CN107331844A - A kind of preparation method of the porous nitrogen-doped graphene nanometer sheet of network - Google Patents
A kind of preparation method of the porous nitrogen-doped graphene nanometer sheet of network Download PDFInfo
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- CN107331844A CN107331844A CN201710529298.9A CN201710529298A CN107331844A CN 107331844 A CN107331844 A CN 107331844A CN 201710529298 A CN201710529298 A CN 201710529298A CN 107331844 A CN107331844 A CN 107331844A
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
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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
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- 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 invention discloses a kind of preparation method of the porous nitrogen-doped graphene nanometer sheet of network.The present invention is mixed by itrogenous organic substance and water soluble salt template, and high-temperature gradient calcining prepares the porous nitrogen-doped graphene nanometer sheet of network under direct inert atmosphere.The porous nitrogen-doped graphene nanometer sheet of network of preparation is as sodium/potassium cell negative electrode material, with excellent performance.
Description
Technical field
The present invention relates to a kind of preparation method of the porous nitrogen-doped graphene nanometer sheet of network.
Background technology
Graphene is the nano material of the lattice structure for the regular hexagon extension that a class carbon atom is constituted, due to its property
Energy is excellent and with a variety of potential applications.Receive the extensive concern of people.However, easily layer-layer again between two-dimensional graphene
The special property for making it lose two-dimensional nanostructure is overlapped mutually, therefore, folding between graphene molecules layer-layer how is prevented
Plus, it is remained unchanged in macro-scale and keep its graphene characteristic to turn into the key issue that scientific research needs are solved.
Therefore, constructed, worked as so as to keep the two-dimensional characteristics of graphene to turn into macro-scale by three-dimensional network graphene
Study hotspot (the Nat Mater, 2011,10 of modern field of nanometer material technology: 424; Adv Mater, 2012, 24: 5083;
CN201611191949.X;CN201611232796.9).Correlative study shows that heteroatom doping can change stone with N doping
Cloud density on black alkene molecule, thus with unique material property, the graphene of nitrogen atom doping is due to graphene point
Polarity in sub between C-N keys, causes nitrogen-doped graphene catalytic oxidation-reduction performance to be better than graphene.Three-dimensional nitrogen-doped graphene
Preparation method is generally obtained by three-dimensional grapheme in ammonia atmosphere reduction(ACS Nano, 2013, 7(5): 4042), it is this
Method technique is cumbersome, while the use of ammonia has certain danger, thus a kind of simple scale of exploitation prepares network N doping
The method of graphene nanometer sheet is very necessary.
The content of the invention
In view of the above-mentioned problems of the prior art, the purpose of the present invention is to propose to a kind of porous nitrogen-doped graphene of network
The preparation method of nanometer sheet.
The present invention is mixed by itrogenous organic substance and water soluble salt template, and under direct inert atmosphere prepared by high-temperature gradient calcining
The porous nitrogen-doped graphene nanometer sheet of network.
A kind of preparation method of the porous nitrogen-doped graphene nanometer sheet of network, it is characterised in that by itrogenous organic substance and Ke Shui
Soluble template is mixed, and is then inserted gradient in atmosphere furnace and is calcined:1-10 DEG C of programming rate/min is first according to, is warming up to
300-500 DEG C, after insulation 0.5-2h, it is continuously heating to 600-1500 DEG C, 1-10 DEG C of programming rate/min, soaking time is
1-3 h, are down to after room temperature and take out;It is block into black after calcining, after crushing, 2-5 times 30-100 DEG C of material quality is added every time
Distilled water filtering and washing, 60-120 DEG C of constant temperature 12-24 h of filter residue is dried, the porous nitrogen-doped graphene nanometer sheet of network is obtained.
Itrogenous organic substance of the present invention is selected from triammonium citrate, ethylenediamine tetra-acetic acid or ethanedioic acid diethylamine.
Water soluble salt template is selected from sodium acid carbonate or saleratus.
Itrogenous organic substance and the mass ratio of water soluble salt template are 1:0.1-10.
Abundant raw materials of the present invention, cheap and easy to get, equipment requirement are simple, environment-friendly, product quality stable.Wherein pass through
High-temperature gradient is calcined under direct inert atmosphere after itrogenous organic substance and water soluble salt template are mixed, and passes through crushing, washing, drying
When the porous nitrogen-doped graphene nanometer sheet of network.
The porous nitrogen-doped graphene nanometer sheet of network of preparation is as sodium/potassium cell negative electrode material, with excellent performance.
The present invention is compared with other network-like graphene nano piece preparation methods, with advantages below:
1st, this method raw material is cheap and easy to get, and it is itrogenous organic substance and water soluble salt to prepare raw materials used, and the place of production is extensively and price
It is cheap;
2nd, this method is without high-vacuum apparatus, and equipment requirement is simple;
3rd, this method environment is relatively friendly, is not related to inflammable gas, produces contained most of for inorganic salts in waste water, it is easy to return
Receive, environmental pollution is small;
4th, prepared material is as sodium/potassium GND, with excellent performance, while can be widely used for energy storage, photocatalysis is high
The fields such as molecular stuffing.
