CN109817977A - Carbon negative electrode material of sodium ion battery and preparation method thereof - Google Patents
Carbon negative electrode material of sodium ion battery and preparation method thereof Download PDFInfo
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Abstract
Present invention discloses a kind of Carbon negative electrode material of sodium ion battery and preparation method thereof, the wherein preparation method of Carbon negative electrode material of sodium ion battery, by being dissolved original biomass carbon source with containing the heteroatomic ionic liquid such as nitrogen, phosphorus, boron, then dissolved matter is roasted at high temperature, high-content Heteroatom doping carbon negative pole material is prepared.By containing heteroatomic ion liquid dissolving original biomass carbon sources such as nitrogen, phosphorus, boron, being allowed to be heated more evenly in pyrolysis；On the other hand, content of heteroatoms in material can largely be improved containing hetero atoms such as nitrogen, phosphorus, boron in ionic liquid.The Carbon negative electrode material of sodium ion battery prepared by this method is doped with the hetero atom of higher amount, makes it have higher high rate performance and stable circulation performance.
Description
Technical field
The present invention relates to sodium-ion battery technical field more particularly to a kind of Carbon negative electrode material of sodium ion battery and its preparations
Method.
Background technique
As the unsustainable property and pollution on the environment problem of fossil energy are got worse, new energy is as a kind of
Cleaning, renewable energy obtain extensive concern, and gradually apply to the fields such as electric car and energy storage.With lithium ion battery
It compares, sodium-ion battery has sodium resource abundant, it is considered to be energy-storage battery technology of new generation.
However, due to sodium ion radiusGreater than lithium ion radiusSodium-ion battery is caused to be faced with
The problem that high rate performance is poor, cyclical stability is low.Introduced in carbon material covalent Heteroatom doping (N, B, P, S etc.) be it is a kind of very
The strategy of promising regulation physicochemical properties, can largely improve the chemical property of carbon material, will be this kind of total
Carbon negative pole material of the carbon material of valence Heteroatom doping as sodium-ion battery can improve the multiplying power and circulation of sodium-ion battery
Performance.But the content of heteroatoms ratio such as nitrogen phosphate and sulfur contained in biomass in itself is lower, this directly determine its as sodium from
Sub- battery cathode multiplying power and cyclical stability can be relatively low, therefore direct carbonization biomass is difficult to meet its answering extensively in energy storage field
With.
Summary of the invention
In order to overcome the deficiencies of the prior art, the present invention provides a kind of preparation method of Carbon negative electrode material of sodium ion battery, solution
The certainly problem of sodium-ion battery high rate performance and stable circulation performance difference.
To solve the above problems, the technical solution adopted by the present invention are as follows:
A kind of preparation method of Carbon negative electrode material of sodium ion battery includes at least following steps:
By setting amount by original biomass carbon source be added to containing in N, P, S and B any one or more element from
In the reaction flask of sub- liquid, it is heated to original biomass carbon source and is dissolved completely in ionic liquid, obtain the mixture dissolved；
Mixture is transferred in high temperature process furnances, the temperature of setting is heated under atmosphere of inert gases and keeps 5-
8h, cooled to room temperature obtain the carbon product of Heteroatom doping, electric using the carbon product of the Heteroatom doping as sodium ion
Pond carbon negative pole material.
Further, original biomass carbon source is added to containing any one or more in N, P, S and B by the amount of setting
In the reaction flask of the ionic liquid of element, it is heated to original biomass carbon source and is dissolved completely in ionic liquid, obtain dissolving
Mixture the step of before, comprising:
By the biomass mechanical grinding dried at powder, powder is placed on drying in vacuum drying oven, obtains original biomass
Carbon source.
Further, powder is placed in step dry in vacuum drying oven, the drying temperature range of vacuum drying oven is 80-
120 DEG C, drying time range is 12-48 hours.
Further, biomass is one of peanut shell, rice husk, corncob and soybean stalk or a variety of.
