CN104009242B - The porous carbon network structure material preparation method of the N doping of a kind of fuel battery cathod catalyst metal/metal oxide load - Google Patents
The porous carbon network structure material preparation method of the N doping of a kind of fuel battery cathod catalyst metal/metal oxide load Download PDFInfo
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- CN104009242B CN104009242B CN201410181761.1A CN201410181761A CN104009242B CN 104009242 B CN104009242 B CN 104009242B CN 201410181761 A CN201410181761 A CN 201410181761A CN 104009242 B CN104009242 B CN 104009242B
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- Y02E60/13—Energy storage using capacitors
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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
A kind of porous carbon network structure material preparation method of N doping of metal/metal oxide load, the present invention take natural polymer as raw material, add metal salt solution, forming colloidal sol, by adding alkaline matter, obtaining hydrogel, it is washed, freeze drying, obtain the gel done, dry gel is used nitrogen atmosphere heat treatment in tube furnace, obtains product.The present invention 1. is Carbon and nitrogen sources with natural polymer, and source nature, can circulate, this biological quality is large.2.? the material of preparation is the porous carbon network structure material of metal/metal oxide load.3. the material that prepared by the method has very outstanding oxygen electrical catalyze reduction performance.This material very also can have potential using value in various fields such as ultracapacitor, lithium ion battery, organic catalysis, photocatalysis, gas absorption.
Description
Technical field
The invention belongs to carbon composite nano-material field, particularly relate to a kind of preparation method of N doping porous carbon composite network structural material.
Background technology
Porous carbon materials, owing to having large specific area, is widely used in electro-catalysis, organic catalysis, ultracapacitor, photocatalysis, sewage disposal, gas absorption etc.Because N doping can change very many-sided performance of material with carbon element, the porous carbon materials of N doping has potential application in a lot of fields.Such as in fuel battery cathod catalyst method, the porous carbon materials of N doping is desirable catalyst carrier.Metal oxide can work in coordination with the material with carbon element of N doping the performance (improving oxygen Electrochemical Properties) strengthening fuel battery cathod catalyst.Develop the fuel battery cathod catalyst that simple to operate, that raw material sources is cheap method carrys out processability excellent significant.
Summary of the invention
In view of this, the technical problem to be solved in the present invention is to provide a kind of natural polymer to be the porous carbon network structure material that the N doping of metal/metal oxide load prepared by raw material, and the network combined structural material of porous carbon provided by the invention shows significant oxygen Electrochemical Properties.
Take natural polymer chitosan as raw material, add metal salt solution, form colloidal sol, by adding alkaline matter, obtaining hydrogel, it is washed, freeze drying, obtain the gel done, dry gel is used nitrogen atmosphere heat treatment in tube furnace, obtains product.
The present invention adopts following technical scheme to achieve these goals:
A porous carbon network structure material preparation method for the N doping of fuel battery cathod catalyst metal/metal oxide load, is characterized in that: comprise the following steps:
A) take natural polymer chitosan as raw material, add metal salt solution, form colloidal sol;
B) by slowly adding alkalescent material, obtaining hydrogel, it is washed, freeze drying, obtain the gel done;
C) dry gel is used nitrogen atmosphere heat treatment in tube furnace, temperature is 750-850 DEG C, and the time is 0.5-2.5h, obtains product.
The porous carbon network structure material preparation method of the N doping of a kind of metal/metal oxide load of described fuel battery cathod catalyst, is characterized in that: the weight ratio of shitosan and metal salt solution is 2-4:6-10.
The porous carbon network structure material preparation method of the N doping of described a kind of fuel battery cathod catalyst metal/metal oxide load, it is characterized in that: described step a) specifically comprises: take appropriate shitosan, with the acetate dissolution of about 5%, add Co (NO wherein
3)
2, or Mn (NO
3)
2or Ni (NO
3)
2, magnetic agitation, forms uniform colloidal sol.
The porous carbon network structure material preparation method of the N doping of described a kind of fuel battery cathod catalyst metal/metal oxide load, it is characterized in that: described step b) specifically comprise: slowly add ammoniacal liquor with buret, after 1-8 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done.
