CN109888237A - A kind of anode material of lithium-ion battery and preparation method thereof - Google Patents
A kind of anode material of lithium-ion battery and preparation method thereof Download PDFInfo
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- CN109888237A CN109888237A CN201910173315.9A CN201910173315A CN109888237A CN 109888237 A CN109888237 A CN 109888237A CN 201910173315 A CN201910173315 A CN 201910173315A CN 109888237 A CN109888237 A CN 109888237A
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Abstract
The invention belongs to the technical field of sodium-ion battery, it is specifically related to a kind of anode material of lithium-ion battery and preparation method thereof.The negative electrode material is iron-based selenides FeSe2@C.The negative electrode material has the hollow core-shell structure of controlledly synthesis and stablizes pattern, can contact for electrolyte and provide high-specific surface area, can shorten sodium ion diffusion length, and inhibit the expansion of material in charge and discharge process.Volume expansion of the anode material of lithium-ion battery of prior art preparation in charge and discharge process is overcome, the stability of battery is effectively increased, improves the cycle performance and coulombic efficiency of sodium-ion battery.
Description
Technical field
The invention belongs to the technical field of sodium-ion battery, it is specifically related to a kind of anode material of lithium-ion battery and its system
Preparation Method.
Background technique
With the demand of extensive energy storage device rapid growth, various electrochemical energy converting systems include lithium ion battery
(LIB), supercapacitor and metal-air battery have been found, wherein in all battery systems, lithium ion battery by
For many years, but there is lithium metals to be unevenly distributed the problems such as uniform at high price in the earth for business reference.Sodium ion electricity in recent years
Pond due to it is cheap and widely distributed on earth the advantages that cause the interest of researcher, but graphite is as sodium ion
Cell negative electrode material is restricted, and is primarily due to compared with lithium ion, and sodium ion radius is much bigger, therefore explores sodium ion
Cell negative electrode material is completely important.
Recently, transition metal selenides is received due to high theoretical capacity, good chemical stability and environment friendly
Extensive concern, all these features make them become being preferably selected for anode material of lithium-ion battery.However metallic selenium
Compound still suffers from some critically important challenges, for example volume expansion occurs in charge and discharge process, results in electrode material
Dusting；The intrinsic low electric conductivity of metal selenide is also still one and limits its main barrier applied in sodium-ion battery
Hinder.
Summary of the invention
It is an object of the invention to send out in charge and discharge process for existing sodium-ion battery metal selenide negative electrode material
The problem of raw volume expansion and low electric conductivity and provide a kind of anode material of lithium-ion battery and preparation method thereof, the cathode material
Expect that there is the hollow core-shell structure of controlledly synthesis and stablize pattern, can be contacted for electrolyte and high-specific surface area is provided, can contracted
Short sodium ion diffusion length, and in charge and discharge process inhibit material expansion.Overcome the sodium ion of prior art preparation
Volume expansion of the cell negative electrode material in charge and discharge process effectively increases the stability of battery, improves sodium-ion battery
Cycle performance and coulombic efficiency.
