CN106784830A - A kind of preparation method and applications of the Pitch-based Carbon nanometer sheet for anode material of lithium-ion battery - Google Patents
A kind of preparation method and applications of the Pitch-based Carbon nanometer sheet for anode material of lithium-ion battery Download PDFInfo
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- 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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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
The present invention relates to carbon material preparing technical field, a kind of preparation method and applications of Pitch-based Carbon nanometer sheet for anode material of lithium-ion battery, wherein preparation method is comprised the following steps：(1) saturated aqueous sodium chloride is added dropwise in absolute ethyl alcohol; solvent evaporated is obtained sodium chloride template; (2) medium temperature coal pitch is dissolved in N-methyl pyrrolidones and adds sodium chloride template; heating is evaporated N-methyl pyrrolidones; carbonized under inert gas shielding; (3) sample after charing is cooled into room temperature to take out; adopt and be washed with deionized, be dried to obtain nanometer sheet; (4) nanometer sheet is carbonized under ammonia and argon gas mixed atmosphere; room temperature taking-up is cooled to, Pitch-based Carbon nanometer sheet is obtained.The inventive method is simple and easy to apply, and preparation process does not need pickling to go the removing template, sodium chloride template and N-methyl pyrrolidinone solvent can to recycle, and production cost is relatively low.In addition, Pitch-based Carbon nanometer sheet shows reversible storage sodium capacity higher, preferable high rate performance and excellent cycle performance as anode material of lithium-ion battery.
Description
Technical field
The present invention relates to a kind of Pitch-based Carbon nanometer sheet for anode material of lithium-ion battery preparation method and its should
With belonging to carbon material preparing technical field.
Background technology
Increasingly serious with energy crisis and environmental problem, society pushes away to nearly zero carbon emission based on energy internet
Extensively expect very much, this proposes requirements at the higher level to distributed energy storage technology.Meanwhile, New-energy electric vehicle, high ferro/city rail are handed over
The field electrochemical energy storing devices that also active demand high-energy-density, high power density are taken into account such as logical Brake energy recovery.Lithium from
Sub- battery has been widely used in domestic electronic appliances, portable has set because its energy density is high, the advantages of have extended cycle life
Standby and electric automobile.Yet with lithium resource is limited, lithium battery holds at high price, cause it in extensive energy storage system
With extremely limited.Sodium belongs to same main group with lithium, and chemical property is close, and reserves very abundant, the production of sodium-ion battery
Cost will be far below lithium ion battery, and exploitation sodium-ion battery is applied to extensive storage bodies as the substitute of lithium ion battery
It is reasonable.
Because the radius of sodium ion is larger, the charcoal base negative material predominantly carbon-coating spacing used in sodium-ion battery research
The relatively low hard carbon material of larger, degree of graphitization.Hard charcoal presoma is mainly biomass, high molecular polymer, resin etc., wherein
Asphaltic base hard carbon cathode material has Carbon yield high, suitable carbon-coating spacing and excellent electric conductivity, be expected to commercialization sodium from
It is used widely in sub- battery.
The microscopic appearance and structure of hard charcoal negative material can influence material and electrolyte contacts area, sodium ion diffusion path
Deng finally influenceing material electrochemical performance.Patent CN105098186A hard carbon presoma is mixed with soft carbon presoma after through hand over
After the treatment such as connection, solidification, charing, obtain unformed Carbon Materials and be applied to sodium-ion battery, but hard charcoal prepared by the method is born
Pole material is micron particles, and electrolyte and negative material contact not enough fully, influence the chemical property of negative material.Design
Constructing the hard carbon material of storage sodium activity high turns into the key of sodium-ion battery development.Wherein the hard charcoal with multi-stage artery structure is received
The advantages of rice piece has big with electrolyte contacts area, sodium ion transmission path is short, obtains researcher's extensive concern.Hetero atom is mixed
It is miscellaneous substantially to increase the reversible storage sodium active sites of material surface, help to lift the chemical property of material.Therefore, Heteroatom doping
Charcoal nanometer sheet be expected to be applied to high-performance sodium-ion battery.Traditional charcoal nanometer sheet is needed with metal oxide as template after charing
Pickling is wanted to remove removing template, preparation technology is complicated and easily pollutes environment, constrains its widespread adoption.The present invention goes out from coal tar pitch
Hair, using environment-friendly, easy-operating salt template, is prepared for a kind of with excellent storage sodium performance with reference to special charring process
Heteroatom doping hard charcoal nanometer sheet.
