CN110071299A - Dilval/nitrogen-doped carbon elctro-catalyst preparation and in the application that can be filled in zinc and air cell - Google Patents
Dilval/nitrogen-doped carbon elctro-catalyst preparation and in the application that can be filled in zinc and air cell Download PDFInfo
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- CN110071299A CN110071299A CN201910351282.2A CN201910351282A CN110071299A CN 110071299 A CN110071299 A CN 110071299A CN 201910351282 A CN201910351282 A CN 201910351282A CN 110071299 A CN110071299 A CN 110071299A
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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
- H01M12/00—Hybrid cells; Manufacture thereof
- H01M12/08—Hybrid cells; Manufacture thereof composed of a half-cell of a fuel-cell type and a half-cell of the secondary-cell type
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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
- H01M4/9041—Metals or alloys
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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
- H01M4/9075—Catalytic material supported on carriers, e.g. powder carriers
- H01M4/9083—Catalytic material supported on carriers, e.g. powder carriers on carbon or graphite
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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
- Y02E60/10—Energy storage using batteries
Abstract
The present invention provides a kind of dilval/nitrogen-doped carbon (NixFey/ N-C) elctro-catalyst preparation method and in the application that can be filled in zinc and air cell.Firstly, a certain amount of Nickelous nitrate hexahydrate (Ni (NO is gradually added in dimethylformamide (DMF)3)2·6H2O), Fe(NO3)39H2O (Fe (NO3)3·9H2O), terephthalic acid (TPA), triethylene diamine and g-C3N4Consistent obtains presoma after stirring a period of time.It takes remaining solid to carry out ambient anneal after solvent is evaporated, obtains NixFey/ N-C as oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) elctro-catalyst and air electrode of zinc-air battery material can be filled.Compared with prior art, preparation process of the invention is simple, obtained NixFey/ N-C catalyst has the performance of catalysis ORR and OER simultaneously, and electro catalytic activity is high.As air electrode of zinc-air battery can be filled, higher open-circuit voltage, biggish output power density and preferable stability can be obtained.
Description
Technical field
The invention belongs to electro-catalysis application fields, and in particular to a kind of dilval/nitrogen-doped carbon (NixFey/ N-C) electricity urges
The preparation method of agent and in the application that can be filled in zinc and air cell.
Background technique
Chargeable zinc-air battery is converted as energy and storage facilities, due to theoretical specific capacity with higher
(1086Wh/kg), high security and low cost and have been favored by people.Air electrode material is as the important of zinc-air battery
Component part, performance are to influence the principal element of battery quality.Therefore, the performance for promoting air electrode material is to promote battery
The key of performance.
It can fill in zinc-air battery, battery air electrode oxygen in electric discharge obtains being electronically generated hydroxyl generation oxygen also
Original reaction (ORR), hydroxyl, which loses, when charging is electronically generated oxygen and occurs to produce oxygen reaction (OER).Therefore, empty as chargeable zinc
The air electrode material in pneumoelectric pond need to have the performance of catalysis ORR and OER simultaneously.Currently, bifunctional catalyst is mainly with your gold
Belong to based on material, such as Pt/C+RuO2、Pt/C+IrO2And Pt/C+Ir/C etc., still, due to its high cost, rare reserves
And long term stability problem, greatly hinder the scale application in industrialized production.Therefore develop has inexpensively, simultaneously
ORR and OER function, and the non-precious metal catalyst of electro catalytic activity and excellent in stability is can to fill air electrode of zinc-air cell
The important research direction of material.
In recent years, due to having, low cost, large specific surface area, activity height, stability is good etc., and advantages exist nitrogen-doped carbon (N-C)
The field ORR is concerned.N atom doped carbon material has excellent ORR electrocatalysis characteristic, but its OER electricity in ORR catalyst
Catalytic performance is poor, cannot function as bifunctional electrocatalyst.A large number of studies show that the transition metal such as simple Ni, Fe or its chemical combination
Object only has an excellent OER performance and ORR poor performance.
