CN109920652A - A kind of preparation method of nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material - Google Patents
A kind of preparation method of nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material Download PDFInfo
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- CN109920652A CN109920652A CN201811411514.0A CN201811411514A CN109920652A CN 109920652 A CN109920652 A CN 109920652A CN 201811411514 A CN201811411514 A CN 201811411514A CN 109920652 A CN109920652 A CN 109920652A
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Abstract
The present invention relates to a kind of nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material preparation methods, comprising: (1) preparation of zinc-base metal-organic framework materials；(2) N the preparation of self-supporting presoma: is added in ZIF-8 and polyacrylonitrile (PAN), in dinethylformamide (DMF), it is heated with stirring to form uniform precursor pulp, precursor pulp is taken to cover carbon cloth surfaces, then solvent evaporated DMF, self-supporting presoma is obtained, ZIF-8@PAN/CC is named as；(3) nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material preparation: ZIF-8@PAN/CC presoma is placed in tube furnace; under argon atmosphere protection; it is warming up to 600-900 DEG C of certain temperature and is taken out after keeping the temperature a period of time; it is dry after pickling, obtain nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material.
Description
Technical field
The invention belongs to the technology of preparing of nano material and application fields, are specifically related to a kind of nitrogen oxygen doping porous carbon/carbon
The preparation method of cloth self-supporting electrode material.
Background technique
Under the background for the environmental pollution that fossil energy is petered out and is increasingly aggravated, people are dedicated to developing Novel ring
Protect efficient energy device.Supercapacitor is due to its power density height, long service life and advantages of environment protection, rapidly
There is widely applied new type of energy storage device as one kind.Electrode material has conclusive work for the performance of supercapacitor
With.Traditional electrode preparation is because electrode active material is powder, so generally use slurry coated technique, i.e., by active material with
Conductive agent and binder are uniformly mixed into slurry by a certain percentage, then coated in metal collector.Since binder is height
Molecule megohmite insulant, its addition not only reduce the electric conductivity and stability of material, while having also taken up certain space, reduce
The energy density of device.Therefore need to develop the active electrode material of self-supporting a kind of, avoid complicated slurry coated technique with
And the use of insulating adhesive.
Meanwhile active carbon material is the current most common electrode of super capacitor active material, the circulation having had is steady
The advantages that qualitative and excellent electric conductivity, but absorbent charcoal material used at present is because of its relatively low specific capacity, and lead to device
The energy density of part is lower.Largely studies have shown that (such as by the rationally pore-size distribution of adjusting carbon material and heterogeneous element
Nitrogen, oxygen, phosphorus, sulphur etc.) doping, can effectively improve material specific capacity and improve its high rate performance.
Based on background above, this invention address that developing a kind of nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material
Preparation method, with expect can provide some new approach and break-through point for the development of supercapacitor.
Summary of the invention
The present invention provides one kind using polyacrylonitrile and zinc-base metal-organic framework materials as presoma, by carbon cloth
Drop is covered and high temperature pyrolysis, can obtain nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material.This method is simple and easy, is suitble to
Large-scale production.The purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material, including the following steps:
(1) preparation of zinc-base metal-organic framework materials: zinc nitrate and methylimidazole are dissolved in methanol, then are centrifuged
It is dry, required zinc-base metal-organic framework materials are obtained, ZIF-8 is named as；
(2) ZIF-8 of step (1) preparation and polyacrylonitrile (PAN) preparation of self-supporting presoma: are pressed into certain mass ratio
It is added in n,N-Dimethylformamide (DMF), is heated with stirring to form uniform precursor pulp, precursor pulp is taken to cover
Carbon cloth surfaces, then solvent evaporated DMF, obtains self-supporting presoma, is named as ZIF-8@PAN/CC；
(3) nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material preparation: ZIF-8@PAN/ prepared by step (2)
CC presoma is placed in tube furnace, under argon atmosphere protection, after being warming up to 600-900 DEG C of certain temperature and keeping the temperature a period of time
It takes out, it is dry after pickling, obtain nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material.
Preferably, in (1), zinc nitrate and methylimidazole are dissolved in methanol according to the quality proportioning of 1:2-2.5.
(2) in, the ZIF-8 and polyacrylonitrile (PAN) of preparation and the mass ratio of DMF are 1:0.5-3:2-10.