The content of the invention
In order to overcome the deficiencies in the prior art, sodium-ion battery negative pole material to be used for it is an object of the present invention to provide one kind
The preparation method and applications of the Pitch-based Carbon nanometer sheet of material.The present invention from coal tar pitch, using environment-friendly, easy-operating
Salt template, a kind of Heteroatom doping hard charcoal nanometer sheet with excellent storage sodium performance is prepared for reference to special charring process.Should
Method preparation process is simple, and raw material sources enrich, and prepared hard charcoal nanometer sheet has specific capacity as sodium-ion battery negative pole
The advantages of height, good rate capability and excellent cycle performance.
In order to realize foregoing invention purpose, solve the problems of in the prior art, the technical scheme that the present invention takes
It is：A kind of preparation method of Pitch-based Carbon nanometer sheet for anode material of lithium-ion battery, comprises the following steps：
Step 1, absolute ethyl alcohol is placed in reactor first, then saturated aqueous sodium chloride is added dropwise over absolute ethyl alcohol
In, solvent evaporated is obtained sodium chloride template, temperature control at 90-120 DEG C, the saturated aqueous sodium chloride and absolute ethyl alcohol body
Product is than being 1:1-10；
Step 2, medium temperature coal pitch is dissolved in N-methyl pyrrolidones it is placed in oil bath, then is added thereto to by step 1
Obtained sodium chloride template, after being well mixed, heating is evaporated N-methyl pyrrolidones, and temperature control, then will be upper at 200-210 DEG C
Stating during mixture delivers tube furnace under inert gas shielding carries out charing process, and temperature is with 2~10 DEG C/min heating rate liters
To 650~850 DEG C, in 1~3h, the inert gas is selected from the one kind in nitrogen or argon gas, middle temperature coal drip for carbonization time control
The blue or green mass ratio with N-methyl pyrrolidones is 1:20-50, medium temperature coal pitch is 1 with the mass ratio of sodium chloride template:1-20；
Step 3, sample after charing process obtained in step 2 is cooled to room temperature taking-up, adopt and chlorination be washed with deionized
Sodium template, is dried to obtain nanometer sheet；
Step 4, the nanometer sheet for obtaining step 3 are carried out at charing in delivering tube furnace under ammonia and argon gas mixed atmosphere
Reason, temperature rises to 900~1100 DEG C with 2~10 DEG C/min heating rates, and carbonization time is controlled in 1~3h, is cooled to room temperature and is taken
Go out, target material Pitch-based Carbon nanometer sheet is obtained, the ammonia is 1 with argon gas volume flow ratio:0.25-4.
Pitch-based Carbon nanometer sheet prepared by methods described, the application as negative material on sodium-ion battery.
Present invention has the advantages that：A kind of preparation side of the Pitch-based Carbon nanometer sheet for anode material of lithium-ion battery
Method, comprises the following steps：(1) absolute ethyl alcohol is placed in reactor first, then saturated aqueous sodium chloride is added dropwise over nothing
In water-ethanol, solvent evaporated is obtained sodium chloride template, and medium temperature coal pitch is dissolved in N-methyl pyrrolidones and is placed in oil bath by (2)
In, then be added thereto to as sodium chloride template obtained in step 1, after being well mixed, heating is evaporated N-methyl pyrrolidones, then will
Said mixture carries out charing process in delivering tube furnace under inert gas shielding, and (3) are by after charing process obtained in step 2
Sample is cooled to room temperature taking-up, adopts and sodium chloride template is washed with deionized, and is dried to obtain nanometer sheet, and (4) obtain step 3
Nanometer sheet is processed in delivering tube furnace under ammonia and argon gas mixed atmosphere, is cooled to room temperature taking-up, and target material is obtained
Pitch-based Carbon nanometer sheet.Compared with the prior art, preparation method provided by the present invention is simple and easy to apply, the preparation of charcoal nanometer sheet
Journey does not need pickling to remove removing template, environmental protection；Sodium chloride template and nmp solvent can be recycled, and production cost is relatively low；System
Standby raw material and template are cheap, abundance, it is easy to accomplish large-scale production；In addition, Pitch-based Carbon prepared by the present invention
Nanometer sheet shows reversible storage sodium capacity higher as anode material of lithium-ion battery, preferable high rate performance and excellent follows
Ring performance.
