CN106972180A - One-step calcination method synthesizes the hollow chain form nitrogen-doped carbon nanometer pipe encapsulation difunctional oxygen reduction catalyst of cementite - Google Patents
One-step calcination method synthesizes the hollow chain form nitrogen-doped carbon nanometer pipe encapsulation difunctional oxygen reduction catalyst of cementite Download PDFInfo
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- CN106972180A CN106972180A CN201710249578.4A CN201710249578A CN106972180A CN 106972180 A CN106972180 A CN 106972180A CN 201710249578 A CN201710249578 A CN 201710249578A CN 106972180 A CN106972180 A CN 106972180A
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- cementite
- doped carbon
- carbon nanometer
- oxygen reduction
- nanometer pipe
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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
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Catalysts (AREA)
Abstract
It is an object of the invention to provide the hollow chain form nitrogen-doped carbon nanometer pipe encapsulation difunctional oxygen reduction catalyst preparation method of cementite of one kind synthesis, this method can be synthesized by using cheap raw material using shirtsleeve operation method.The hollow chain form nitrogen-doped carbon nanometer pipe encapsulation difunctional oxygen reduction catalyst of cementite proposed by the present invention is by made from high-temperature calcination.Cementite and the unique structural property of nitrogen-doped carbon nanometer pipe are effectively combined by it, successfully cementite nanometer atom is encapsulated in hollow chain form nitrogen-doped carbon nanometer pipe, the advantage of the two is taken full advantage of, the oxygen reduction catalytic activity of composite catalyst is improved by collective effect.Compared with prior art, the present invention has advantages below：Preparation method is simple, and product yield is high, environment-friendly, it is easy to accomplish production in enormous quantities etc. all makes the present invention have extremely wide application prospect.
Description
Technical field
The present invention relates to synthesize the hollow chain form nitrogen-doped carbon nanometer pipe encapsulation difunctional oxygen reduction catalyst of cementite
Preparation method.
Background technology
Proton Exchange Membrane Fuel Cells is as future source of energy application conversion equipment in sustainable energy and new energy technology
Attracted attention in research and development.It is equivalent to the power plant of an automatic running, and it can pass through chemical reaction
Mode realize effective conversion between chemical energy and electric energy.Compared with conventional batteries, Proton Exchange Membrane Fuel Cells possesses one
The characteristics of a little conventional batteries can not reach, such as：High conversion efficiency, energy density are high, the interval big, specific power of operation temperature and compare energy
Amount is high, fast response time the advantages of, therefore obtained the extensive favor Proton Exchange Membrane Fuel Cells of researcher and why can
Produce so high conversion efficiency key link and be cathodic oxygen reduction catalyst.At present, glass carbon is pem fuel electricity
Business cathod catalyst in pond, but be due to many reasons influence so that its commercialized development receives serious obstruction,
Such as cost is high, dynamics is delayed, easily poison.In order to solve these restriction problems, how research reduces catalyst cost, develops
High catalytic activity and the strong novel cathode catalyst of anti-poisoning capability just turn into the key that Proton Exchange Membrane Fuel Cells develops.
In recent years, the N doping iron base composite material that carbon is modified makees some existing relevant reports of cathodic oxygen reduction catalyst,
But these method building-up processes are complicated, cost is high, and material property is still not ideal enough.Therefore, a kind of preparation simple and easy to apply is selected
Method, the N doping iron-based cathod catalyst tool for preparing high performance carbon modification is of great significance.
The content of the invention
It is an object of the invention to provide the hollow chain form nitrogen-doped carbon nanometer pipe encapsulation cementite hydrogen reduction of one kind synthesis
By using cheap raw material, using shirtsleeve operation method, through high-temperature calcination chemistry occurs for method for preparing catalyst, this method
Reaction can synthesize hollow chain form nitrogen-doped carbon nanometer pipe encapsulation cementite oxygen reduction catalyst.Nitrogen proposed by the present invention is mixed
Miscellaneous carbon nanotube encapsulation cementite electrocatalysis material is by made from high-temperature calcination.It is by cementite and nitrogen-doped carbon nanometer pipe
Unique structural property is effectively combined, and successfully cementite nanometer atom is encapsulated in nitrogen-doped carbon nanometer pipe, filled
Divide and make use of the advantage of the two, the oxygen reduction catalytic activity of composite catalyst is improved by collective effect.
Compared with prior art, the present invention has advantages below：Based on high-temperature calcination, using original cheap and easy to get
Material, hollow chain form nitrogen-doped carbon nanometer pipe encapsulation cementite oxygen reduction catalyst is can obtain by simply preparing.Preparation side
Method is simple, and product yield is high, environment-friendly, it is easy to accomplish all make the features such as production in enormous quantities the present invention have it is extremely wide should
Use prospect.
Brief description of the drawings
Fig. 1 is the X-ray powder diffraction figure that first embodiment of the invention prepares sample；
Fig. 2 is hollow chain form nitrogen-doped carbon nanometer pipe encapsulation cementite oxygen reduction catalyst prepared by first embodiment of the invention
Scanning electron microscope diagram；
Embodiment
With reference to specific embodiment, the present invention is further elaborated.These embodiments are interpreted as being merely to illustrate this hair
It is bright rather than limit the scope of the invention.After the content of the invention recorded has been read, the principle based on the present invention
The various changes or modification made to the present invention equally fall into claims of the present invention limited range.