Further, mixture is transferred in high temperature process furnances, the temperature of setting is heated under atmosphere of inert gases
And 5-8h is kept, cooled to room temperature, after the step of obtaining the carbon product of Heteroatom doping, comprising:
The carbon product of Heteroatom doping is rinsed 3-5 times in Buchner funnel with deionized water, the sample obtained after washing
It is sufficiently dry in vacuum drying oven.
Further, ionic liquid includes one or more of borate, phosphate and quaternary ammonium salt.
Further, ionic liquid is 1- ethyl-3-methylimidazole tetrafluoroborate.
Further, described that mixture is transferred in high temperature process furnances, setting is heated under atmosphere of inert gases
Temperature and the step of keep 5-8h in, inert gas includes nitrogen and/or helium, and the rate of gas is 5L/min-10L/min.
Further, described that mixture is transferred in high temperature process furnances, setting is heated under atmosphere of inert gases
Temperature and the step of keep 5-8h in, be heated to 800 DEG C first with the rate of 5 DEG C -10 DEG C/min, after 800 DEG C of holding 1h, then
Any temperature being heated to the rate of 5 DEG C/min in 1200 DEG C -1500 DEG C of temperature range, and at 1200 DEG C -1500 DEG C
5h is kept at any temperature in temperature range.
The present invention also provides a kind of Carbon negative electrode material of sodium ion battery, Carbon negative electrode material of sodium ion battery passes through above-mentioned any
A kind of preparation method preparation gained of Carbon negative electrode material of sodium ion battery.
The utility model has the advantages that the present invention provides a kind of Carbon negative electrode material of sodium ion battery and preparation method thereof, wherein sodium ion
The preparation method of battery carbon negative pole material, by with containing the heteroatomic ionic liquid such as nitrogen, phosphorus, boron by original biomass carbon source
Dissolution, then dissolved matter is roasted at high temperature, high-content Heteroatom doping carbon negative pole material is prepared.By containing nitrogen, phosphorus,
The heteroatomic ion liquid dissolving original biomass carbon source such as boron is allowed to be heated more evenly in pyrolysis；On the other hand, ionic liquid
Containing hetero atoms such as nitrogen, phosphorus, boron in body, content of heteroatoms in material can be largely improved.It is obtained by this method preparation
The Carbon negative electrode material of sodium ion battery obtained, is doped with the hetero atom of higher amount, makes it have higher high rate performance and circulation
Stability.
Detailed description of the invention
Fig. 1 is the SEM figure of carbon negative pole material prepared by the embodiment of the present invention 1；
Fig. 2 is the constituent content figure of carbon negative pole material prepared by the embodiment of the present invention 1；
Fig. 3 is the sodium-ion battery high rate performance figure of carbon negative pole material prepared by the embodiment of the present invention 1；
Fig. 4 is the sodium-ion battery cycle life figure of carbon negative pole material prepared by the embodiment of the present invention 1.
The embodiments will be further described with reference to the accompanying drawings for the realization, the function and the advantages of the object of the present invention.
Specific embodiment
It should be appreciated that described herein, specific examples are only used to explain the present invention, is not intended to limit the present invention.
Embodiment 1:
A kind of preparation method of Carbon negative electrode material of sodium ion battery, includes the following steps:
(1) peanut shell dried is clayed into power with machinery, the partial size of powder is 10 μm of -1mm, 100 in vacuum drying oven
DEG C original biomass carbon source is used as after dry 24 hours；In this step, using peanut shell as biological material, to utilize itself
The hetero atoms such as the nitrogen phosphate and sulfur contained；By peanut shell wear into partial size be 10 μm of -1mm powder in favor of more fully dry and
It is preferably reacted in subsequent step；100 DEG C drying 24 hours in vacuum drying oven guarantee peanut shell powder in the drying process not
It can be reacted with the substance in air, obtain the original biomass carbon source for not mixing other materials；In some other implementation
In example, the original biomass carbon source that this step obtains can also be obtained by other means.