The technical solution of the present invention is as follows: a kind of anode material of lithium-ion battery is iron-based selenides FeSe2@C。
The preparation method of the anode material of lithium-ion battery, first synthesis iron base metal framework presoma Fe-MIL-
88A, so
Ferrous metals frame precursor Fe-MIL-88A is subjected to dopamine cladding, then high-temperature calcination under an inert atmosphere afterwards, is connect
Carry out the selective etch of hydrochloric acid, carry out high temperature selenizing with selenium powder after etching and iron-based selenides FeSe be prepared2@C。
The preparation method of the anode material of lithium-ion battery, comprising the following steps:
(1) it the preparation of ferrous metals frame precursor Fe-MIL-88A: measures DMF and sets in a round bottom flask, Fe is then added
(NO3)3 .9H2O and fumaric acid are stirred 30min；It is transferred in 110 DEG C of oil bath pan after mixing evenly and carries out reaction 1h, instead
It is respectively washed 3 times after answering with DMF and methanol, is dried for standby in 70 DEG C of baking oven；
(2) Fe is prepared2O3@PDA: step (1) is prepared into resulting ferrous metals frame precursor Fe-MIL-88A and dopamine
Being added to pH value is 8.5, stirs 6h in the buffer that concentration is 10mmol/L；Then the centrifugation for being 10000 revs/min in revolving speed
Product is centrifuged and collected under machine, is respectively washed 3 times using deionized water and ethyl alcohol, is dried for standby in 70 DEG C of baking oven；
(3) Fe is prepared2O3@C: by step (2) resulting Fe2O3@PDA carries out calcining 2h in inert gas under the conditions of 500 DEG C,
Calcining terminate be placed on concentration be 2mol/L hydrochloric acid in is stirred 1~6h, then revolving speed be 10000 revs/min from
Product is centrifuged and collected under scheming, is respectively washed 3 times using deionized water and ethyl alcohol, is dried for standby in 70 DEG C of baking oven；
(4) FeSe is prepared2@C: by step (3) resulting Fe2O3@C and selenium powder are put into porcelain boat, then 400 DEG C in inert gas
Under the conditions of carry out calcining 2h, be cooled to room temperature to get FeSe2@C-material.
DMF is 8mL, Fe (NO in the step (1)3)3 .9H2O is 0.16g, fumaric acid 0.042g.
Ferrous metals frame precursor Fe-MIL-88A in mass ratio in the step (2): dopamine is 1:0.5~1.
According to mass ratio Fe in the step (4)2O3@C: selenium powder 1:2.
Buffer is Tris buffer in the step (2).
The invention has the benefit that present invention synthesis iron base metal framework presoma Fe-MIL-88A first, then will
Ferrous metals frame precursor Fe-MIL-88A carries out dopamine cladding, then high-temperature calcination under an inert atmosphere, then carries out salt
The selective etch of acid carries out high temperature selenizing with selenium powder after etching and the iron-based selenides with hollow core-shell structure is prepared
FeSe2@C, wherein prepared FeSe2The shape of@C be " gumbo " shape, 0.5~1.5 μm of length, diameter range be 200~
300nm.It is found through experiments that, the selection of the dopamine dosage and etch period is to formation hollow nucleocapsid knot of the present invention
Structure plays key or even decisive role, when the ratio of dopamine dosage and ferrous metals frame precursor Fe-MIL-88A
When for 1:1, carbon-coating with a thickness of 200nm.From transmission electron microscope as can be seen that when etch period is 3h, Fe2O3Partial size can subtract
Few 100nm or so；When etch period is 6h, Fe2O3Partial size can be smaller, thus formed a hollow core-shell structure.
The product is applied on anode material of lithium-ion battery and is had the advantage that
1, the ferrous metals frame precursor Fe-MIL-88A that synthesizes of the present invention has ultra-high surface area and orderly adjustable porous
Structure, so that aperture is adjustable and can functional modification；Porous structure can provide more active sites for battery, shorten ion
Diffusion length is conducive to the progress of cell electrochemical reaction.
2, one layer of dopamine is wrapped up in the outside of ferrous metals frame precursor Fe-MIL-88A, is forged in inert gas high temperature
Will form carbon-coating during burning, the carbon-coating is able to suppress the volume expansion of material during battery charging and discharging, thus
Improve the stable circulation performance of battery.Furthermore the electric conductivity of material can be enhanced in carbon-coating, can also be improved the specific capacity of battery.
3, due to rationally designing hydrochloric acid selective etch Fe2O3, by the control to etch period, prepare in described
Empty core-shell structure, progress 1h, 3h and 6h etching it was found that, being continuously increased with etch period, Fe2O3Stick
Length and diameter is steadily decreasing, and eventually forms carbon-coating package Fe2O3The hollow core-shell structure of stick.The structure can provide volume
Outer cushion space and stress reduces bring volume expansion in charge and discharge process, has to sodium-ion battery cycle performance is improved
Critically important meaning.