Brief description of the drawings
Fig. 1 is the porous nitrogen-doped graphene nanometer sheet TEM photos of prepared network in embodiment 1.
Fig. 2 is the porous nitrogen-doped graphene nanometer sheet TEM photos of prepared network in embodiment 3.
Fig. 3 is the porous nitrogen-doped graphene nanometer sheet nitrogen content EDX spectrograms of prepared network in embodiment 1.
Fig. 4 is the prepared porous nitrogen-doped graphene nanometer sheet potassium ion half-cell test of network in embodiment 1.
Embodiment
Embodiment 1:
Weigh 10 g triammonium citrates and 30 g sodium acid carbonates ball milling mixings uniformly to add in porcelain boat afterwards, insert argon gas atmosphere stove
In, first, it is warming up to according to 5 DEG C/min of heating rate after 400 DEG C, 2 h of insulation, continuation is warming up to 800 according to 5 DEG C/min
DEG C, after 1 h of insulation, room temperature is down to naturally, takes out sample;After the block sample comminution of gained black, 50 DEG C of distilled water 80 are added
G carries out filtering and washing, is repeated 5 times, and 60 DEG C of 12 h of insulation of filter residue after washing are dried to obtain into the porous N doping of network
Graphene nanometer sheet.
Embodiment 2:
Weigh 10 g triammonium citrates and 100 g saleratus ball milling mixings uniformly to add in porcelain boat afterwards, insert argon gas atmosphere stove
In, first, it is warming up to according to 2 DEG C/min of heating rate after 500 DEG C, 0.5 h of insulation, continuation is warming up to according to 10 DEG C/min
1500 DEG C, it is incubated after 1 h, room temperature is down to naturally, takes out sample;After the block sample comminution of gained black, 100 DEG C of steamings are added
The g of distilled water 500 carries out filtering and washing, is repeated 3 times, and it is more that 80 DEG C of 24 h of insulation of filter residue after washing are dried to obtain into network
Hole nitrogen-doped graphene nanometer sheet.
Embodiment 3:
Weigh 10 g ethanedioic acids diethylamine and 5 g sodium acid carbonates mechanical mixtures uniformly to add in porcelain boat afterwards, insert nitrogen atmosphere stove
In, first, it is warming up to according to 10 DEG C/min of heating rate after 400 DEG C, 2 h of insulation, continuation is warming up to 800 according to 5 DEG C/min
DEG C, after 2 h of insulation, room temperature is down to naturally, takes out sample;After the block sample comminution of gained black, 80 DEG C of distilled water 45 are added
G carries out filtering and washing, is repeated 8 times, and 80 DEG C of 24 h of insulation of filter residue after washing are dried to obtain into the porous N doping of network
Graphene nanometer sheet.
Embodiment 4:
Weigh 10 g ethanedioic acids diethylamine and 10 g saleratus mechanical mixtures uniformly to add in porcelain boat afterwards, insert nitrogen atmosphere
In stove, first, it is warming up to according to 5 DEG C/min of heating rate after 300 DEG C, 1 h of insulation, continuation is warming up to according to 5 DEG C/min
900 DEG C, it is incubated after 1 h, room temperature is down to naturally, takes out sample;After the block sample comminution of gained black, 80 DEG C of distillations are added
The g of water 50 carries out filtering and washing, is repeated 5 times, and it is porous that 120 DEG C of 20 h of insulation of filter residue after washing are dried to obtain into network
Nitrogen-doped graphene nanometer sheet.
Embodiment 5:
Weigh 10 g ethylenediamine tetra-acetic acids and 40 g saleratus mechanical mixtures uniformly to add in porcelain boat afterwards, insert nitrogen atmosphere stove
In, first, it is warming up to according to 5 DEG C/min of heating rate after 500 DEG C, 1 h of insulation, continuation is warming up to 900 according to 5 DEG C/min
DEG C, after 1 h of insulation, room temperature is down to naturally, takes out sample;After the block sample comminution of gained black, 80 DEG C of distilled water 50 are added
G carries out filtering and washing, is repeated 5 times, and 80 DEG C of 20 h of insulation of filter residue after washing are dried to obtain into the porous N doping of network
Graphene nanometer sheet.
Embodiment 6:
Weigh 10 g ethylenediamine tetra-acetic acids and 20 g sodium acid carbonates mechanical mixtures uniformly to add in porcelain boat afterwards, insert nitrogen atmosphere stove
In, first, it is warming up to according to 5 DEG C/min of heating rate after 300 DEG C, 1.5 h of insulation, continuation is warming up to according to 5 DEG C/min
900 DEG C, it is incubated after 1 h, room temperature is down to naturally, takes out sample;After the block sample comminution of gained black, 80 DEG C of distillations are added
The g of water 50 carries out filtering and washing, is repeated 5 times, and 80 DEG C of 14 h of insulation of filter residue after washing are dried to obtain into the porous nitrogen of network
Doped graphene nanometer sheet.