(2) drying peanut shell powder of the 1g as original biomass carbon source is weighed, which is added in batches
Enter into the reaction flask containing 5g 1- ethyl-3-methylimidazole tetrafluoroborate, and 120 DEG C at a temperature of heat, until flower
Raw shell powder is completely dissolved, and obtains the mixture dissolved；The quality of original biomass carbon source and 1- ethyl -3- first in this step
The mass ratio of base tetrafluoroborate can be set by 1:1~1:10, in the present embodiment, according to the matter of original biomass carbon source
It measures and is weighed with the mass ratio of 1- ethyl-3-methylimidazole tetrafluoroborate for 1:5, sufficiently heat, make peanut shell powder complete
It dissolves in 1- ethyl-3-methylimidazole tetrafluoroborate, obtains the mixture of the two.
(3) the good mixture of above-mentioned dissolution is transferred in tube furnace, with the rate of 5 DEG C/min under atmosphere of inert gases
Be heated to 800 DEG C, 800 DEG C at a temperature of keep the temperature 1h, then be heated to 1200 DEG C with the rate of 5 DEG C/min, and in 1200 DEG C of temperature
Degree is lower to keep cooled to room temperature after 5h, obtains the carbon product of Heteroatom doping；In this step, by atmosphere of inert gases
Tube furnace in be heat-treated, avoid oxidation, decarburization；The miscellaneous original obtained under the conditions of Fractional Heat-treatment described in this step
The carbon product of son doping may act as Carbon negative electrode material of sodium ion battery, and rate capability is more excellent, and cyclical stability is preferable.
(4) Heteroatom doping carbon product obtained in previous step is placed in Buchner funnel and rinses 3-5 with deionized water
It is secondary, it is then dry with 100 DEG C of temperature in vacuum drying oven, obtain the carbon negative pole material of high-content Heteroatom doping.This step
Middle progress deionized water flushing is the inorganic ion in order to adhere on the carbon product of Heteroatom doping obtained in previous step
Removal, obtains the carbon product of more pure Heteroatom doping, using it as Carbon negative electrode material of sodium ion battery, rate capability
More excellent, cyclical stability is more preferable.
As shown in Figure 1, the carbon negative pole material of the high-content Heteroatom doping obtained by the preparation method is 3 μ by diameter
M-10 μm and with a thickness of 0.1 μm -3 μm chip architecture form.
Electrochemical results show that the sodium-ion battery made of the carbon negative pole material shows high high rate performance
(see Fig. 3) and excellent cyclical stability (see Fig. 4, table 1), sodium-ion battery at 1C 1570 times circulation after, capacity retention ratio
Still reach 93.3%；After lower 1000 circulations of 2C, capacity retention ratio has reached 93.2%.
As shown in Fig. 2, the atomic percent of nitrogen and boron is 10.15% in the carbon negative pole material.It is mixed due to heteroatomic
Miscellaneous, the d- spacing (interplanar distance) of the material is 0.384nm, and greater than the d- spacing (0.335nm) of graphite, therefore, which has
Conducive to the insertion of sodium ion with move out, improve the high rate performance of sodium-ion battery；Meanwhile hetero atom bring synergistic effect makes
Cyclical stability has obtained further raising.
Embodiment 2:
A kind of preparation method of Carbon negative electrode material of sodium ion battery, includes the following steps:
(1) the soybean stalk dried is clayed into power with machinery, the partial size of powder is 10 μm of -1mm, 100 in vacuum drying oven
DEG C original biomass carbon source is used as after dry 24 hours；In this step, using soybean stalk as biological material, to utilize itself
The hetero atoms such as the nitrogen phosphate and sulfur contained；By soybean stalk wear into partial size be 10 μm of -1mm powder in favor of more fully dry and
It is preferably reacted in subsequent step；100 DEG C drying 24 hours in vacuum drying oven guarantee soybean stalk powder in the drying process not
It can be reacted with the substance in air, obtain the original biomass carbon source for not mixing other materials；In some other implementation
In example, the original biomass carbon source that this step obtains can also be obtained by other means.