Summary of the invention
Dilval nitrogen-doped carbon (Ni in the present inventionxFey/ N-C) elctro-catalyst non precious metal, raw material easily obtain, and make
It is standby low in cost, it is suitble to large-scale production.As the air electrode material that can be filled in zinc-air battery, excellent ORR is shown
Electrocatalysis characteristic and OER electrocatalysis characteristic, have a good application prospect.
In the preferred embodiment, which is Ni2+And Fe3+With g-C3N4It is mixed with to obtain NiFe/N-C electricity
Catalyst.
In further preferred scheme, which is Ni2+And Fe3+With g-C3N4It is mixed with to obtain Ni3Fe/N-C
Elctro-catalyst.
Technical solution of the present invention is the following steps are included: by nickel source, source of iron, g-C3N4In organic solvent, added to benzene
Dioctyl phthalate, triethylene diamine stir evenly, and after evaporating organic solvent, sintering obtains dilval/nitrogen-doped carbon elctro-catalyst.
The g-C3N4It is that 20g urea is subjected to 800-1000 in airoC high temperature pyrolysis obtains.
The nickel source includes Nickelous nitrate hexahydrate Ni (NO3)2·6H2O;The source of iron includes Fe(NO3)39H2O Fe
(NO3)3·9H2O。
The Nickelous nitrate hexahydrate, Fe(NO3)39H2O, terephthalic acid (TPA), triethylene diamine, g-C3N4Mass ratio be
0.01-0.06:0.02-0.12:1-4:2.5-5:2.5-10.
The sintering is in N2Or under Ar atmosphere, with heating rate 1 ~ 3oC/min is warming up to 800-1000oUnder C at annealing
Reason 0.5-1 hours.
The object of the present invention is to provide a kind of novel, efficient, cheap NixFeyThe preparation method of/N-C elctro-catalyst, and
It is applied to the air electrode that can fill zinc and air cell, NiFe/N-C or Ni in further preferred scheme3Fe/N-C is applied to can
Fill the air electrode of zinc and air cell.
Present invention has an advantage that
1. preparing Ni by high temperature pyrolysis methodxFey/ N-C elctro-catalyst, the preparation process is simple, is easily achieved, and is prepared into
The elctro-catalyst arrived has repeatability well.
2.NixFey/ N-C elctro-catalyst is mainly made of the flake graphite containing N doping, is had higher specific surface area, is made
, with excellent ORR catalytic activity, the particle for being uniformly attached to NiFe alloy above is then easy to OER reaction, therefore Ni for itxFey/
N-C elctro-catalyst has excellent ORR and OER electro catalytic activity simultaneously, has potential application in zinc and air cell that can fill.
Detailed description of the invention
Fig. 1 is the SEM photograph of the lower NiFe/N-C elctro-catalyst prepared of embodiment 1.
Fig. 2 is the XRD spectrum and standard PDF card comparison diagram of the lower NiFe/N-C elctro-catalyst prepared of embodiment 1.
Fig. 3 is the lower Ni prepared of embodiment 23Fe/N-C elctro-catalyst and RuO2LSV curve in 1MKOH.
Fig. 4 is the lower Ni prepared of embodiment 23The LSV of Fe/N-C elctro-catalyst and Pt/C in 0.1M KOH when 1600rpm
Curve.
Fig. 5 is the lower Ni prepared of embodiment 23Fe/N-C elctro-catalyst is as battery when can fill air electrode of zinc-air battery
Open-circuit voltage.
Fig. 6 is the lower Ni prepared of embodiment 23Fe/N-C elctro-catalyst is as battery when can fill air electrode of zinc-air battery
Discharge polarization curve.
Fig. 7 is the lower Ni prepared of embodiment 23Fe/N-C elctro-catalyst is as charge and discharge when can fill air electrode of zinc-air battery
Current density is 10mA cm-2When stability test.