Brief description of the drawings
Fig. 1 is the stereoscan photograph figure of Pitch-based Carbon nanometer sheet prepared by the embodiment of the present invention 2.
Fig. 2 is Pitch-based Carbon nanometer sheet transmission electron microscope photo figure prepared by the embodiment of the present invention 2.
Fig. 3 is the X ray diffracting spectrum of Pitch-based Carbon nanometer sheet prepared by the embodiment of the present invention 2.
Fig. 4 is the Pitch-based Carbon nanometer sheet prepared with the embodiment of the present invention 2 different current densities in sodium ion half-cell
Under charge-discharge performance curve map.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
The absolute ethyl alcohol of 500ml is placed in reactor first, then the saturated aqueous sodium chloride of 100ml is added dropwise over
In absolute ethyl alcohol, 90 DEG C of solvent evaporateds are obtained sodium chloride template；2g medium temperature coal pitch is dissolved in 80g N-methyls pyrrolidones simultaneously
It is placed in oil bath, then is added thereto to 20g sodium chloride templates, after being well mixed, 205 DEG C of heating is evaporated N-methyl pyrrolidones,
Said mixture is delivered under nitrogen protection again carry out charing process in tube furnace, temperature is risen to 5 DEG C/min heating rates
700 DEG C, carbonization time is 2h, is cooled to room temperature taking-up, and sodium chloride template is washed with deionized, and is dried to obtain nanometer sheet；
The nanometer sheet that will be obtained again carries out charing process, temperature in delivering tube furnace under 100ml ammonias and 50ml argon gas mixed atmospheres
900 DEG C are risen to 5 DEG C/min heating rates, carbonization time is 2h, be cooled to room temperature taking-up, target material Pitch-based Carbon is obtained and receives
Rice piece, XRD is characterized and found, 002 interlamellar spacing of Pitch-based Carbon nanometer sheet is up to 0.350nm.By Pitch-based Carbon nanometer sheet and acetylene
Black, PVDF (polyvinylidene fluoride) is according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, is assembled in glove box
Sodium-ion battery.Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is
0.01-3V, measures the Pitch-based Carbon nanometer sheet in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 125.6mAh g-1。
Embodiment 2
The absolute ethyl alcohol of 1000ml is placed in reactor first, then the saturated aqueous sodium chloride of 100ml is dropwise added
Enter in absolute ethyl alcohol, 90 DEG C of solvent evaporateds are obtained sodium chloride template；2g medium temperature coal pitch is dissolved in 80g N-methyl pyrrolidones
It is placed in oil bath, then is added thereto to 20g sodium chloride templates, after being well mixed, 205 DEG C of heating is evaporated N-methyl pyrrolidines
Ketone, then said mixture is delivered under nitrogen protection carry out charing process in tube furnace, temperature is with 5 DEG C/min heating rate liters
To 700 DEG C, carbonization time is 2h, is cooled to room temperature taking-up, and sodium chloride template is washed with deionized, and is dried to obtain nanometer
Piece；The nanometer sheet that will be obtained again carries out charing process in delivering tube furnace under 75ml ammonias and 75ml argon gas mixed atmospheres, temperature
Degree rises to 1000 DEG C with 5 DEG C/min heating rates, and carbonization time is 2h, is cooled to room temperature taking-up, and target material asphaltic base is obtained
Charcoal nanometer sheet, XRD is characterized and found, 002 interlamellar spacing of Pitch-based Carbon nanometer sheet is up to 0.378nm.By Pitch-based Carbon nanometer sheet with
Acetylene black, PVDF (polyvinylidene fluoride) are according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, in glove box
Assembling sodium-ion battery.Battery performance, charging/discharging voltage model are tested on Land CT2001A type battery test systems
It is 0.01-3V to enclose, and measures the Pitch-based Carbon nanometer sheet in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 320.4mAh
g-1。
Embodiment 3
The absolute ethyl alcohol of 1000ml is placed in reactor first, then the saturated aqueous sodium chloride of 100ml is dropwise added