4. the advantages of coating dopamine essentially consists in Fe-base compound can be combined well with the functional group on dopamine surface,
Enable carbon-coating to be uniformly coated on the surface of ferrous metals frame so that hydrochloric acid selective etch obtain it is more uniform,
And process control, meanwhile, the carbon-coating of cladding, which also helps, inhibits battery bring volume expansion in charge and discharge process.
In conclusion the iron-based selenides FeSe that the present invention prepares2@C is as negative electrode material in sodium-ion battery application
In the process, hollow core-shell structure has been rationally designed, then has coated one layer of dopamine on surface, by high-temperature calcination dopamine has been turned
It is melted into agraphitic carbon, the electric conductivity of material is enhanced, significantly improves the cycle performance of sodium-ion battery, improve the appearance of battery
Amount and service life, realize industrialized to sodium-ion battery have positive meaning.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture that embodiment 1 prepares gained ferrous metals frame precursor Fe-MIL-88A.
Fig. 2 is that embodiment 1 prepares gained FeSe2The electron scanning micrograph of@C.
Fig. 3 is that embodiment 1 prepares gained FeSe2The XRD diagram of@C.
Fig. 4 is that embodiment 1 prepares gained FeSe2The transmission electron microscope picture of@C.
Fig. 5 is FeSe prepared by embodiment 1-32@C is applied to sodium ion electricity respectively as anode material of lithium-ion battery
High rate performance figure in pond.As seen from Figure 5, the battery of prepared material specific capacity under different multiplying powers is all very high, works as electricity
Current density can also be maintained at 500mAh/g when returning to 0.2A/g.
Specific embodiment
Below by embodiment, the present invention is described in detail.
Wherein involved raw material pass through Shanghai Mike's woods reagent Co., Ltd and are obtained.
Embodiment 1
The anode material of lithium-ion battery is iron-based selenides FeSe2@C。
The preparation method of the anode material of lithium-ion battery, comprising the following steps:
(1) preparation of ferrous metals frame precursor Fe-MIL-88A: 8mL DMF(dimethylformamide is measured) it is placed in round bottom burning
In bottle, 0.16g Fe (NO is then added3)3 .9H2O and 0.042g fumaric acid is stirred 30min；It is transferred to after mixing evenly
Reaction 1h is carried out in 110 DEG C of oil bath pan, is respectively washed 3 times, is dried in 70 DEG C of baking oven standby with DMF and methanol after reaction
With；
(2) Fe is prepared2O3@PDA(p-phenylenediamine): step (1) is prepared into resulting ferrous metals frame precursor Fe-MIL-
It is 8.5 that 88A and dopamine, which are added to pH value, 6h is stirred in the Tris buffer that concentration is 10mmol/L, wherein iron in mass ratio
Base Metal frame precursor Fe-MIL-88A: dopamine 1:1；Then revolving speed be 10000 revs/min of centrifuge carry out from
The heart simultaneously collects product, is respectively washed 3 times using deionized water and ethyl alcohol, is finally dried for standby in 70 DEG C of baking oven；
(3) Fe is prepared2O3@C: by step (2) resulting Fe2O3@PDA carries out calcining 2h in argon atmosphere under the conditions of 500 DEG C,
Calcining terminate be placed on 20mL concentration be 2mol/L hydrochloric acid in is stirred 6h, then revolving speed be 10000 revs/min from
Scheming is centrifuged and is collected product, is respectively washed 3 times using deionized water and ethyl alcohol, finally is carried out drying in 70 DEG C of baking oven standby
With；
(4) FeSe is prepared2@C: by step (3) resulting Fe2O3@C and selenium powder are put into porcelain boat according to mass ratio 1:2, then in argon
Calcining 2h is carried out in gas atmosphere under the conditions of 400 DEG C, is cooled to room temperature to get FeSe2@C-material.
As seen from Figure 1, the presoma pattern being prepared is " gumbo " shape, and surface smoother, corner angle are clearly more demarcated,
Uniform in size, length is 0.5~1.5 μm, and diameter range is 200~300nm.
From Figure 2 it can be seen that iron-based selenides is successfully prepared, compared with presoma, the sample surfaces after selenizing have the east of a shape
West, this be in selenidation process caused by, the selenides of formation is formed on surface.