Specific embodiment:
Embodiment 1
20g urea is carried out to high temperature pyrolysis in air and obtains g-C3N4, by 0.2 mmol Nickelous nitrate hexahydrate (Ni (NO3)2 ·
6H2) and 0.2mmol Fe(NO3)39H2O (Fe (NO O3)3 ·9H2O it) sequentially adds in 20mL dimethylformamide (DMF), to
0.544g terephthalic acid (TPA), 0.86g triethylene diamine and 0.73 g g-C are added after dissolution3N4, then it is sufficiently stirred for 24 hours;
Obtained solid is again put into after elder generation 4h is warming up to 600 DEG C in tube furnace products therefrom, then passes through 5h liter by then evaporation solvent
Temperature is naturally cooling to room temperature after EP (end of program), to obtain NiFe/N-C elctro-catalyst to 900 DEG C of heat preservation 1h.
Fig. 1 is the SEM figure of the NiFe/N-C elctro-catalyst prepared under the example, and Cong Tuzhong can see that sample mainly by piece
Shape graphite composition, is attached to the particle of some NiFe alloys, also the evengranular distribution of NiFe alloy visible in detail above
On the carbon material, size is about 20-50 nm.
Fig. 2 is the XRD spectrum of the NiFe/N-C elctro-catalyst prepared under the example, and Cong Tuzhong is it can be found that 44o、51oWith
74.5oThe diffraction maximum at place is corresponding with NiFe alloy standard card PDF#47-1417, illustrates the presence of NiFe alloy;Furthermore
26oLocate the typical diffractive peak that wide diffraction maximum is graphitized carbon, illustrates that we are successfully prepared NiFe/N-C material.
Embodiment 2
20g urea is carried out to high temperature pyrolysis in air and obtains g-C3N4, by 0.3 mmol Nickelous nitrate hexahydrate (Ni (NO3)2 ·
6H2) and 0.1 mmol Fe(NO3)39H2O (Fe (NO O3)3 ·9H2O it) sequentially adds in 20mL dimethylformamide (DMF), to
0.544g terephthalic acid (TPA), 0.86g triethylene diamine and 0.73 g g-C are added after dissolution3N4, then it is sufficiently stirred for 24 hours;
Obtained solid is again put into after elder generation 4h is warming up to 600 DEG C in tube furnace products therefrom, then passes through 5h liter by then evaporation solvent
Temperature is naturally cooling to room temperature after EP (end of program), to obtain Ni to 900 DEG C of heat preservation 1h3Fe/N-C elctro-catalyst.
Fig. 3 is the Ni prepared under the example3Fe/N-C elctro-catalyst and RuO2LSV curve in 1 M KOH, Cong Tuzhong
It can be seen that NiFe/N-C elctro-catalyst is compared to RuO in the case where oxygen saturation2Having lower overpotential is 293mV, and
RuO2Current potential be 360 mV, show this method preparation NiFe/N-C elctro-catalyst have excellent OER catalytic performance.
Fig. 4 is the Ni prepared under the example3The LSV of Fe/N-C elctro-catalyst and Pt/C in 0.1M KOH when 1600rpm
Curve, it can be seen that under the conditions of oxygen-saturated, the half wave potential of NiFe/N-C elctro-catalyst is 0.81V, close to business Pt/
C(0.84V), 6.38 mA cm of limiting current density-2, it is higher than Pt/C(5.88 mA cm-2), illustrate the Ni of this method preparation3Fe/
N-C elctro-catalyst also has excellent ORR electrocatalysis characteristic.
Fig. 5 is the Ni prepared under the example3Fe/N-C elctro-catalyst is as battery when can fill air electrode of zinc-air battery
Open-circuit voltage, it can be seen from the figure that Ni3Fe/N-C elctro-catalyst is as open-circuit voltage when can fill air electrode of zinc-air battery
For 1.48V, higher level is in it can fill zinc and air cell field.
Fig. 6 is the Ni prepared under the example3Fe/N-C elctro-catalyst is as battery when can fill air electrode of zinc-air battery
Discharge polarization curve, as can be seen from the figure Ni3Fe/N-C elctro-catalyst can still export biggish electricity in larger voltage
Stream, and peak power output density is 142mW cm-2, it is at the leading level in same system.