The invention successfully prepares nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material.Compared with prior art, originally
Invention operating method is simple, facilitates large-scale production.Pass through the doping of nitrogen oxygen dual element and the regulation of porous structure, Ke Yiti
The specific capacity of high-activity carbon material, while accelerating mass transport process.And this method avoid insulating adhesives in traditional electrode
It uses, promotes giving full play to for active material performance.
Detailed description of the invention
Fig. 1 is NO-PC/CC scanned photograph prepared by the embodiment of the present invention 1；Nitrogen oxygen doping porous carbon can be observed by figure
It is coated in carbon cloth, ensure that the stability of material, while also improving the transfer velocity of electronics.
Fig. 2 is that NO-PC/CC prepared by the embodiment of the present invention 1 transmits photo；Obtained carbon material as we can see from the figure
With porous structure.
Fig. 3 is the XPS elemental analysis map of NO-PC/CC prepared by the embodiment of the present invention 1；Nitrogen as we know from the figure, oxygen,
The presence of three kinds of elements of carbon, it was demonstrated that nitrogen, the doping of oxygen element.
Specific embodiment
The specific embodiment of preparation method of the present invention is given below.Preparation that these embodiments are only used for that the present invention will be described in detail
Method is not intended to limit the protection scope of the claim of this application.
Embodiment 1
(1) preparation of zinc-base metal-organic framework materials: by certain density zinc nitrate methanol solution (2.9g, 200mL)
It is added in methylimidazole methanol solution (6.5g, 200mL), persistently stirs 1h, be then centrifuged for drying, obtain required zinc-base metal
Organic framework material (is named as ZIF-8).
(2) ZIF-8 of step (1) preparation and polyacrylonitrile (PAN) preparation of self-supporting presoma: are pressed into certain mass ratio
It is added in n,N-Dimethylformamide (DMF), is heated with stirring to form uniform precursor pulp at 85 DEG C.Wherein three
Mass ratio is (1:1:3).It takes 0.1mL slurry uniformly to drip and is layed onto 1cm2Carbon cloth surfaces, then solvent evaporated DMF, available
Self-supporting presoma.(being named as ZIF-8@PAN/CC).
(3) nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material preparation: ZIF-8@PAN/ prepared by step (2)
CC presoma is placed in tube furnace, under argon atmosphere protection, is warming up to 800 DEG C and is taken out after keeping the temperature 2h, dry after pickling,
Obtain nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material (being named as NO-PC/CC).
Embodiment 2
(1) preparation of zinc-base metal-organic framework materials: by certain density zinc nitrate methanol solution (2.9g, 200mL)
It is added in methylimidazole methanol solution (6.5g, 200mL), persistently stirs 1h, be then centrifuged for drying, obtain required zinc-base metal
Organic framework material (is named as ZIF-8).
(2) ZIF-8 of step (1) preparation and polyacrylonitrile (PAN) preparation of self-supporting presoma: are pressed into certain mass ratio
It is added in n,N-Dimethylformamide (DMF), is heated with stirring to form uniform precursor pulp at 85 DEG C.Wherein three
Mass ratio is (1:0.5:3).It takes 0.1mL slurry uniformly to drip and is layed onto 1cm2Carbon cloth surfaces, then solvent evaporated DMF, can obtain
To self-supporting presoma.(being named as ZIF-8@PAN/CC).
(3) nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material preparation: ZIF-8@PAN/ prepared by step (2)
CC presoma is placed in tube furnace, under argon atmosphere protection, is warming up to 800 DEG C and is taken out after keeping the temperature 2h, dry after pickling,
Obtain nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material (being named as NO-PC/CC).
Embodiment 3
(1) preparation of zinc-base metal-organic framework materials: by certain density zinc nitrate methanol solution (2.9g, 200mL)
It is added in methylimidazole methanol solution (6.5g, 200mL), persistently stirs 1h, be then centrifuged for drying, obtain required zinc-base metal
Organic framework material (is named as ZIF-8).
(2) ZIF-8 of step (1) preparation and polyacrylonitrile (PAN) preparation of self-supporting presoma: are pressed into certain mass ratio
It is added in n,N-Dimethylformamide (DMF), is heated with stirring to form uniform precursor pulp at 85 DEG C.Wherein three
Mass ratio is (1:1:10).It takes 0.1mL slurry uniformly to drip and is layed onto 1cm2Carbon cloth surfaces, then solvent evaporated DMF, available
Self-supporting presoma.(being named as ZIF-8@PAN/CC).