Enter in absolute ethyl alcohol, 90 DEG C of solvent evaporateds are obtained sodium chloride template；2g medium temperature coal pitch is dissolved in 80g N-methyl pyrrolidones
It is placed in oil bath, then is added thereto to 20g sodium chloride templates, after being well mixed, 205 DEG C of heating is evaporated N-methyl pyrrolidines
Ketone, then said mixture is delivered under nitrogen protection carry out charing process in tube furnace, temperature is with 5 DEG C/min heating rate liters
To 700 DEG C, carbonization time is 2h, is cooled to room temperature taking-up, and sodium chloride template is washed with deionized, and is dried to obtain nanometer
Piece；The nanometer sheet that will be obtained again carries out charing process in delivering tube furnace under 60ml ammonias and 90ml argon gas mixed atmospheres, temperature
Degree rises to 1100 DEG C with 5 DEG C/min heating rates, and carbonization time is 2h, is cooled to room temperature taking-up, and target material asphaltic base is obtained
Charcoal nanometer sheet, XRD is characterized and found, 002 interlamellar spacing of hard carbon nanometer sheet is up to 0.343nm.By Pitch-based Carbon nanometer sheet and acetylene
Black, PVDF (polyvinylidene fluoride) is according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, is assembled in glove box
Sodium-ion battery.Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is
0.01-3V, measures the Pitch-based Carbon nanometer sheet in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 163.5mAh g-1。
Embodiment 4
The absolute ethyl alcohol of 1000ml is placed in reactor first, then the saturated aqueous sodium chloride of 100ml is dropwise added
Enter in absolute ethyl alcohol, 90 DEG C of solvent evaporateds are obtained sodium chloride template；2g medium temperature coal pitch is dissolved in 80g N-methyl pyrrolidones
It is placed in oil bath, then is added thereto to 20g sodium chloride templates, after being well mixed, 205 DEG C of heating is evaporated N-methyl pyrrolidines
Ketone, then said mixture is delivered under nitrogen protection carry out charing process in tube furnace, temperature is with 5 DEG C/min heating rate liters
To 700 DEG C, carbonization time is 2h, is cooled to room temperature taking-up, and sodium chloride template is washed with deionized, and is dried to obtain nanometer
Piece；The nanometer sheet that will be obtained again carries out charing process in delivering tube furnace under 50ml ammonias and 100ml argon gas mixed atmospheres, temperature
Degree rises to 1100 DEG C with 5 DEG C/min heating rates, and carbonization time is 1h, is cooled to room temperature taking-up, and target material asphaltic base is obtained
Charcoal nanometer sheet, XRD is characterized and found, 002 interlamellar spacing of hard carbon nanometer sheet is up to 0.352nm.By Pitch-based Carbon nanometer sheet and acetylene
Black, PVDF (polyvinylidene fluoride) is according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, is assembled in glove box
Sodium-ion battery.Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is
0.01-3V, measures the Pitch-based Carbon nanometer sheet in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 195.5mAh g-1。
Embodiment 5
The absolute ethyl alcohol of 500ml is placed in reactor first, then the saturated aqueous sodium chloride of 100ml is added dropwise over
In absolute ethyl alcohol, 110 DEG C of solvent evaporateds are obtained sodium chloride template；2g medium temperature coal pitch is dissolved in 80g N-methyl pyrrolidones
It is placed in oil bath, then is added thereto to 20g sodium chloride templates, after being well mixed, 205 DEG C of heating is evaporated N-methyl pyrrolidines
Ketone, then said mixture is carried out into charing process in dispensing tube furnace under argon gas protection, temperature is with 5 DEG C/min heating rate liters
To 700 DEG C, carbonization time is 2h, is cooled to room temperature taking-up, and sodium chloride template is washed with deionized, and is dried to obtain nanometer
Piece；The nanometer sheet that will be obtained again is carried out at charing in delivering tube furnace under 37.5ml ammonias and 112.5ml argon gas mixed atmospheres
Reason, temperature rises to 1000 DEG C with 5 DEG C/min heating rates, and carbonization time is 2h, is cooled to room temperature taking-up, and target material drip is obtained