Fig. 7 is the Ni prepared under the example3Fe/N-C elctro-catalyst is as charge and discharge when can fill air electrode of zinc-air battery
Electric density is 10mA cm-2When stability test, as can be seen from the figure battery charge and discharge electricity density be 10mA cm-2When, electricity
Still there are lower charging voltage and higher discharge voltage in pond, and by being up to 120 hours cyclic charging and discharging tests, electricity
The charging/discharging voltage in pond does not vary widely, illustrates that stability test is preferable, practical application value with higher.
Embodiment 3
20g urea is carried out to high temperature pyrolysis in air and obtains g-C3N4, by 0.1 mmol Nickelous nitrate hexahydrate (Ni (NO3)2 ·
6H2) and 0.3mmol Fe(NO3)39H2O (Fe (NO O3)3 ·9H2O it) sequentially adds in 20mL dimethylformamide (DMF), to
0.544g terephthalic acid (TPA), 0.86g triethylene diamine and 0.73 g g-C are added after dissolution3N4, then it is sufficiently stirred for 24 hours;
Obtained solid is again put into after elder generation 4h is warming up to 600 DEG C in tube furnace products therefrom, then passes through 5h liter by then evaporation solvent
Temperature is naturally cooling to room temperature after EP (end of program), to obtain NiFe/N-C elctro-catalyst to 900 DEG C of heat preservation 1h.
Embodiment 4
20g urea is carried out to high temperature pyrolysis in air and obtains g-C3N4, by 0.3 mmol Nickelous nitrate hexahydrate (Ni (NO3)2 ·
6H2) and 0.1mmol Fe(NO3)39H2O (Fe (NO O3)3 ·9H2O it) sequentially adds in 20mL dimethylformamide (DMF), to
0.544g terephthalic acid (TPA), 0.86g triethylene diamine and 1.46 g g-C are added after dissolution3N4, then it is sufficiently stirred for 24 hours;
Obtained solid is again put into after elder generation 4h is warming up to 600 DEG C in tube furnace products therefrom, then passes through 5h liter by then evaporation solvent
Temperature is naturally cooling to room temperature after EP (end of program), to obtain Ni to 900 DEG C of heat preservation 1h3Fe/N-C elctro-catalyst.
Claims (10)
1. a kind of dilval/nitrogen-doped carbon elctro-catalyst, which is characterized in that the catalyst is NixFey/ N-C elctro-catalyst.
2. dilval according to claim 1/nitrogen-doped carbon elctro-catalyst, which is characterized in that the catalyst is Ni2+With
Fe3+With g-C3N4It is mixed with to obtain NiFe/N-C elctro-catalyst.
3. dilval according to claim 1/nitrogen-doped carbon elctro-catalyst, which is characterized in that the catalyst is Ni2+With
Fe3+With g-C3N4It is mixed with to obtain Ni3Fe/N-C elctro-catalyst.
4. dilval according to claim 1-3/nitrogen-doped carbon elctro-catalyst, which is characterized in that described
Catalyst is by nickel source, source of iron, g-C3N4In organic solvent, added terephthalic acid (TPA), triethylene diamine stir evenly, and steam
After sending out organic solvent, sintering obtains dilval/nitrogen-doped carbon elctro-catalyst.
5. dilval according to claim 4/nitrogen-doped carbon elctro-catalyst, which is characterized in that the g-C3N4Being will
20g urea carries out 800-1000 in airoC high temperature pyrolysis obtains.
6. dilval according to claim 4/nitrogen-doped carbon elctro-catalyst, which is characterized in that the nickel source includes
Nickelous nitrate hexahydrate Ni (NO3)2·6H2O;The source of iron includes Fe(NO3)39H2O Fe (NO3)3·9H2O。
7. dilval according to claim 6/nitrogen-doped carbon elctro-catalyst, which is characterized in that Nickelous nitrate hexahydrate, nine
Nitric hydrate iron, terephthalic acid (TPA), triethylene diamine, g-C3N4Mass ratio be 0.01-0.06:0.02-0.12:1-4:2.5-
5:2.5-10.