(2) the drying soybean for weighing 1g as original biomass carbon source obstructs powder, and drying soybean stalk powder is added in batches
Enter into the reaction flask containing 5g 1- ethyl-3-methylimidazole hexafluorophosphate, and 120 DEG C at a temperature of heat, until big
Beans stalk powder is completely dissolved, and obtains the mixture dissolved；The quality of original biomass carbon source and 1- ethyl -3- first in this step
The mass ratio of base tetrafluoroborate can be set by 1:1~1:10, in the present embodiment, according to the matter of original biomass carbon source
It measures and is weighed with the mass ratio of 1- ethyl-3-methylimidazole tetrafluoroborate for 1:5, sufficiently heated, make soybean stalk powder complete
It dissolves in 1- ethyl-3-methylimidazole tetrafluoroborate, obtains the mixture of the two.
(3) the good mixture of above-mentioned dissolution is transferred in tube furnace, with the rate of 5 DEG C/min under atmosphere of inert gases
Be heated to 800 DEG C, 800 DEG C at a temperature of keep the temperature 1h, then be heated to 1200 DEG C with the rate of 5 DEG C/min, and at 1200 DEG C
At a temperature of keep 5h after cooled to room temperature, obtain the carbon product of Heteroatom doping；In this step, by inert gas atmosphere
It is heat-treated in the tube furnace enclosed, avoids oxidation, decarburization；It is obtained under the conditions of Fractional Heat-treatment described in this step miscellaneous
Atom doped carbon product may act as Carbon negative electrode material of sodium ion battery, and rate capability is more excellent, and cyclical stability is preferable.
(4) Heteroatom doping carbon product obtained in previous step is placed in Buchner funnel and rinses 3-5 with deionized water
It is secondary, it is then dry with 100 DEG C of temperature in vacuum drying oven, obtain the carbon negative pole material of high-content Heteroatom doping.This step
Middle progress deionized water flushing is the inorganic ion in order to adhere on the carbon product of Heteroatom doping obtained in previous step
Removal, obtains the carbon product of more pure Heteroatom doping, using it as Carbon negative electrode material of sodium ion battery, rate capability
More excellent, cyclical stability is more preferable.
Referring to table 1, show the Carbon anode material for the high-content Heteroatom doping that the preparation method obtains by electro-chemical test
Material, the capacity retention ratio at 4C are 104.2%, and capacity retention ratio is 94.8% after 1000 circulations at 1C, at 2C
Capacity retention ratio is 93.5% after 1000 circulations.As it can be seen that the carbon for the high-content Heteroatom doping that the preparation method obtains is negative
Pole material shows good rate capability, has excellent long-term cycle stability.
Embodiment 3:
A kind of preparation method of Carbon negative electrode material of sodium ion battery, includes the following steps:
(1) rice husk dried is clayed into power with machinery, the partial size of powder is 10 μm of -1mm, 100 in vacuum drying oven
DEG C original biomass carbon source is used as after dry 24 hours；In this step, using rice husk as biological material, to utilize itself
The hetero atoms such as the nitrogen phosphate and sulfur contained；By rice husk wear into partial size be 10 μm of -1mm powder in favor of more fully dry and
It is preferably reacted in subsequent step；100 DEG C drying 24 hours in vacuum drying oven guarantee rice husk powder in the drying process not
It can be reacted with the substance in air, obtain the original biomass carbon source for not mixing other materials；In some other implementation
In example, the original biomass carbon source that this step obtains can also be obtained by other means.
(2) drying rice husk powder of the 1g as original biomass carbon source is weighed, which is added portionwise
Into the reaction flask containing 5g bromination 1- cetyl -3- (11- hydroxyl undecyl) -2-methylimidazole quaternary ammonium salt, and at 120 DEG C
At a temperature of heat, until rice husk powder is completely dissolved, obtain the mixture dissolved；Original biomass carbon source in this step
Quality and the mass ratio of 1- ethyl-3-methylimidazole tetrafluoroborate can be set by 1:1~1:10, in the present embodiment, press
The mass ratio of quality and 1- ethyl-3-methylimidazole tetrafluoroborate according to original biomass carbon source weighs for 1:5, sufficiently adds
Heat allows rice husk powder to be completely dissolved in 1- ethyl-3-methylimidazole tetrafluoroborate, obtains the mixture of the two.