(3) nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material preparation: ZIF-8@PAN/ prepared by step (2)
CC presoma is placed in tube furnace, under argon atmosphere protection, is warming up to 800 DEG C and is taken out after keeping the temperature 2h, dry after pickling,
Obtain nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material (being named as NO-PC/CC).
Embodiment 4
(1) preparation of zinc-base metal-organic framework materials: by certain density zinc nitrate methanol solution (2.9g, 200mL)
It is added in methylimidazole methanol solution (6.5g, 200mL), persistently stirs 1h, be then centrifuged for drying, obtain required zinc-base metal
Organic framework material (is named as ZIF-8).
(2) ZIF-8 of step (1) preparation and polyacrylonitrile (PAN) preparation of self-supporting presoma: are pressed into certain mass ratio
It is added in n,N-Dimethylformamide (DMF), is heated with stirring to form uniform precursor pulp at 85 DEG C.Wherein three
Mass ratio is (1:1:3).It takes 0.1mL slurry uniformly to drip and is layed onto 1cm2Carbon cloth surfaces, then solvent evaporated DMF, available
Self-supporting presoma.(being named as ZIF-8@PAN/CC).
(3) nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material preparation: ZIF-8@PAN/ prepared by step (2)
CC presoma is placed in tube furnace, under argon atmosphere protection, is warming up to 900 DEG C and is taken out after keeping the temperature 2h, dry after pickling,
Obtain nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material (being named as NO-PC/CC).
Claims (3)
1. a kind of nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material preparation method, including the following steps:
(1) preparation of zinc-base metal-organic framework materials: zinc nitrate and methylimidazole are dissolved in methanol, then are centrifuged dry
It is dry, required zinc-base metal-organic framework materials are obtained, ZIF-8 is named as；
(2) preparation of self-supporting presoma: by the ZIF-8 of step (1) preparation and polyacrylonitrile (PAN) by certain mass than being added
In n,N-Dimethylformamide (DMF), it is heated with stirring to form uniform precursor pulp, precursor pulp is taken to cover carbon cloth
Surface, then solvent evaporated DMF, obtains self-supporting presoma, is named as ZIF-8@PAN/CC；
(3) nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material preparation: before the ZIF-8@PAN/CC of step (2) preparation
It drives body to be placed in tube furnace, under argon atmosphere protection, is warming up to 600-900 DEG C of certain temperature and is taken after keeping the temperature a period of time
Out, dry after pickling, obtain nitrogen oxygen doping porous carbon/carbon cloth self-supporting electrode material.
2. preparation method according to claim 1, which is characterized in that (1) in, by zinc nitrate and methylimidazole according to 1:
The quality proportioning of 2-2.5 is dissolved in methanol.
3. preparation method according to claim 1, which is characterized in that (2) in, the ZIF-8 of preparation and polyacrylonitrile (PAN) and
The mass ratio of DMF is 1:0.5-3:2-10.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105862174A (en) * | 2016-04-08 | 2016-08-17 | 合肥工业大学 | Preparation method of novel metal organic complex fibers and derivative porous carbon fibers thereof |
| CN108878158A (en) * | 2017-05-16 | 2018-11-23 | 中国科学院福建物质结构研究所 | A kind of preparation method and purposes of C-base composte material |
-
2018
- 2018-11-24 CN CN201811411514.0A patent/CN109920652A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105862174A (en) * | 2016-04-08 | 2016-08-17 | 合肥工业大学 | Preparation method of novel metal organic complex fibers and derivative porous carbon fibers thereof |
| CN108878158A (en) * | 2017-05-16 | 2018-11-23 | 中国科学院福建物质结构研究所 | A kind of preparation method and purposes of C-base composte material |
Non-Patent Citations (2)
| Title |
|---|
| ZHENHUA LI,ET AL.: ""Electrosynthesis of Well-Defined Metal–Organic Framework Films and the Carbon Nanotube Network Derived from Them toward Electrocatalytic Applications"", 《ACS APPL. MATER. INTERFACES》 * |
| ZUXING MAO,ET AL.: ""Facile synthesis of nitrogen-doped porous carbon as robust electrode for supercapacitors"", 《MATERIALS RESEARCH BULLETIN》 * |
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