Implement a preparation method：
By 1.08 g iron chloride, 0.02 g polyvinylpyrrolidones and 1 g melamines are dissolved among 50 mL ethanol,
The above-mentioned solution 1h of mechanical agitation becomes uniform dispersion liquid after ultrasound, and solvent is evaporated into complete with Rotary Evaporators, obtained
Dried powder 800 DEG C of high-temperature calcination 2h under nitrogen protective condition, are cooled to room temperature standby.Then with 6 M salt acid dip 24
H, respectively with drying in 60 DEG C of baking ovens is placed in after ethanol and distillation water washing, obtains final product.Control sample is also by same
Method is made, but does not add polyvinylpyrrolidone.
Claims (5)
1. a kind of method that nitrogen-doped carbon nanometer pipe encapsulates the difunctional oxygen reduction catalyst of cementite, using iron chloride as source of iron, three
Poly cyanamid is carbon source, and polyvinylpyrrolidone is dispersant, and three is dissolved among 50 mL ethanol, mechanical agitation after ultrasound
Above-mentioned solution 1h becomes uniform dispersion liquid.
2. solvent is evaporated complete by the dispersion liquid Rotary Evaporators that the claims 1 are obtained, dried powder is obtained in nitrogen
800 DEG C of high-temperature calcination 2h, are cooled to room temperature standby under the conditions of gas shielded.
3. 6 M of the black powder that the claims 2 the are obtained h of salt acid dip 24, respectively with ethanol and distillation water washing
After be placed in 60 DEG C of baking ovens dry.
4. as described in the claims 3, by carrying out electro-chemical test to obtained electrocatalysis material, to its hydrogen reduction
It can be evaluated.
5. composite catalyst has the characteristics that：
（1）When rotating speed reaches 1600 turns, limiting current density reaches 6.2 mAcm-2, take-off potential is -0.076 V；
（2）Specific surface area is about 206 m2g-1。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710249578.4A CN106972180A (en) | 2017-04-17 | 2017-04-17 | One-step calcination method synthesizes the hollow chain form nitrogen-doped carbon nanometer pipe encapsulation difunctional oxygen reduction catalyst of cementite |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710249578.4A CN106972180A (en) | 2017-04-17 | 2017-04-17 | One-step calcination method synthesizes the hollow chain form nitrogen-doped carbon nanometer pipe encapsulation difunctional oxygen reduction catalyst of cementite |
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| CN106972180A true CN106972180A (en) | 2017-07-21 |
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| CN201710249578.4A Pending CN106972180A (en) | 2017-04-17 | 2017-04-17 | One-step calcination method synthesizes the hollow chain form nitrogen-doped carbon nanometer pipe encapsulation difunctional oxygen reduction catalyst of cementite |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112259751A (en) * | 2020-10-27 | 2021-01-22 | 广东工业大学 | ORR and OER bifunctional catalyst, and preparation method and application thereof |
| CN113231107A (en) * | 2021-04-29 | 2021-08-10 | 陕西科技大学 | Carbon nanotube-coated vanadium nitride/iron carbide composite electrocatalyst and preparation method and application thereof |
| CN114887644A (en) * | 2022-05-27 | 2022-08-12 | 济宁学院 | Nitrogen-doped iron carbide/carbon nanoenzyme and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1585725A (en) * | 2002-03-15 | 2005-02-23 | 大阪瓦斯株式会社 | Iron/carbon composite, carbonaceous material comprising the iron/carbon composite, and process for producing the same |
| CN105271229A (en) * | 2015-10-10 | 2016-01-27 | 华南理工大学 | Method for in-situ preparation of iron carbide filled doped carbon nanotube |
| CN105540590A (en) * | 2015-12-17 | 2016-05-04 | 中北大学 | Preparation method of Fe3C nanowire filled and nitrogen doped carbon nanotube composite with high specific surface area |
-
2017
- 2017-04-17 CN CN201710249578.4A patent/CN106972180A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1585725A (en) * | 2002-03-15 | 2005-02-23 | 大阪瓦斯株式会社 | Iron/carbon composite, carbonaceous material comprising the iron/carbon composite, and process for producing the same |
| CN105271229A (en) * | 2015-10-10 | 2016-01-27 | 华南理工大学 | Method for in-situ preparation of iron carbide filled doped carbon nanotube |
| CN105540590A (en) * | 2015-12-17 | 2016-05-04 | 中北大学 | Preparation method of Fe3C nanowire filled and nitrogen doped carbon nanotube composite with high specific surface area |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112259751A (en) * | 2020-10-27 | 2021-01-22 | 广东工业大学 | ORR and OER bifunctional catalyst, and preparation method and application thereof |
| CN112259751B (en) * | 2020-10-27 | 2022-06-14 | 广东工业大学 | ORR and OER bifunctional catalyst, and preparation method and application thereof |
| CN113231107A (en) * | 2021-04-29 | 2021-08-10 | 陕西科技大学 | Carbon nanotube-coated vanadium nitride/iron carbide composite electrocatalyst and preparation method and application thereof |
| CN114887644A (en) * | 2022-05-27 | 2022-08-12 | 济宁学院 | Nitrogen-doped iron carbide/carbon nanoenzyme and preparation method and application thereof |
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Application publication date: 20170721 |