(3) mixture for obtaining previous step is transferred in tube furnace, with the speed of 5 DEG C/min under atmosphere of inert gases
Rate is heated to 800 DEG C, 800 DEG C at a temperature of keep the temperature 1h, then be heated to 1200 DEG C with the rate of 5 DEG C/min, and at 1200 DEG C
At a temperature of keep 5h after cooled to room temperature, obtain the carbon product of Heteroatom doping；In this step, by inert gas atmosphere
It is heat-treated in the tube furnace enclosed, avoids oxidation, decarburization；It is obtained under the conditions of Fractional Heat-treatment described in this step miscellaneous
Atom doped carbon product may act as Carbon negative electrode material of sodium ion battery, and rate capability is more excellent, and cyclical stability is preferable.
(4) Heteroatom doping carbon product obtained in previous step is placed in Buchner funnel and rinses 3-5 with deionized water
It is secondary, it is then dry with 100 DEG C of temperature in vacuum drying oven, obtain the carbon negative pole material of high-content Heteroatom doping.This step
Middle progress deionized water flushing is the inorganic ion in order to adhere on the carbon product of Heteroatom doping obtained in previous step
Removal, obtains the carbon product of more pure Heteroatom doping, using it as Carbon negative electrode material of sodium ion battery, rate capability
More excellent, cyclical stability is more preferable.
Referring to table 1, show the Carbon anode material for the high-content Heteroatom doping that the preparation method obtains by electro-chemical test
Material, the capacity retention ratio at 4C are 103.5%, and capacity retention ratio is 94.6% after 1000 circulations at 1C, at 2C
Capacity retention ratio is 93.8% after 1000 circulations.As it can be seen that the carbon for the high-content Heteroatom doping that the preparation method obtains is negative
Pole material shows good rate capability, has excellent long-term cycle stability.
The carbon negative pole material being prepared in the various embodiments described above is fabricated to the chemical property after battery referring to table 1:
Table 1: the carbon negative pole material of each embodiment preparation is fabricated to the chemical property contrast table after battery
Carbon negative electrode material of sodium ion battery provided by the invention and preparation method thereof, wherein Carbon negative electrode material of sodium ion battery
Preparation method, original biomass carbon source is dissolved with containing the heteroatomic ionic liquid such as nitrogen, phosphorus, boron, then dissolved matter is existed
High-content Heteroatom doping carbon negative pole material is prepared in roasting under high temperature.By containing the heteroatomic ionic liquids such as nitrogen, phosphorus, boron
Body dissolves original biomass carbon source, is allowed to be heated more evenly in pyrolysis；On the other hand, nitrogen, phosphorus, boron etc. are contained in ionic liquid
Hetero atom can largely improve content of heteroatoms in material.The sodium-ion battery carbon prepared by this method is negative
Pole material is doped with the hetero atom of higher amount, makes it have higher high rate performance and stable circulation performance.
The above description is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art
For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification,
Equivalent replacement, improvement etc., should be included within scope of the presently claimed invention.
Claims (10)
1. a kind of preparation method of Carbon negative electrode material of sodium ion battery, which is characterized in that include at least following steps:
Original biomass carbon source is added to the ionic liquid containing any one or more element in N, P, S and B by the amount of setting
It in the reaction flask of body, is heated to the original biomass carbon source and is dissolved completely in the ionic liquid, obtain having dissolved mixed
Close object；
The mixture is transferred in high temperature process furnances, the temperature of setting is heated under atmosphere of inert gases and keeps 5-
8h, cooled to room temperature obtain the carbon product of Heteroatom doping, electric using the carbon product of the Heteroatom doping as sodium ion
Pond carbon negative pole material.