As can be seen from Figure 3 come, the prepared FeSe come out2@C and standard PDF card completely coincide, it was demonstrated that synthesis
Required for material out is exactly us.
As can be seen from Figure 4 prepared FeSe2@C is hollow core-shell structure, and carbon-coating is wrapped in FeSe2, illustrate to prepare
Sample it is successful.
Embodiment 2
The preparation method of the anode material of lithium-ion battery, comprising the following steps:
(1) preparation of ferrous metals frame precursor Fe-MIL-88A: 8mL DMF(dimethylformamide is measured) it is placed in round bottom burning
In bottle, 0.16g Fe (NO is then added3)3 .9H2O and 0.042g fumaric acid is stirred 30min；It is transferred to after mixing evenly
Reaction 1h is carried out in 110 DEG C of oil bath pan, is respectively washed 3 times, is dried in 70 DEG C of baking oven standby with DMF and methanol after reaction
With；
(2) Fe is prepared2O3@PDA(p-phenylenediamine): step (1) is prepared into resulting ferrous metals frame precursor Fe-MIL-
It is 8.5 that 88A and dopamine, which are added to pH value, 6h is stirred in the Tris buffer that concentration is 10mmol/L, wherein iron in mass ratio
Base Metal frame precursor Fe-MIL-88A: dopamine 1:1；Then revolving speed be 10000 revs/min of centrifuge carry out from
The heart simultaneously collects product, is respectively washed 3 times using deionized water and ethyl alcohol, is finally dried for standby in 70 DEG C of baking oven；
(3) Fe is prepared2O3@C: by step (2) resulting Fe2O3@PDA carries out calcining 2h in argon atmosphere under the conditions of 500 DEG C,
Calcining terminate be placed on 20mL concentration be 2mol/L hydrochloric acid in is stirred 3h, then revolving speed be 10000 revs/min from
Scheming is centrifuged and is collected product, is respectively washed 3 times using deionized water and ethyl alcohol, finally is carried out drying in 70 DEG C of baking oven standby
With；
(4) FeSe is prepared2@C: by step (3) resulting Fe2O3@C and selenium powder are put into porcelain boat according to mass ratio 1:2, then in argon
Calcining 2h is carried out in gas atmosphere under the conditions of 400 DEG C, is cooled to room temperature to get FeSe2@C-material.
Embodiment 3
The preparation method of the anode material of lithium-ion battery, comprising the following steps:
(1) preparation of ferrous metals frame precursor Fe-MIL-88A: 8mL DMF(dimethylformamide is measured) it is placed in round bottom burning
In bottle, 0.16g Fe (NO is then added3)3 .9H2O and 0.042g fumaric acid is stirred 30min；It is transferred to after mixing evenly
Reaction 1h is carried out in 110 DEG C of oil bath pan, is washed respectively wash 3 times with DMF and methanol after reaction, dried in 70 DEG C of baking oven standby
With；
(2) Fe is prepared2O3@PDA(p-phenylenediamine): step (1) is prepared into resulting ferrous metals frame precursor Fe-MIL-
It is 8.5 that 88A and dopamine, which are added to pH value, 6h is stirred in the Tris buffer that concentration is 10mmol/L, wherein iron in mass ratio
Base Metal frame precursor Fe-MIL-88A: dopamine 1:0.5；Then it is carried out in the centrifuge that revolving speed is 10000 revs/min
It is centrifuged and is collected product, is respectively washed 3 times using deionized water and ethyl alcohol, is finally dried for standby in 70 DEG C of baking oven；
(3) Fe is prepared2O3@C: by step (2) resulting Fe2O3@PDA carries out calcining 2h in argon atmosphere under the conditions of 500 DEG C,
Calcining terminate be placed on 20mL concentration be 2mol/L hydrochloric acid in is stirred 1h, then revolving speed be 10000 revs/min from
Scheming is centrifuged and is collected product, is respectively washed 3 times using deionized water and ethyl alcohol, finally is carried out drying in 70 DEG C of baking oven standby
With；
(4) FeSe is prepared2@C: by step (3) resulting Fe2O3@C and selenium powder are put into porcelain boat according to mass ratio 1:2, then in argon
Calcining 2h is carried out in gas atmosphere under the conditions of 400 DEG C, is cooled to room temperature to get FeSe2@C-material.
