CN107732240A - The preparation method of anode material of lithium-ion battery, and negative material prepared therefrom - Google Patents
The preparation method of anode material of lithium-ion battery, and negative material prepared therefrom Download PDFInfo
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- CN107732240A CN107732240A CN201710792943.6A CN201710792943A CN107732240A CN 107732240 A CN107732240 A CN 107732240A CN 201710792943 A CN201710792943 A CN 201710792943A CN 107732240 A CN107732240 A CN 107732240A
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- ion battery
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- alkali metal
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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
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- 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
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a kind of preparation method of the negative material of sodium-ion battery, and negative material prepared therefrom, the negative pole comprising the negative material, the sodium-ion battery comprising the negative pole.The preparation method of the negative material of the sodium-ion battery, it comprises the following steps：1) pitch, the second material and alkali metal salt are mixed and be ground；2) mixture obtained in step 1) is subjected to tabletting under 10MPa to 50MPa pressure；3) by the block powder obtained in step 2), in atmosphere of inert gases or under vacuum conditions at a temperature of 600~800 DEG C, low-temperature carbonization is handled 0.5~5 hour；4) product obtained in step 3) is washed and dries to obtain hard carbon presoma；5) the high temperature cabonization processing hard carbon presoma 0.5~5 hour at 800~1500 DEG C in atmosphere of inert gases or under vacuum conditions, wherein, the ratio of the quality of the gross mass and the alkali metal salt of the pitch and the second material is 1:1~1:20.
Description
Technical field
The present invention relates to a kind of preparation method of the negative material of sodium-ion battery, and negative material prepared therefrom, bag
Negative pole containing the negative material, the sodium-ion battery comprising the negative pole, more specifically, it is related to a kind of next using template pressed disc method
The method for preparing the negative material of sodium-ion battery, the negative pole comprising the negative material, the sodium-ion battery comprising the negative pole.
Background technology
Continue to increase with the development and the size of population of society, global energy demand improves constantly, Devoting Major Efforts To Developing and
Using regenerative resource, such as solar energy, wind energy, geothermal energy, tide energy, dependence of the mankind to fossil energy is progressively broken away from, is
Promote the only possible approach of social sustainable development.In current energy storage system, chemical energy storage battery due to flexibility,
High efficiency and without territory restriction, is most promising large-scale energy storage device.
Lithium ion battery is as high specific energy batteries system, in portable type electronic product, electric tool and electric automobile field
Developed rapidly.However, being limited by lithium resource, the development of extensive accumulation power supply possibly can not be supported.Therefore, develop
Aboundresources, the cheap advanced battery system of cost, it is the inevitable outlet for solving following extensive storing up electricity application.Sodium element and lithium
In same main group, chemical property is similar, and electrode potential also relatively, and the aboundresources of sodium, it is low to refine cost.If
Lithium is substituted with sodium, the sodium-ion battery of excellent working performance is developed, the competitive advantage bigger than lithium ion battery will be possessed.Cause
This, seeks the storage sodium electrode material of high power capacity and excellent cycling performance as the study hotspot in current battery field.
For at present, graphite cathode largely is used in lithium ion battery, but sodium ion is difficult to be embedded in graphite layers, causes it
Store up sodium poor effect.Coulombic efficiency is very low first due to it for expanded graphite, and titanium-based negative material is due to its poor Stability Analysis of Structures
Property and reversible capacity, are unsuitable for commercially producing.For porous carbon materials due to its large specific surface area, stable structure can
More storage sodium capacity are provided.But during current synthesizing porous carbon material, the selection to reactant or template requires higher, and portion
Divide synthetic method preparation technology complicated, process is difficult to control, higher so as to result in the cost of synthetic material, and is not suitable for big
Amount production.Meanwhile large specific surface area also results in the decay of battery reversible capacity, and a series of side reactions can be produced, cause electricity
Fail in pond.Therefore, to realize that higher reversible sodium ion is embedded and abjection capacity is, it is necessary to find suitable template, while control more
The specific surface area and pore-size distribution of hole carbon material are only key.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the negative material of sodium-ion battery.Sodium prepared by this method
The negative material of ion battery has level pore structure, and has large specific surface area, is adapted to the insertion and abjection of sodium ion, together
When ensure that higher reversible capacity.