Blue or green base charcoal nanometer sheet, XRD is characterized and found, 002 interlamellar spacing of Pitch-based Carbon nanometer sheet is up to 0.384nm.By Pitch-based Carbon nanometer
Piece is with acetylene black, PVDF (polyvinylidene fluoride) according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, in gloves
Sodium-ion battery is assembled in case.Battery performance, discharge and recharge electricity are tested on Land CT2001A type battery test systems
Pressure scope is 0.01-3V, measures the Pitch-based Carbon nanometer sheet in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach
240.5mAh g-1。
Embodiment 6
The absolute ethyl alcohol of 800ml is placed in reactor first, then the saturated aqueous sodium chloride of 100ml is added dropwise over
In absolute ethyl alcohol, 100 DEG C of solvent evaporateds are obtained sodium chloride template；2g medium temperature coal pitch is dissolved in 80g N-methyl pyrrolidones
It is placed in oil bath, then is added thereto to 10g sodium chloride templates, after being well mixed, 205 DEG C of heating is evaporated N-methyl pyrrolidines
Ketone, then said mixture is carried out into charing process in dispensing tube furnace under argon gas protection, temperature is with 5 DEG C/min heating rate liters
To 700 DEG C, carbonization time is 2h, is cooled to room temperature taking-up, and sodium chloride template is washed with deionized, and is dried to obtain nanometer
Piece；The nanometer sheet that will be obtained again carries out charing process in delivering tube furnace under 33ml ammonias and 117ml argon gas mixed atmospheres, temperature
Degree rises to 1000 DEG C with 5 DEG C/min heating rates, and carbonization time is 2h, is cooled to room temperature taking-up, and target material asphaltic base is obtained
Charcoal nanometer sheet, XRD is characterized and found, 002 interlamellar spacing of Pitch-based Carbon nanometer sheet is up to 0.370nm.By Pitch-based Carbon nanometer sheet with
Acetylene black, PVDF (polyvinylidene fluoride) are according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, in glove box
Assembling sodium-ion battery.Battery performance, charging/discharging voltage model are tested on Land CT2001A type battery test systems
It is 0.01-3V to enclose, and measures the Pitch-based Carbon nanometer sheet in charge-discharge velocity 0.1Ag-1Under conditions of reversible capacity reach 216.0mAh
g-1。
Comparative example 1
The absolute ethyl alcohol of 1000ml is placed in reactor first, then the saturated aqueous sodium chloride of 100ml is dropwise added
Enter in absolute ethyl alcohol, 90 DEG C of solvent evaporateds are obtained sodium chloride template；2g medium temperature coal pitch is dissolved in 80g N-methyl pyrrolidones
It is placed in oil bath, then is added thereto to 20g sodium chloride templates, after being well mixed, 205 DEG C of heating is evaporated N-methyl pyrrolidines
Ketone, then the mixture that will be obtained carries out charing process in dispensing tube furnace under 75ml ammonias and 75ml argon gas mixed atmospheres, temperature
Degree rises to 1000 DEG C with 5 DEG C/min heating rates, and carbonization time is 2h, is cooled to room temperature taking-up, and chlorine is washed with deionized
Change sodium template, be dried to obtain target material Pitch-based Carbon nanometer sheet, XRD is characterized and found, 002 interlamellar spacing of Pitch-based Carbon nanometer sheet
It is 0.342nm.By hard charcoal nanometer sheet and acetylene black, PVDF (polyvinylidene fluoride) according to 7:2:1 mass ratio prepares negative material,
Collector is Copper Foil, and sodium-ion battery is assembled in glove box.Battery is tested on Land CT2001A type battery test systems
Chemical property, charging/discharging voltage scope is 0.01-3V, measures the Pitch-based Carbon nanometer sheet in charge-discharge velocity 0.1A g-1's
Under the conditions of first reversible capacity be 228.6mAh g-1。
Comparative example 2
The absolute ethyl alcohol of 1000ml is placed in reactor first, then the saturated aqueous sodium chloride of 100ml is dropwise added
Enter in absolute ethyl alcohol, 90 DEG C of solvent evaporateds are obtained sodium chloride template；2g medium temperature coal pitch is dissolved in 80g N-methyl pyrrolidones
It is placed in oil bath, then is added thereto to 20g sodium chloride templates, after being well mixed, 205 DEG C of heating is evaporated N-methyl pyrrolidines