2. the preparation method of Carbon negative electrode material of sodium ion battery according to claim 1, which is characterized in that described by setting
Amount original biomass carbon source is added to the reaction flask containing the ionic liquid of any one or more element in N, P, S and B
In, it is heated to the step of original biomass carbon source is dissolved completely in the ionic liquid, obtains the mixture dissolved
Before, comprising:
By the biomass mechanical grinding dried at powder, the powder is placed on drying in vacuum drying oven, obtains the initial life
Substance carbon source.
3. the preparation method of Carbon negative electrode material of sodium ion battery according to claim 2, which is characterized in that it is described will be described
Powder is placed in step dry in vacuum drying oven, and the drying temperature range of the vacuum drying oven is 80-120 DEG C, drying time
Range is 12-48 hours.
4. the preparation method of Carbon negative electrode material of sodium ion battery according to claim 2, which is characterized in that the biomass
For peanut shell, rice husk, corncob and soybean stalk one of or it is a variety of.
5. the preparation method of Carbon negative electrode material of sodium ion battery according to claim 1, which is characterized in that it is described will be described
Mixture is transferred in high temperature process furnances, and the temperature of setting is heated under atmosphere of inert gases and keeps 5-8h, natural cooling
To room temperature, after the step of obtaining the carbon product of Heteroatom doping, comprising:
The carbon product of the Heteroatom doping is rinsed 3-5 times in Buchner funnel with deionized water, the sample obtained after washing
It is sufficiently dry in vacuum drying oven.
6. the preparation method of Carbon negative electrode material of sodium ion battery according to claim 1, which is characterized in that the ionic liquid
Body includes one or more of borate, phosphate and quaternary ammonium salt.
7. the preparation method of Carbon negative electrode material of sodium ion battery according to claim 6, which is characterized in that the ionic liquid
Body is 1- ethyl-3-methylimidazole tetrafluoroborate.
8. the preparation method of Carbon negative electrode material of sodium ion battery according to claim 1, which is characterized in that it is described will be described
In the step of mixture is transferred in high temperature process furnances, and the temperature of setting is heated under atmosphere of inert gases and keeps 5-8h,
The inert gas includes nitrogen and/or helium, and the rate of gas is 5L/min-10L/min.
9. the preparation method of Carbon negative electrode material of sodium ion battery according to claim 1, which is characterized in that it is described will be described
In the step of mixture is transferred in high temperature process furnances, and the temperature of setting is heated under atmosphere of inert gases and keeps 5-8h,
800 DEG C are heated to the rate of 5 DEG C -10 DEG C/min first, is heated to after 800 DEG C of holding 1h, then with the rate of 5 DEG C/min
Any temperature in 1200 DEG C -1500 DEG C of temperature range, and any temperature in 1200 DEG C -1500 DEG C of the temperature range
Degree is lower to keep 5h.
10. a kind of Carbon negative electrode material of sodium ion battery, which is characterized in that the Carbon negative electrode material of sodium ion battery is wanted by right
The preparation method of Carbon negative electrode material of sodium ion battery described in any one of 1-9 is asked to prepare gained.
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| CN113745509A (en) * | 2021-08-09 | 2021-12-03 | 华侨大学 | Phosphorus-nitrogen doped biomass hard carbon material and preparation method and application thereof |
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| CN108649224A (en) * | 2018-04-28 | 2018-10-12 | 南京林业大学 | Method, negative material and the battery of lithium ion battery negative material are prepared based on biological material |
| CN109004199A (en) * | 2018-08-01 | 2018-12-14 | 北京理工大学 | A kind of preparation method of sodium-ion battery cathode biomass hard carbon material |
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| CN107673348A (en) * | 2017-09-30 | 2018-02-09 | 青岛海澄知识产权事务有限公司 | A kind of biomass-based porous agraphitic carbon nanosphere sodium-ion battery |
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