CN109192998A - A kind of nitrogen co-doped composite Nano carbon material of cobalt-and its preparation method and application - Google Patents

A kind of nitrogen co-doped composite Nano carbon material of cobalt-and its preparation method and application Download PDF

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Publication number
CN109192998A
CN109192998A CN201810926950.5A CN201810926950A CN109192998A CN 109192998 A CN109192998 A CN 109192998A CN 201810926950 A CN201810926950 A CN 201810926950A CN 109192998 A CN109192998 A CN 109192998A
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China
Prior art keywords
cobalt
nitrogen
composite nano
carbon material
doped composite
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CN201810926950.5A
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Chinese (zh)
Inventor
张超
陈山
刘天西
封其春
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Donghua University
National Dong Hwa University
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Donghua University
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • H01M4/88—Processes of manufacture
    • H01M4/8825—Methods for deposition of the catalytic active composition
    • 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
    • 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
    • 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 present invention provides nitrogen co-doped composite Nano carbon material of a kind of cobalt-and its preparation method and application, which is made after the nitrogen co-doped composite nano materials presoma of cobalt-to be transferred under inert atmosphere to heat up be carbonized using a step solvent-thermal method and be made；The preparation method comprises the following steps: by melamine, Cobalt salts and terephthalaldehyde are dissolved separately in solvent, carry out solvent thermal reaction, filtering, it is centrifuged and is dried to obtain powder, acetone is added to mix, is centrifugated out slurry of solids, washs, vacuum drying obtains presoma, it is placed on heating under inert atmosphere to be carbonized, finally washes, is dried in vacuo, obtain the nitrogen co-doped composite Nano carbon material of cobalt-.The method of the present invention is simple, and precursor preparation is easy, and-nitrogen co-doped composite Nano carbon material is prepared in step carbonization, and the material catalytic performance is excellent, good cycling stability；It is relatively cheap as non-precious metal catalyst material, above there is good prospect in the application of Proton Exchange Membrane Fuel Cells energy storage material.

