower carry out dependence test, the voltage range of setting are 0-0.8V (vs.SCE), and sweeping speed is 1mV s-1, the LSV curve measured is indulged
Coordinate transformation is current density, available LSV polarization curve.ORR test is completed on Pine electrochemical workstation, is surveyed
Method for testing is essentially the same, and the voltage range of setting is 0.1- (- 0.9) V (vs.SCE), and sweeping speed is 1mV s-1.The pole LSV can be obtained
Change curve.)
According to result above, it can be seen that method proposed by the present invention is simple and efficient, convenient and efficient；With being closed under simple process
At the double-perovskite oxide for providing double-function catalyzing effect, and the double-perovskite oxide synthesized
La0.4Sr0.6Ni0.5Fe0.5O3With high activity and durability, have in the storage of various electrochemical energies and conversion equipment extensive
Application prospect, such as the fields such as alkaline fuel cell and metal-air battery.
Illustrative description has been done to the present invention above, it should explanation, the case where not departing from core of the invention
Under, any simple deformation, modification or other skilled in the art can not spend the equivalent replacement of creative work equal
Fall into protection scope of the present invention.
Unaccomplished matter of the present invention is well-known technique.
Claims (3)
1. a kind of preparation method of difunctional perofskite type oxide oxygen electrode catalyst, it is characterized in that this method includes following step
It is rapid:
Step 1: La is synthesized using sol-gal process1-xSrxNi1-yFeyO3Gel Precursor:
The aqueous solution of isometric lanthanum nitrate, strontium nitrate, nickel nitrate and ferric nitrate is respectively configured；
Wherein, the concentration of lanthanum nitrate hexahydrate is the lanthanum nitrate containing 0.1~0.9g in every 5ml deionized water；Substance in other solution
Amount abide by molar ratio lanthanum nitrate: strontium nitrate: nickel nitrate: ferric nitrate=(1-x): x:(1-y): y；0.2≦x≦0.6；0.1
≦y≦0.7；
Step 2: upper step is obtained into each metal ion salt solution and is mixed, the first mixed solution is obtained, ethylene glycol then is added to it,
Obtain the second mixed solution；The second mixed solution is added in citric acid solution again, third mixed solution is obtained after stirring；It will
Third mixed solution heating water bath is to 70~90 DEG C until at gel；Gelling temp is finally risen to 650~800 DEG C, heat preservation 6~
9h；Finally obtain La1-xSrxNi1-yFeyO3Powder, i.e., difunctional perofskite type oxide oxygen electrode catalyst；
Wherein, molar ratio is (lanthanum nitrate+strontium nitrate+nickel nitrate+ferric nitrate): citric acid=1:1；The volume of ethylene glycol is first
The 20~30% of mixed solution；Citric acid solution is 0.9~1.1 times of the first mixed liquor volume.
2. the preparation method of difunctional perofskite type oxide oxygen electrode catalyst as described in claim 1, it is characterized in that
To catalyst be partial size be 100~200nm powdered object.
3. the application of difunctional perofskite type oxide oxygen electrode catalyst as described in claim 1, it is characterized in that for urging
Change the oxygen evolution reaction (OER) and oxygen reduction reaction (ORR) of fuel cell and electrolytic cell.
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