Ketone, then said mixture is carried out into charing process in dispensing tube furnace under argon gas protection, temperature is with 5 DEG C/min heating rate liters
To 700 DEG C, carbonization time is 2h, is cooled to room temperature taking-up, and sodium chloride template is washed with deionized, and is dried to obtain nanometer
Piece；The nanometer sheet that will be obtained carries out charing process in delivering tube furnace under argon gas protection, and temperature is with 5 DEG C/min heating rate liters
To 1000 DEG C, carbonization time is 2h, is cooled to room temperature taking-up, and target material Pitch-based Carbon nanometer sheet is obtained, and XRD is characterized and found,
002 interlamellar spacing of Pitch-based Carbon nanometer sheet is 0.348nm.Pitch-based Carbon nanometer sheet and acetylene black, PVDF (are gathered into inclined difluoro second
Alkene) according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, and sodium-ion battery is assembled in glove box.In Land
Battery performance is tested on CT2001A type battery test systems, charging/discharging voltage scope is 0.01-3V, measures the pitch
Base charcoal nanometer sheet is in charge-discharge velocity 0.1Ag-1Under conditions of first reversible capacity be 136.7mAh g-1。
Comparative example 3
Charing process is carried out during 2g medium temperature coal pitch is delivered into tube furnace under 75ml ammonias and 75ml argon gas mixed atmospheres,
Temperature rises to 1000 DEG C with 5 DEG C/min heating rates, and carbonization time is 2h, is cooled to room temperature taking-up, and be washed with deionized
Sodium chloride template, is dried to obtain target material Pitch-based Carbon nanometer sheet.It is again that Pitch-based Carbon nanometer sheet and acetylene black, PVDF is (poly-
Vinylidene fluoride) according to 7:2:1 mass ratio prepares negative material, and collector is Copper Foil, and sodium-ion battery is assembled in glove box.
Battery performance is tested on Land CT2001A type battery test systems, charging/discharging voltage scope is 0.01-3V, is measured
The Pitch-based Carbon nanometer sheet is in charge-discharge velocity 0.1Ag-1Under conditions of first reversible capacity be 140.5mAh g-1。
Claims (2)
1. the preparation method of a kind of Pitch-based Carbon nanometer sheet for anode material of lithium-ion battery, it is characterised in that including following
Step：
Step 1, first absolute ethyl alcohol is placed in reactor, then saturated aqueous sodium chloride is added dropwise in absolute ethyl alcohol,
Solvent evaporated is obtained sodium chloride template, temperature control at 90-120 DEG C, the saturated aqueous sodium chloride and absolute ethyl alcohol volume
Than being 1:1-10；
Step 2, medium temperature coal pitch is dissolved in N-methyl pyrrolidones it is placed in oil bath, then is added thereto to be obtained by step 1
Sodium chloride template, be well mixed after, heating be evaporated N-methyl pyrrolidones, temperature control at 200-210 DEG C, then will it is above-mentioned mix
Compound carries out charing process in delivering tube furnace under inert gas shielding, and temperature rises to 650 with 2~10 DEG C/min heating rates
~850 DEG C, carbonization time control is selected from the one kind in nitrogen or argon gas, medium temperature coal pitch and nitrogen in 1~3h, the inert gas
The mass ratio of methyl pyrrolidone is 1:20-50, medium temperature coal pitch is 1 with the mass ratio of sodium chloride template:1-20；
Step 3, sample after charing process obtained in step 2 is cooled to room temperature taking-up, adopt and sodium chloride mould be washed with deionized
Plate, is dried to obtain nanometer sheet；
Step 4, the nanometer sheet for obtaining step 3 carry out charing process in delivering tube furnace under ammonia and argon gas mixed atmosphere,
Temperature rises to 900~1100 DEG C with 2~10 DEG C/min heating rates, and the ratio of the ammonia and argon gas is 1:0.25-4, charing
Time control is cooled to room temperature taking-up in 1~3h, and target material Pitch-based Carbon nanometer sheet, the ammonia and argon gas volume is obtained
Flow-rate ratio is 1:0.25-4.
2. the Pitch-based Carbon nanometer sheet that according to claim 1 prepared by method, as negative material on sodium-ion battery
Using.