Another object of the present invention is to provide the negative material of the sodium-ion battery obtained by the preparation method.
It is still another object of the present invention to provide the negative pole of the negative material comprising the sodium-ion battery.
A further object of the present invention is to provide the sodium-ion battery for including the negative pole.
According to an aspect of the invention, there is provided a kind of preparation method of the negative material of sodium-ion battery, it includes
Following steps：
1) pitch, the second material and alkali metal salt are mixed and be ground；
2) mixture obtained in step 1) is subjected to tabletting under 10MPa to 50MPa pressure；
3) by the block powder obtained in step 2) in atmosphere of inert gases or under vacuum conditions at 600~800 DEG C
At a temperature of low-temperature carbonization handle 0.5~5 hour；
4) product obtained in step 3) is washed and dries to obtain hard carbon presoma；
5) the high temperature cabonization processing hard carbon forerunner at 800~1500 DEG C in atmosphere of inert gases or under vacuum conditions
Body 0.5~5 hour.
Wherein, the pitch is selected from least one of selected from coal tar pitch and petroleum asphalt and bitumen.
Second material is in phenolic resin, lignin, epoxy resin, poly furfuryl alcohol, polyvinyl alcohol, polyvinyl chloride
At least one, preferably phenolic resin.The phenolic resin can be selected from linear phenolic resin, thermosetting phenolic resin and water-soluble
At least one of property phenolic resin.The molecular weight of second material influences less on the structure of product, and its molecular weight is not by special
Limitation.
The mass ratio of the pitch and second material is 1:10~10:1, preferably 1:5~5:1.
The alkali metal salt is that not molten and reaction of not decomposing alkali metal salt, the example include at a temperature of 800 DEG C,
Lithium chloride, potassium chloride, sodium chloride, lithium sulfate, potassium sulfate and sodium sulphate, preferably sodium salt, most preferably sodium chloride.
The ratio of the quality of the gross mass and the alkali metal salt of the pitch and the second material is 1:1~1:20, preferably
1:1~1:15, more preferably 1:1~1:10.
The grinding is in order that pitch, the second material and alkali metal salt are sufficiently mixed to obtain well mixed chemical combination
Thing, preferably grind 0.5 to 24 hour.Preferably, it is ground using ball mill.It is further preferred that wet ball grinding, addition
Solvent is not particularly limited, such as can be absolute ethyl alcohol；When carrying out described ball milling, the rotating speed of ball mill is 400Hz, ball
For material than being 10: 1, preferable Ball-milling Time is 1~12 hour.
The temperature of the drying is not particularly limited, preferably 30~100 DEG C, preferably 70~80 DEG C.
The pressure of the tabletting is 10MPa to 50MPa, preferably 20 to 40MPa, more preferably 30MPa.
Described low-temperature carbonization treatment temperature be 600~800 DEG C, preferably 700~800 DEG C, the low-temperature carbonization time be 0.5~
5 hours, preferably 1~2 hour.
The high temperature cabonization treatment temperature is 800~1500 DEG C, preferably 1000~1500 DEG C, more preferably 1100~1400
DEG C, the time of the high temperature cabonization processing is 0.5~5 hour, preferably 1~2 hour.
According to another aspect of the present invention, there is provided the negative material of the sodium-ion battery prepared by methods described.
According to another aspect of the invention, there is provided a kind of negative pole for sodium-ion battery, it includes the sodium ion
The negative material of battery.
In accordance with a further aspect of the present invention, there is provided a kind of sodium-ion battery, it includes the negative pole.
Shown by electro-chemical test, the anode material of lithium-ion battery prepared according to preparation method of the present invention has
There is the embedding de- ability of good reversible sodium ion, high rate performance is excellent, has good cyclical stability, and preparation method is simple,
Abundant raw material, cost is cheap, suitable for the occasion of demand high power capacity and high power discharge, be expected to turn into a kind of practical sodium from
Sub- cell negative electrode material.
Brief description of the drawings
Fig. 1 is the SEM photograph of the negative material of 1 obtained sodium-ion battery according to an embodiment of the invention.
Fig. 2 is the graph of pore diameter distribution of the negative material of according to embodiments of the present invention 1 obtained sodium-ion battery.