Compared with prior art, the invention provides a kind of porous carbon network structure material preparation method of N doping of metal/metal oxide load, the present invention has following features:
1. be Carbon and nitrogen sources with natural polymer chitosan, source nature, can circulate, this biological quality is large.Whole material preparation method is simple, is easy to realize industrialization.
2. the porous carbon network structure material of the N doping of metal/metal oxide load that prepared by the method has very outstanding oxygen electrical catalyze reduction performance.
3. the porous carbon network structure material of synthesis, BET surface area is large, and the nitrogen element content of doping is high.This material probably also can have potential using value in various fields such as ultracapacitor, lithium ion battery, organic catalysis, photocatalysis, gas absorption.
Accompanying drawing explanation
In Fig. 1, Fig. 1 a is the stereoscan photograph of the product that the embodiment of the present invention 1 prepares; Fig. 1 b is the transmission electron microscope photo of the product that the embodiment of the present invention 1 prepares; Fig. 1 c is the high-resolution-ration transmission electric-lens photo of the product that the embodiment of the present invention 1 prepares;
Fig. 2 is the x-ray diffraction pattern of the product that the embodiment of the present invention 1 prepares;
Fig. 3 is the BET result of the product that the embodiment of the present invention 1 prepares;
Fig. 4 is oxygen electroreduction catalytic performance and its stability of the product that the embodiment of the present invention 1 prepares.
Embodiment,
In order to further illustrate the present invention, below in conjunction with embodiment, product preparation method provided by the invention is described in detail.
Embodiment 1
Take 2 grams of shitosans, use 5% acetate dissolution, add Co (NO wherein
3)
25 grams, magnetic agitation 2 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 2-6 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 800 DEG C, time 1.5h in tube furnace.Obtain product.
Embodiment 2
Take 2 grams of shitosans, use 5% acetate dissolution, add Co (NO wherein
3)
210 grams, magnetic agitation 1 hour, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-8 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 750 DEG C, time 1.5h in tube furnace.Obtain product.
Embodiment 3
Take 4 grams of shitosans, use 5% acetate dissolution, add Co (NO wherein
3)
210 grams, magnetic agitation 2 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 4-8 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 750 DEG C, time 2h in tube furnace.Obtain product.
Embodiment 4
Take 2 grams of shitosans, use 5% acetate dissolution, add Co (NO wherein
3)
210 grams, magnetic agitation 0.5 hour, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-10 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 700 DEG C, time 2.5h in tube furnace.Obtain product.
Embodiment 5
Take 2 grams of shitosans, use 5% acetate dissolution, add Co (NO wherein
3)
24 grams, magnetic agitation 0.5 hour, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-6 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 750 DEG C, time 1h in tube furnace.Obtain product.
Embodiment 6
Take 2 grams of shitosans, use 5% acetate dissolution, add Co (NO wherein
3)
26 grams, magnetic agitation 1.5 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 2-3 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 750 DEG C, time 2h in tube furnace.Obtain product.
Embodiment 7
Take 2 grams of shitosans, use 5% acetate dissolution, add Ni (NO wherein
3)
26 grams, magnetic agitation 1.5 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-6 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 750 DEG C, time 1h in tube furnace.Obtain product.
Embodiment 8
Take 2 grams of shitosans, use 5% acetate dissolution, add Ni (NO wherein
3)
28 grams, magnetic agitation 1 hour, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-6 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 800 DEG C, time 2h in tube furnace.Obtain product.
Embodiment 9
Take 4 grams of shitosans, use 5% acetate dissolution, add Ni (NO wherein
3)
28 grams, magnetic agitation 2 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-6 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 700 DEG C, time 1h in tube furnace.Obtain product.
Embodiment 10
Take 4 grams of shitosans, use 5% acetate dissolution, add Mn (NO wherein
3)
28 grams, magnetic agitation 2 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 2-6 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 750 DEG C, time 1h in tube furnace.Obtain product.