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Cited By (11)
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| CN107732240A (en) * | 2017-09-05 | 2018-02-23 | 合肥工业大学 | The preparation method of anode material of lithium-ion battery, and negative material prepared therefrom |
| CN108002361A (en) * | 2017-12-08 | 2018-05-08 | 大连理工大学 | A kind of preparation method of high sulfur content nitrogen sulphur codope pitch base carbon material |
| CN108163832A (en) * | 2017-12-08 | 2018-06-15 | 大连理工大学 | A kind of preparation method and applications of pitch base carbon nanometer sheet |
| CN108807892A (en) * | 2018-06-06 | 2018-11-13 | 郑州中科新兴产业技术研究院 | A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material |
| CN109461902A (en) * | 2018-09-29 | 2019-03-12 | 大连理工大学 | A kind of preparation method and applications of two ferrous selenides/honeycomb carbon composite |
| CN110386626A (en) * | 2018-04-16 | 2019-10-29 | 中国科学技术大学 | A kind of cobalt protoxide thin slice, preparation method and its decompose the application in water entirely in visible light catalytic |
| CN110451475A (en) * | 2019-07-05 | 2019-11-15 | 北京化工大学 | A kind of preparation method of Pitch-based Carbon microballoon and its application as sodium ion battery electrode material |
| CN111377432A (en) * | 2020-03-24 | 2020-07-07 | 中国科学院化学研究所 | Method for preparing layered nano carbon material by coal solvent heat treatment |
| CN113224295A (en) * | 2021-05-19 | 2021-08-06 | 东北大学 | Preparation method and application of asphalt-based nano carbon sheet |
| CN114314673A (en) * | 2021-12-30 | 2022-04-12 | 合肥学院 | Preparation method of flaky FeOCl nano material |
| CN114373925A (en) * | 2020-10-14 | 2022-04-19 | 天津工业大学 | Preparation method and application of oxidation modified amorphous carbon material |
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| CN106099109A (en) * | 2016-06-22 | 2016-11-09 | 大连理工大学 | A kind of preparation method and applications of asphaltic base hard charcoal nanometer sheet |
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| CN105845973A (en) * | 2016-05-12 | 2016-08-10 | 陕西科技大学 | Preparation method for porous carbon negative electrode material of sodium ion battery in low temperature through self-assembly |
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| CN107732240A (en) * | 2017-09-05 | 2018-02-23 | 合肥工业大学 | The preparation method of anode material of lithium-ion battery, and negative material prepared therefrom |
| CN108002361B (en) * | 2017-12-08 | 2020-11-10 | 大连理工大学 | Preparation method of high-sulfur-content nitrogen-sulfur co-doped asphalt-based carbon material |
| CN108002361A (en) * | 2017-12-08 | 2018-05-08 | 大连理工大学 | A kind of preparation method of high sulfur content nitrogen sulphur codope pitch base carbon material |
| CN108163832A (en) * | 2017-12-08 | 2018-06-15 | 大连理工大学 | A kind of preparation method and applications of pitch base carbon nanometer sheet |
| CN108163832B (en) * | 2017-12-08 | 2020-11-20 | 大连理工大学 | Preparation method and application of asphalt-based carbon nanosheet |
| CN110386626A (en) * | 2018-04-16 | 2019-10-29 | 中国科学技术大学 | A kind of cobalt protoxide thin slice, preparation method and its decompose the application in water entirely in visible light catalytic |
| CN108807892A (en) * | 2018-06-06 | 2018-11-13 | 郑州中科新兴产业技术研究院 | A kind of preparation method of asphaltic base silicon-carbon nanometer sheet lithium cell negative pole material |
| CN109461902A (en) * | 2018-09-29 | 2019-03-12 | 大连理工大学 | A kind of preparation method and applications of two ferrous selenides/honeycomb carbon composite |
| CN109461902B (en) * | 2018-09-29 | 2021-07-16 | 大连理工大学 | Preparation method and application of iron diselenide/honeycomb carbon composite material |
| CN110451475A (en) * | 2019-07-05 | 2019-11-15 | 北京化工大学 | A kind of preparation method of Pitch-based Carbon microballoon and its application as sodium ion battery electrode material |
| CN111377432A (en) * | 2020-03-24 | 2020-07-07 | 中国科学院化学研究所 | Method for preparing layered nano carbon material by coal solvent heat treatment |
| CN114373925A (en) * | 2020-10-14 | 2022-04-19 | 天津工业大学 | Preparation method and application of oxidation modified amorphous carbon material |
| CN113224295A (en) * | 2021-05-19 | 2021-08-06 | 东北大学 | Preparation method and application of asphalt-based nano carbon sheet |
| CN114314673A (en) * | 2021-12-30 | 2022-04-12 | 合肥学院 | Preparation method of flaky FeOCl nano material |
| CN114314673B (en) * | 2021-12-30 | 2023-10-20 | 合肥学院 | Preparation method of flaky FeOCl nano material |
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