8. dilval according to claim 6/nitrogen-doped carbon elctro-catalyst, which is characterized in that the organic solvent
Including dimethylformamide.
9. dilval according to claim 6/nitrogen-doped carbon elctro-catalyst, which is characterized in that the sintering is in N2
Or under Ar atmosphere, with heating rate 1 ~ 3oC/min is warming up to 800-1000oIt is made annealing treatment 0.5-1 hours under C.
10. dilval according to claim 1-3/nitrogen-doped carbon elctro-catalyst can fill zinc and air cell in preparation
Application on air electrode.
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Cited By (9)
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CN111129522A (en) * | 2019-12-06 | 2020-05-08 | 同济大学 | Preparation and application of nickel-iron alloy/nitrogen-doped carbon fiber serving as zinc-air battery oxygen electrocatalyst |
CN111437858A (en) * | 2020-03-10 | 2020-07-24 | 上海电力大学 | N/O double-doped metal carbon-coated carbide nanoparticle composite material and preparation method thereof |
CN111477883A (en) * | 2020-05-11 | 2020-07-31 | 叶际宽 | MOFs-derived porous carbon-coated NiFe nano-alloy oxygen evolution catalyst and preparation method thereof |
CN112599805A (en) * | 2020-12-16 | 2021-04-02 | 三峡大学 | Preparation method and application of CoSb/NC electrocatalyst |
CN113097498A (en) * | 2021-03-29 | 2021-07-09 | 江苏科技大学 | Iron-cobalt alloy nanocrystalline/nitrogen-doped carbon tube composite material and preparation method and application thereof |
CN113663712A (en) * | 2021-09-16 | 2021-11-19 | 西华师范大学 | Efficient bimetallic OER catalyst derived based on double-template method and preparation method thereof |
CN114481188A (en) * | 2022-01-30 | 2022-05-13 | 吉林大学 | Preparation method of surface nitrogen-doped electrode |
CN114678545A (en) * | 2022-04-08 | 2022-06-28 | 中南大学 | Electrocatalytic material, preparation method and application thereof |
CN117317265A (en) * | 2023-11-30 | 2023-12-29 | 北京大学 | Catalyst, preparation method thereof and zinc-air battery |
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CN111477883A (en) * | 2020-05-11 | 2020-07-31 | 叶际宽 | MOFs-derived porous carbon-coated NiFe nano-alloy oxygen evolution catalyst and preparation method thereof |
CN112599805A (en) * | 2020-12-16 | 2021-04-02 | 三峡大学 | Preparation method and application of CoSb/NC electrocatalyst |
CN113097498A (en) * | 2021-03-29 | 2021-07-09 | 江苏科技大学 | Iron-cobalt alloy nanocrystalline/nitrogen-doped carbon tube composite material and preparation method and application thereof |
CN113663712A (en) * | 2021-09-16 | 2021-11-19 | 西华师范大学 | Efficient bimetallic OER catalyst derived based on double-template method and preparation method thereof |
CN113663712B (en) * | 2021-09-16 | 2023-09-01 | 西华师范大学 | Efficient bimetallic OER catalyst derived based on double-template method and preparation method thereof |
CN114481188A (en) * | 2022-01-30 | 2022-05-13 | 吉林大学 | Preparation method of surface nitrogen-doped electrode |
CN114678545A (en) * | 2022-04-08 | 2022-06-28 | 中南大学 | Electrocatalytic material, preparation method and application thereof |
CN117317265A (en) * | 2023-11-30 | 2023-12-29 | 北京大学 | Catalyst, preparation method thereof and zinc-air battery |
CN117317265B (en) * | 2023-11-30 | 2024-03-26 | 北京大学 | Catalyst, preparation method thereof and zinc-air battery |
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