Fig. 3 is first all charging and discharging curves of the negative material of according to embodiments of the present invention 1 sodium-ion battery.
Fig. 4 is the high rate performance curve of the negative material of according to embodiments of the present invention 1 sodium-ion battery.
Fig. 5 is the cycle performance curve of the negative material of according to embodiments of the present invention 1 sodium-ion battery.
Embodiment
The pitch comes from asphalt (No. 70), place of production Shandong；The phenolic resin (4022), from Shanghai；It is described
The alkali metal salts such as sodium chloride, potassium chloride, sodium sulphate, from Chemical Reagent Co., Ltd., Sinopharm Group.
Embodiment 1
1g pitches, 1g phenolic resin, 8g sodium chloride and a small amount of absolute ethyl alcohol are weighed, adds in ball grinder and grinds 10 hours；
Dried at 80 DEG C, tabletting, pressure 30MPa are carried out to the powder using tablet press machine；Take the block powder to insert in tube furnace, lead to
Enter argon gas, 750 DEG C of constant temperature 2 hours；Sample is taken out and washed after being cooled to room temperature to remove sodium chloride；After being dried at 80 DEG C, take
The powder is inserted in tube furnace, is passed through argon gas, 1100 DEG C of constant temperature 2 hours, obtains porous carbon materials, as sodium-ion battery is negative
Pole material.
The particle size of porous carbon materials obtained by the present embodiment is 5~40 μm, and Fig. 1 is the SEM electron microscopes of porous carbon, is shown
The material diameter macropores are 0.5~3 μm；The as shown by data that isothermal nitrogen adsorption detachment assays obtain, its BET specific surface area reach
30m2/ g, Fig. 2 graph of pore diameter distribution show that its pore-size distribution concentrates on 3nm or so, and total pore volume reaches 0.074cm3/ g, and the material
Material has micropore and mesoporous simultaneously, therefore hierarchical porous structure is presented.
Gained carbon material is mixed by 90 with carbon black, sodium carboxymethylcellulose (CMC), butadiene-styrene rubber (SBR)：10：5：5 weight
Amount is than uniformly, being applied as electrode film.Using the electrode film as working electrode, metallic sodium piece is to electrode, 1mol L-1NaPF6(EC-
DMC=1:1) battery is assembled into for electrolyte, and tests its chemical property.As shown in Figure 3 under 0.1C current densities, material
Reversible capacity be 280mAh g-1.Shown in Fig. 4 under 32C current densities, the reversible capacity of material is 66mAh/g, shown in Fig. 5
Under 1C current densities, for circulating battery after 550 weeks, capacity remains at 188mAh/g.
Embodiment 2
1g pitches, 1g phenolic resin, 8g potassium chloride and a small amount of absolute ethyl alcohol are weighed, adds in ball grinder and grinds 10 hours；
Dried at 80 DEG C, tabletting, pressure 30MPa are carried out to the powder using tablet press machine；Take the block powder to insert in tube furnace, lead to
Enter argon gas, 750 DEG C of constant temperature 2 hours；Sample is taken out and washed after being cooled to room temperature to remove potassium chloride；After being dried at 80 DEG C, take
The powder is inserted in tube furnace, is passed through argon gas, 1100 DEG C of constant temperature 2 hours, obtains porous carbon materials.
In addition to the porous carbon materials of gained in example 2 are used as into the negative material of sodium-ion battery, with implementation
The identical mode assembled battery of example 1 simultaneously tests its chemical property.As a result it is shown in table 1 below.
Embodiment 3
1g pitches, 1g phenolic resin, 8g sodium sulphate and a small amount of absolute ethyl alcohol are weighed, adds in ball grinder and grinds 10 hours；
Dried at 80 DEG C, tabletting, pressure 30MPa are carried out to the powder using tablet press machine；Take the block powder to insert in tube furnace, lead to
Enter argon gas, 750 DEG C of constant temperature 2 hours；Sample is taken out and washed after being cooled to room temperature to remove sodium sulphate；After being dried at 80 DEG C, take
The powder is inserted in tube furnace, is passed through argon gas, 1100 DEG C of constant temperature 2 hours, obtains porous carbon materials.