Embodiment 7:
Weigh 10 g ethanedioic acids diethylamine and 50 g saleratus mechanical mixtures uniformly to add in porcelain boat afterwards, insert nitrogen atmosphere
In stove, first, it is warming up to according to 5 DEG C/min of heating rate after 300 DEG C, 1.5 h of insulation, continuation is warming up to according to 5 DEG C/min
900 DEG C, it is incubated after 1 h, room temperature is down to naturally, takes out sample;After the block sample comminution of gained black, 80 DEG C of distillations are added
The g of water 50 carries out filtering and washing, is repeated 5 times, and 80 DEG C of 14 h of insulation of filter residue after washing are dried to obtain into the porous nitrogen of network
Doped graphene nanometer sheet.
Embodiment 8:
Weigh 10 g triammonium citrates and 2 g saleratus mechanical mixtures uniformly to add in porcelain boat afterwards, insert nitrogen atmosphere stove
In, first, it is warming up to according to 5 DEG C/min of heating rate after 300 DEG C, 1.5 h of insulation, continuation is warming up to according to 5 DEG C/min
900 DEG C, it is incubated after 1 h, room temperature is down to naturally, takes out sample;After the block sample comminution of gained black, 80 DEG C of distillations are added
The g of water 30 carries out filtering and washing, is repeated 5 times, and 80 DEG C of 14 h of insulation of filter residue after washing are dried to obtain into the porous nitrogen of network
Doped graphene nanometer sheet.
Test example 1
Network-like graphene nanometer sheet obtained by each embodiment is assembled sodium ion by this test example as sodium ion battery electrode material
Half-cell:It is to electrode, 0.8 M KPF to select sodium piece6It is dissolved in EC/DMC (1:1 volume ratio) as electrolyte, in glove box
(Water content is less than 0.1 ppm, and oxygen content is less than 0.3 ppm)In carry out CR2032 half-cell assemblings after test.Test electric current close
Spend for 0.1A/g, shown in testing result table 1, the potassium electrical property of embodiment 1 is as shown in Figure 4.
The porous nitrogen-doped graphene nanometer sheet 0.1A g of network of each embodiment of table 1-1Potassium electrical property testing result
。
Claims (4)
1. a kind of preparation method of the porous nitrogen-doped graphene nanometer sheet of network, it is characterised in that by itrogenous organic substance with can be water-soluble
Property the mixing of salt template, then insert gradient in atmosphere furnace and calcine:1-10 DEG C of programming rate/min is first according to, 300- is warming up to
500 DEG C, it is incubated after 0.5-2h, is continuously heating to 600-1500 DEG C, 1-10 DEG C of programming rate/min, soaking time is 1-3
H, is down to after room temperature and takes out;It is block into black after calcining, after crushing, 2-5 times of 30-100 DEG C of distillation of material quality is added every time
Water filtering and washing, 60-120 DEG C of constant temperature 12-24 h of filter residue is dried, the porous nitrogen-doped graphene nanometer sheet of network is obtained.
2. the preparation method according to claim 1, it is characterised in that itrogenous organic substance is selected from triammonium citrate, ethylenediamine
Tetraacethyl or ethanedioic acid diethylamine.
3. the preparation method according to claim 1, it is characterised in that water soluble salt template is selected from sodium acid carbonate or carbonic acid
Hydrogen potassium
4. the preparation method according to claim 1 or 2 or 3, it is characterised in that itrogenous organic substance and water soluble salt template
Mass ratio be 1:0.1-10.
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Cited By (3)
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CN108232116A (en) * | 2017-12-15 | 2018-06-29 | 江苏大学 | A kind of preparation method of nitrogen, phosphor codoping Graphene gel electrochemistry storage sodium electrode |
CN108735991A (en) * | 2018-05-07 | 2018-11-02 | 北京科技大学 | A kind of kalium ion battery negative material and preparation method and electrolyte |
CN109286018A (en) * | 2018-12-06 | 2019-01-29 | 中国科学院兰州化学物理研究所 | A kind of preparation method of ultra-thin two-dimension carbon plate |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108232116A (en) * | 2017-12-15 | 2018-06-29 | 江苏大学 | A kind of preparation method of nitrogen, phosphor codoping Graphene gel electrochemistry storage sodium electrode |
CN108735991A (en) * | 2018-05-07 | 2018-11-02 | 北京科技大学 | A kind of kalium ion battery negative material and preparation method and electrolyte |
CN108735991B (en) * | 2018-05-07 | 2021-03-05 | 北京科技大学 | Negative electrode material for potassium ion battery, preparation method and electrolyte |
CN109286018A (en) * | 2018-12-06 | 2019-01-29 | 中国科学院兰州化学物理研究所 | A kind of preparation method of ultra-thin two-dimension carbon plate |
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