Embodiment 11
Take 4 grams of shitosans, use 5% acetate dissolution, add Mn (NO wherein
3)
210 grams, magnetic agitation 2 hours, forms uniform colloidal sol.Be placed in the atmosphere of ammonia, 3-6 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done, dry gel used nitrogen atmosphere heat treatment, 800 DEG C, time 1h in tube furnace.Obtain product.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (3)
1. a preparation method for the porous carbon network structure material of the N doping of fuel battery cathod catalyst metal/metal oxide load, is characterized in that: comprise the following steps:
A) take natural polymer chitosan as raw material, take appropriate shitosan, with the acetate dissolution of 5%, add metal salt solution wherein, form colloidal sol; Wherein slaine is Co (NO
3)
2, Mn (NO
3)
2or Ni (NO
3)
2;
B) by slowly adding alkalescent material, obtaining hydrogel, it is washed, freeze drying, obtain the gel done;
C) dry gel is used nitrogen atmosphere heat treatment in tube furnace, temperature is 750-850
oc, the time is 0.5-2.5h, obtains product.
2. the preparation method of the porous carbon network structure material of the N doping of fuel battery cathod catalyst metal/metal oxide according to claim 1 load, is characterized in that: the weight ratio of shitosan and metal salt solution is 2-4:6-10.
3. the preparation method of the porous carbon network structure material of the N doping of fuel battery cathod catalyst metal/metal oxide according to claim 1 load, it is characterized in that: described step b) specifically comprises: slowly add ammoniacal liquor with buret, after 1-8 hour, obtain hydrogel, it is washed, freeze drying, obtain the gel done.
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| CN104617311A (en) * | 2014-11-20 | 2015-05-13 | 安徽大学 | Nitrogen and cobalt doped mesoporous carbon/graphene composite material and preparation method thereof |
| CN106252673B (en) * | 2016-08-22 | 2019-06-25 | 首都师范大学 | A kind of preparation method of the Fe-N/C oxygen reduction reaction catalyst based on natural plants tissue |
| CN106356537B (en) * | 2016-11-18 | 2019-05-28 | 中南大学 | A kind of preparation method of N doping porous carbon foam material and its application in metal-air battery |
| CN106783236B (en) * | 2017-02-20 | 2018-08-10 | 青岛科技大学 | A kind of N doping graphitized carbon/transition metal oxide nano composite material and preparation method thereof |
| CN107293730B (en) * | 2017-07-31 | 2020-06-16 | 中南大学 | Ni @ N-C composite positive electrode material, preparation method and application in lithium air battery |
| CN107578928B (en) * | 2017-09-11 | 2019-01-11 | 桂林电子科技大学 | A kind of nickel based on persimmon tannin absorption, the porous carbon composite of cobalt doped and its preparation method and application |
| CN107958793B (en) * | 2017-11-07 | 2019-05-21 | 桂林电子科技大学 | A kind of three-dimensional grapheme and preparation method and application of CoO doping |
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| CN111434607A (en) * | 2019-01-11 | 2020-07-21 | 国家纳米科学中心 | Metal phosphide and heteroatom-doped porous carbon composite material and preparation and application thereof |
| CN109678133A (en) * | 2019-01-14 | 2019-04-26 | 桂林电子科技大学 | A kind of C-base composte material and its preparation method and application of nickel oxide doping |
| CN112198201B (en) * | 2020-07-27 | 2022-05-20 | 重庆医科大学 | Indole electrochemical sensor constructed based on nitrogen-doped ordered mesoporous carbon modified electrode and application thereof |
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| CN112736261A (en) * | 2021-01-07 | 2021-04-30 | 天津大学 | Porous carbon network supported platinum nanoparticle composite catalyst and preparation method thereof |
| CN113782743B (en) * | 2021-08-27 | 2022-07-12 | 合肥国轩高科动力能源有限公司 | Lithium ion battery positive electrode material and preparation method and application thereof |
| CN115382533A (en) * | 2022-04-11 | 2022-11-25 | 嘉兴学院 | Method for directly preparing and molding spherical metal oxide-based catalyst |
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Application publication date: 20140827 Assignee: Chizhou Kecheng new material development Co., Ltd. Assignor: Anhui University Contract record no.: X2019340000004 Denomination of invention: Preparation method of fuel cell cathodic catalyst metal/metal oxide loaded nitrogen-doped porous carbon network-structure material Granted publication date: 20160210 License type: Exclusive License Record date: 20190926 |