In addition to the porous carbon materials of gained in embodiment 3 are used as into the negative material of sodium-ion battery, with implementation
The identical mode assembled battery of example 1 simultaneously tests its chemical property.As a result it is shown in table 1 below.
Embodiment 4
1g pitches, 3g phenolic resin, 8g sodium chloride and a small amount of absolute ethyl alcohol are weighed, adds in ball grinder and grinds 10 hours；
Dried at 80 DEG C, tabletting, pressure 30MPa are carried out to the powder using tablet press machine；Take the block powder to insert in tube furnace, lead to
Enter argon gas, 750 DEG C of constant temperature 2 hours；Sample is taken out and washed after being cooled to room temperature to remove sodium chloride；After being dried at 80 DEG C, take
The powder is inserted in tube furnace, is passed through argon gas, 1100 DEG C of constant temperature 2 hours, obtains porous carbon materials.
In addition to the porous carbon materials of gained in example 4 are used as into the negative material of sodium-ion battery, with implementation
The identical mode assembled battery of example 1 simultaneously tests its chemical property.As a result it is shown in table 1 below.
Comparative example 1
1g pitches, 1g phenolic resin and a small amount of absolute ethyl alcohol are weighed, adds in ball grinder and grinds 10 hours；Dried at 80 DEG C
It is dry, tabletting, pressure 30MPa are carried out to the powder using tablet press machine；Take the block powder to insert in tube furnace, be passed through argon gas,
750 DEG C of constant temperature 2 hours；Sample is taken out and washed after being cooled to room temperature；After being dried at 80 DEG C, the powder is taken to insert in tube furnace,
It is passed through argon gas, 1100 DEG C of constant temperature 2 hours, obtains porous carbon materials.
In addition to the porous carbon materials of the gained in comparative example 1 to be used as to the negative material of sodium-ion battery, with implementation
The identical mode assembled battery of example 1 simultaneously tests its chemical property.As a result it is shown in table 1 below.
Comparative example 2
1g pitches, 8g sodium chloride and a small amount of absolute ethyl alcohol are weighed, adds in ball grinder and grinds 10 hours；Dried at 80 DEG C,
Tabletting, pressure 30MPa are carried out to the powder using tablet press machine；Take the block powder to insert in tube furnace, be passed through argon gas, 750
DEG C constant temperature 2 hours；Sample is taken out and washed after being cooled to room temperature to remove sodium chloride；After being dried at 80 DEG C, the powder is taken to insert
In tube furnace, argon gas is passed through, 1100 DEG C of constant temperature 2 hours, obtain porous carbon materials.
In addition to the porous carbon materials of the gained in comparative example 2 to be used as to the negative material of sodium-ion battery, with implementation
The identical mode assembled battery of example 1 simultaneously tests its chemical property.As a result it is shown in table 1 below.
After tested, the negative material correlated performance test result that above-described embodiment 1 is prepared to embodiment 4 and comparative example 1-2
It is as shown in table 1 respectively.
Table 1：The chemical property after battery is made in the material of each embodiment
As can be seen from the table above, using embodiment 1, resulting negative material performance is good, especially material
Cycle performance is significantly improved compared with comparative example under the high magnification of material.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., it should be included in the protection of the claim of the present invention
Within the scope of.
Claims (10)
1. a kind of preparation method of the negative material of sodium-ion battery, it comprises the following steps：
1) pitch, the second material and alkali metal salt are mixed and be ground；
2) mixture obtained in step 1) is subjected to tabletting under 10MPa to 50MPa pressure；
3) by the block powder obtained in step 2) in atmosphere of inert gases or under vacuum conditions in 600~800 DEG C of temperature
Lower low-temperature carbonization is handled 0.5~5 hour；
4) product obtained in step 3) is washed and dries to obtain hard carbon presoma；
5) the high temperature cabonization processing hard carbon presoma at 800~1500 DEG C in atmosphere of inert gases or under vacuum conditions
0.5~5 hour,
Wherein, the ratio of the quality of the gross mass and the alkali metal salt of the pitch and the second material is 1:1~1:20, it is described
Second material is selected from least one of phenolic resin, lignin, epoxy resin, poly furfuryl alcohol, polyvinyl alcohol and polyvinyl chloride.