Description

A kind of nitrogen co-doped composite Nano carbon material of cobalt-and its preparation method and application
Technical field
The invention belongs to electrode catalyst of fuel cell Material Field, in particular to composite Nano carbon materials preparation method for material and Applied technical field.
Background technique
With the rapid development of the global economy, the worsening of fossil fuel rapidly depleted with environmental pollution, to can hold Continuous and renewable energy demand is continuously increased, this have stimulated researcher to high-efficiency cleaning energy conversion, develop novel storage Equipment is furtherd investigate to meet the nervous energy demand in the following whole world.
The feature that Proton Exchange Membrane Fuel Cells is protruded due to it in various energy storage devices: such as high conversion efficiency, fuel It is easy to get, environmental-friendly, long circulation life and outstanding stability and safety become current ubiquitous portal The next-generation energy storage system of potential application in electronic product, power supply backup and hybrid vehicle.Recently, proton exchange membrane Fuel cell is successfully applied to New-energy electric vehicle.
Sustainable and environment friendly material is mentioned, people expect being exactly carbon material first.The source of carbon material is very It is abundant, be it is inexhaustible, chemical contamination is small.In general, the transfer efficiency of Proton Exchange Membrane Fuel Cells and Catalyst material on electrode used in cyclical stability strong depend-ence.Various porous carbon materials are fired for proton exchange membrane Expect the common material of catalyst material crime on battery electrode, by electrode/electrolyte interface adsorption of oxygen carry out oxygen also Original reaction.Active carbon (AC) based on carbon, the derivative (CDC) of carbon, the porous material such as carbon nanotube (CNT) and graphene (GR) Expect the specific surface area height due to them, electric conductivity height and excellent chemical stability and thermal stability and is used as by further investigation Catalyst on the electrode of Proton Exchange Membrane Fuel Cells.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of nitrogen co-doped composite Nano carbon material of cobalt-and its preparation sides Method and application, this method design is simple, is easy preparation；The nitrogen co-doped composite Nano carbon material of the cobalt-, catalytic performance is excellent, follows Ring stability is good, relatively cheap as non-precious metal catalyst material, in Proton Exchange Membrane Fuel Cells energy storage material using upper There is good prospect.
In order to solve the above-mentioned technical problems, the present invention provides a kind of nitrogen co-doped composite Nano carbon material of cobalt-, features It is, is made to be transferred under inert atmosphere after the nitrogen co-doped composite nano materials presoma of cobalt-using a step solvent-thermal method and heat up Carbonization is carried out to be made.
Preferably, the nitrogen co-doped composite nano materials presoma of the cobalt-be by melamine, four acetate hydrate cobalts and Terephthalaldehyde is made by solvent-thermal method.
The present invention also provides the preparation methods of the nitrogen co-doped composite Nano carbon material of above-mentioned cobalt-, which is characterized in that packet Include following steps:
(1) melamine, Cobalt salts and terephthalaldehyde are dissolved separately in solvent, are carried out in addition reaction kettle molten Agent thermal response, filtering are centrifuged and are dried to obtain powder, and acetone supersound washing is added, is centrifugated out slurry of solids, wash, and do It is dry, obtain the nitrogen co-doped composite nano materials presoma of cobalt-；
(2) the nitrogen co-doped composite nano materials presoma of cobalt-obtained is placed in heating under inert atmosphere to be carbonized, most It washes, be dried in vacuo afterwards, obtain the nitrogen co-doped composite Nano carbon material of cobalt-.
Preferably, the molar ratio of the melamine in the step (1), Cobalt salts and terephthalaldehyde is 20:1:30.
Preferably, the Cobalt salts in the step (1) are four acetate hydrate cobalts.
Preferably, the solvent in the step (1) is DMF, and reaction temperature is 150-200 DEG C.
Preferably, the inert atmosphere in the step (2) is argon atmosphere.
Preferably, the technological parameter of the carbonization in the step (2) are as follows: 2-5 DEG C of heating rate/min, carburizing temperature 700- 900 DEG C, soaking time 1-5h.
Preferably, 6-12h is washed with deionized to adopt in step (2) washing.
Preferably, the vacuum drying in the step (1) and (2) is the 60-100 DEG C of dry 6-18h in vacuum drying oven.
The present invention also provides a kind of non noble metal oxygen reduction catalysts, which is characterized in that is co-doped with containing above-mentioned cobalt-nitrogen Miscellaneous composite Nano carbon material.
The present invention also provides above-mentioned non noble metal oxygen reduction catalysts in the storage for preparing Proton Exchange Membrane Fuel Cells Application in energy material.
Compared with prior art, the beneficial effects of the present invention are:
(1) the method for the present invention design is simple, and precursor preparation is easy, and the cobalt-that step carbonization is prepared is nitrogen co-doped multiple Close nano-carbon material.
(2) the nitrogen co-doped composite Nano carbon material catalytic performance of cobalt-that the present invention is prepared is excellent, cyclical stability It is good；It is relatively cheap as Nonmetal catalyst materials, before the application of Proton Exchange Membrane Fuel Cells energy storage material above has well Scape.
Detailed description of the invention
Fig. 1 is a variety of multiple SEM figure of Co@CNT-800-2 material in embodiment 1；
Fig. 2 is a variety of multiple SEM figure of Co@CNT-800-0 material in comparative example 1；
Fig. 3 is a variety of multiple SEM figure of Co@CNT-800-1 material in comparative example 2；
Fig. 4 is a variety of multiple SEM figure of Co@CNT-800-3 material in comparative example 2；
Fig. 5 is that embodiment 1 and comparative example 1, comparative example 2 and comparative example 3 are recycled with the LSV under the sweep speed of 10mV/s Figure；
Fig. 6 is Co@CNT-800-2 material methanol tolerance stability test curve in embodiment 1；
Fig. 7 is the TEM figure of Co@CNT-800-2 material in embodiment 1.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Range.
Embodiment 1
It is nitrogen co-doped compound that cobalt-is made by using a step solvent-thermal method in a kind of nitrogen co-doped composite Nano carbon material of cobalt- It is transferred under inert atmosphere to heat up be carbonized after nano material presoma and be made.
The nitrogen co-doped composite Nano carbon material of the cobalt-the preparation method comprises the following steps:
(1) by 6mmol melamine, tetra- acetate hydrate cobalt of 0.3mmol and 9mmol terephthalaldehyde are dissolved separately in It is transferred in reaction kettle in 30mL, 20mL, 10mL DMF and after stirring, carries out solvent thermal reaction under the conditions of 150 DEG C, overnight, Sample filtering is taken out, is centrifuged under the conditions of 6000rpm and dries in an oven, obtain uniformly mixed powder, 100ml is then added Acetone supersound washing 10min, then separates out slurry of solids with supercentrifuge and is washed with deionized, in triplicate.60℃ 8h is dried in vacuo to get the nitrogen co-doped composite nano materials presoma of cobalt-.
(2) 200mg cobalt-nitrogen co-doped composite nano materials presoma powder is poured into porcelain crucible, puts tube furnace into, Logical argon gas, heating is carbonized under an argon atmosphere, and heating rate is 2 DEG C/min, and the temperature of carbonization is 800 DEG C, soaking time For 2h, the nitrogen co-doped composite Nano carbon material of cobalt-is obtained, adopts and 10h is washed with deionized, 60 DEG C of dryings in vacuum drying oven 8h obtains the nitrogen co-doped composite Nano carbon material of cobalt-, is named as Co@CNT-800-2.
(3) with active material Co@CNT-800-2: dehydrated alcohol: Nafion (water content 5wt%)=5mg:350 μ L:95 μ L prepares slurry, and ultrasound 0.5h, is then coated on glass-carbon electrode (d=2mm) in ultrasonic machine, controls active material 0.296mg/ cm2。
(4) using silver chloride electrode as reference electrode, graphite rod is to electrode, and electrolyte selects the potassium hydroxide of 0.1mol/L molten Liquid tests its chemical property with Shanghai Chen Hua electrochemical workstation.
Fig. 1 shows: finding out that Co@CNT-800-2 is carbon nanotubular from SEM figure, is respectively 10k, 50k times magnification from a to b Number.
Fig. 5 shows that Co@CNT-800-2 has excellent hydrogen reduction catalytic performance, and half wave potential is suitable with Pt/C, shows this The catalytic performance of kind oxygen reduction catalyst material is excellent.
Fig. 6 shows: curve is stablized, and illustrates that the Co@CNT-800-2 in embodiment 1 has good methanol tolerance stability.
Fig. 7 shows: Co@CNT-800-2 is carbon nanotube.
Comparative example 1
It is prepared according to the preparation method of embodiment 1, unlike, the melamine rubs with four acetate hydrate cobalts You are added without metal, the product being prepared is named as Co@CNT-800-0 than being 1:0.
Fig. 2 shows: the Co@CNT-800-0 in comparative example 1, finds out that Co@CNT-800-0 is carbon nanosheet shape from SEM figure, It is respectively 10k, 50k amplification factor from a to b.
Comparative example 2
It is prepared according to the preparation method of embodiment 1, unlike, the melamine rubs with four acetate hydrate cobalts You are than for 40:1, the product being prepared simultaneously is named as Co@CNT-800-1 after carbonization.
Fig. 3 shows: the Co@CNT-800-1 in comparative example 2, finds out that Co@CNT-800-1 catalyst is carbon nanometer from SEM figure Tubulose is respectively 10k, 50k amplification factor from a to b.
Comparative example 3
It is prepared according to the preparation method of embodiment 1, unlike, the melamine rubs with four acetate hydrate cobalts You are than for 10:1, the product being prepared simultaneously is named as Co@CNT-800-3 after carbonization.
Fig. 4 shows: the Co@CNT-800-3 in comparative example 1, finds out that Co@CNT-800-3 catalyst is carbon nanometer from SEM figure Tubulose is respectively 10k, 50k amplification factor from a to b.

Claims (10)

1. a kind of nitrogen co-doped composite Nano carbon material of cobalt-, which is characterized in that cobalt-nitrogen is made using a step solvent-thermal method and is co-doped with It is transferred under inert atmosphere to heat up be carbonized after miscellaneous composite nano materials presoma and be made.
2. the nitrogen co-doped composite Nano carbon material of cobalt-as described in claim 1, which is characterized in that the cobalt-is nitrogen co-doped Composite nano materials presoma is to be made by melamine, four acetate hydrate cobalts and terephthalaldehyde by solvent-thermal method.
3. the preparation method of the nitrogen co-doped composite Nano carbon material of cobalt-of any of claims 1 or 2, which is characterized in that including with Lower step:
(1) melamine, Cobalt salts and terephthalaldehyde are dissolved separately in solvent, carry out solvent thermal reaction, filtered, from The heart is simultaneously dried to obtain powder, and acetone or alcohol is added and mixes, is centrifugated out slurry of solids, washs, and vacuum drying obtains cobalt- Nitrogen co-doped composite nano materials presoma；
(2) the nitrogen co-doped composite nano materials presoma of cobalt-obtained is placed in heating under inert atmosphere to be carbonized, last water It washes, be dried in vacuo, obtain the nitrogen co-doped composite Nano carbon material of cobalt-.
4. the preparation method of the nitrogen co-doped composite Nano carbon material of cobalt-as claimed in claim 3, which is characterized in that the step Suddenly the molar ratio of the melamine in (1), Cobalt salts and terephthalaldehyde is 20:1:30.
5. the preparation method of the nitrogen co-doped composite Nano carbon material of cobalt-as claimed in claim 3, which is characterized in that the step Suddenly the Cobalt salts in (1) are four acetate hydrate cobalts, and solvent DMF, reaction temperature is 150-200 DEG C.
6. the preparation method of the nitrogen co-doped composite Nano carbon material of cobalt-as claimed in claim 3, which is characterized in that the step Suddenly the inert atmosphere in (2) is argon atmosphere.
7. the preparation method of the nitrogen co-doped composite Nano carbon material of cobalt-as claimed in claim 3, which is characterized in that the step Suddenly the technological parameter of the carbonization in (2) are as follows: 2-5 DEG C of heating rate/min, 700-900 DEG C of carburizing temperature, soaking time 1-5h.
8. the preparation method of the nitrogen co-doped composite Nano carbon material of cobalt-as claimed in claim 3, which is characterized in that the step Suddenly 6~12h is washed with deionized to adopt in (2) washing, and the vacuum drying in the step (1) and (2) is in vacuum drying oven 60-100 DEG C of dry 6-18h.
9. a kind of non noble metal oxygen reduction catalyst, which is characterized in that nitrogen co-doped multiple containing cobalt-of any of claims 1 or 2 Close nano-carbon material.
10. non noble metal oxygen reduction catalyst as claimed in claim 9 is in the energy storage material for preparing Proton Exchange Membrane Fuel Cells In application.
CN201810926950.5A 2018-08-15 2018-08-15 A kind of nitrogen co-doped composite Nano carbon material of cobalt-and its preparation method and application Pending CN109192998A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112331869A (en) * 2020-11-06 2021-02-05 五邑大学 Cobalt-nitrogen double-doped hybrid carbon material and preparation method thereof
CN112723341A (en) * 2020-12-15 2021-04-30 南京工业大学 Diatom doped carbon nanotube and preparation method and application thereof

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Publication number Priority date Publication date Assignee Title
CN103007976A (en) * 2012-12-11 2013-04-03 湖南科技大学 Doped polyaniline directly-carbonized composite electrocatalyst, preparation method and application
CN104953135A (en) * 2015-04-30 2015-09-30 北京化工大学 N-doped carbon nano tube loaded cobalt-based electro-catalytic material and preparation method thereof
CN105413730A (en) * 2015-11-25 2016-03-23 青岛大学 Preparation method of cobalt electro-catalysis oxygen reduction material wrapping nitrogen-doped carbon nanotube
CN106669758A (en) * 2016-12-26 2017-05-17 华东理工大学 Dual-function oxygen electrode catalyst containing non-noble-metal nanoparticles coated with nitrogen-doped porous carbon layer and preparation method of dual-function oxygen electrode catalyst
CN106887620A (en) * 2015-12-15 2017-06-23 中国科学院上海高等研究院 Cobalt nitrogen-doped carbon Nanorods Catalyst and preparation method and application

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103007976A (en) * 2012-12-11 2013-04-03 湖南科技大学 Doped polyaniline directly-carbonized composite electrocatalyst, preparation method and application
CN104953135A (en) * 2015-04-30 2015-09-30 北京化工大学 N-doped carbon nano tube loaded cobalt-based electro-catalytic material and preparation method thereof
CN105413730A (en) * 2015-11-25 2016-03-23 青岛大学 Preparation method of cobalt electro-catalysis oxygen reduction material wrapping nitrogen-doped carbon nanotube
CN106887620A (en) * 2015-12-15 2017-06-23 中国科学院上海高等研究院 Cobalt nitrogen-doped carbon Nanorods Catalyst and preparation method and application
CN106669758A (en) * 2016-12-26 2017-05-17 华东理工大学 Dual-function oxygen electrode catalyst containing non-noble-metal nanoparticles coated with nitrogen-doped porous carbon layer and preparation method of dual-function oxygen electrode catalyst

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112331869A (en) * 2020-11-06 2021-02-05 五邑大学 Cobalt-nitrogen double-doped hybrid carbon material and preparation method thereof
CN112723341A (en) * 2020-12-15 2021-04-30 南京工业大学 Diatom doped carbon nanotube and preparation method and application thereof
CN112723341B (en) * 2020-12-15 2024-02-27 南京工业大学 Diatomic doped carbon nano tube and preparation method and application thereof

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