2. preparation method according to claim 1, wherein, the mass ratio of the pitch and second material is 1:10~
10:1。
3. preparation method according to claim 1, wherein, the pitch is selected from selected from coal tar pitch and petroleum asphalt and bitumen
At least one of；And second material is phenolic resin.
4. preparation method according to claim 1, the alkali metal salt is not molten at a temperature of 800 DEG C and not decomposed
The alkali metal salt of reaction.
5. preparation method according to claim 1, wherein, the alkali metal salt be selected from lithium chloride, potassium chloride, sodium chloride,
Lithium sulfate, potassium sulfate and sodium sulphate.
6. preparation method according to claim 1, wherein, described low-temperature carbonization treatment temperature is 700~800 DEG C, with
And the high temperature cabonization treatment temperature is 1000~1500 DEG C, preferably 1100~1400 DEG C.
7. preparation method according to claim 1, wherein, the mass ratio of the pitch and second material is 1:5~
5:1, and the ratio of the quality of the gross mass and the alkali metal salt of the pitch and the second material is 1:1~1:10.
8. the negative material of sodium-ion battery prepared by method according to any one of claim 1 to 7.
9. a kind of negative pole for sodium-ion battery, it includes the negative material of the sodium-ion battery described in claim 8.
10. a kind of sodium-ion battery, it includes the negative pole for sodium-ion battery described in claim 9.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110921647A (en) * | 2019-12-10 | 2020-03-27 | 合肥工业大学 | Hard carbon microsphere with adjustable morphology and pore structure, preparation method and application thereof |
| CN111170298A (en) * | 2020-01-19 | 2020-05-19 | 宁波瞬能科技有限公司 | Preparation method and application of lignin-based hard carbon |
| CN111785963A (en) * | 2020-07-28 | 2020-10-16 | 合肥国轩高科动力能源有限公司 | High-carbon-residue-rate negative electrode material precursor and preparation method and application thereof |
| CN112397715A (en) * | 2020-10-10 | 2021-02-23 | 北京化工大学 | Hard carbon material, preparation method thereof and sodium ion battery |
| CN113800496A (en) * | 2021-08-06 | 2021-12-17 | 深圳市德方纳米科技股份有限公司 | Hard carbon material and preparation method and application thereof |
| CN115676804A (en) * | 2022-12-23 | 2023-02-03 | 郑州中科新兴产业技术研究院 | Asphalt-based porous hard carbon negative electrode material and preparation method and application thereof |
| CN116741992A (en) * | 2023-05-24 | 2023-09-12 | 长沙理工大学 | Porous hard carbon material and preparation method thereof, negative electrode plate and sodium ion battery |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110921647A (en) * | 2019-12-10 | 2020-03-27 | 合肥工业大学 | Hard carbon microsphere with adjustable morphology and pore structure, preparation method and application thereof |
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| CN111785963A (en) * | 2020-07-28 | 2020-10-16 | 合肥国轩高科动力能源有限公司 | High-carbon-residue-rate negative electrode material precursor and preparation method and application thereof |
| CN112397715A (en) * | 2020-10-10 | 2021-02-23 | 北京化工大学 | Hard carbon material, preparation method thereof and sodium ion battery |
| CN113800496A (en) * | 2021-08-06 | 2021-12-17 | 深圳市德方纳米科技股份有限公司 | Hard carbon material and preparation method and application thereof |
| CN115676804A (en) * | 2022-12-23 | 2023-02-03 | 郑州中科新兴产业技术研究院 | Asphalt-based porous hard carbon negative electrode material and preparation method and application thereof |
| CN115676804B (en) * | 2022-12-23 | 2024-01-30 | 郑州中科新兴产业技术研究院 | Porous hard carbon anode material based on asphalt, and preparation method and application thereof |
| CN116741992A (en) * | 2023-05-24 | 2023-09-12 | 长沙理工大学 | Porous hard carbon material and preparation method thereof, negative electrode plate and sodium ion battery |
| CN116741992B (en) * | 2023-05-24 | 2024-02-02 | 长沙理工大学 | Porous hard carbon material and preparation method thereof, negative electrode plate and sodium ion battery |
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