Claims (7)
1. a kind of anode material of lithium-ion battery, which is characterized in that the negative electrode material is iron-based selenides FeSe2@C。
2. a kind of preparation method of anode material of lithium-ion battery described in claim 1, which is characterized in that synthesis iron base gold first
Belong to frame precursor Fe-MIL-88A, then by ferrous metals frame precursor Fe-MIL-88A progress dopamine cladding, then
High-temperature calcination under inert atmosphere then carries out the selective etch of hydrochloric acid, carries out high temperature selenizing with selenium powder after etching and be prepared
Iron-based selenides FeSe2@C。
3. the preparation method of anode material of lithium-ion battery according to claim 2, which comprises the following steps:
(1) it the preparation of ferrous metals frame precursor Fe-MIL-88A: measures DMF and sets in a round bottom flask, Fe is then added
(NO3)3 .9H2O and fumaric acid are stirred 30min；It is transferred in 110 DEG C of oil bath pan after mixing evenly and carries out reaction 1h, instead
It is respectively washed 3 times after answering with DMF and methanol, is dried for standby in 70 DEG C of baking oven；
(2) Fe is prepared2O3@PDA: step (1) is prepared into resulting ferrous metals frame precursor Fe-MIL-88A and dopamine adds
Entering to pH value is 8.5, stirs 6h in the buffer that concentration is 10mmol/L；Then the centrifuge for being 10000 revs/min in revolving speed
Under be centrifuged and collected product, respectively washed 3 times using deionized water and ethyl alcohol, be dried for standby in 70 DEG C of baking oven；
(3) Fe is prepared2O3@C: by step (2) resulting Fe2O3@PDA carries out calcining 2h in inert gas under the conditions of 500 DEG C, forge
Sintering beam is placed in the hydrochloric acid that concentration is 2mol/L and is stirred 1~6h, the centrifugation for being then 10000 revs/min in revolving speed
Product is centrifuged and collected under machine, is respectively washed 3 times using deionized water and ethyl alcohol, is dried for standby in 70 DEG C of baking oven；
(4) FeSe is prepared2@C: by step (3) resulting Fe2O3@C and selenium powder are put into porcelain boat, then 400 DEG C in inert gas
Under the conditions of carry out calcining 2h, be cooled to room temperature to get FeSe2@C-material.
4. the preparation method of anode material of lithium-ion battery according to claim 3, which is characterized in that in the step (1)
DMF is 8mL, Fe (NO3)3 .9H2O is 0.16g, fumaric acid 0.042g.
5. the preparation method of anode material of lithium-ion battery according to claim 4, which is characterized in that in the step (2)
Ferrous metals frame precursor Fe-MIL-88A in mass ratio: dopamine is 1:0.5~1.
6. the preparation method of anode material of lithium-ion battery according to claim 5, which is characterized in that in the step (4)
According to mass ratio Fe2O3@C: selenium powder 1:2.
7. the preparation method of anode material of lithium-ion battery according to claim 3, which is characterized in that in the step (2)
Buffer is Tris buffer.
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|---|---|---|---|---|
| CN110459766A (en) * | 2019-07-11 | 2019-11-15 | 华南师范大学 | Micro- cube of composite material, electrode slice, sodium-ion battery with hierarchical structure and preparation method thereof |
| CN110534740A (en) * | 2019-08-25 | 2019-12-03 | 湘潭大学 | A kind of cellular porous carbon FeSe of compound N doping2The preparation method and product of/C |
| CN111092211A (en) * | 2019-12-31 | 2020-05-01 | 青岛科技大学 | Micro-cavity liquid state vulcanization preparation method of carbon and sulfide composite electrode material |
| CN111554874A (en) * | 2020-06-18 | 2020-08-18 | 电子科技大学 | FeS2-xSexSolid solution cathode material and preparation method thereof |
| CN111900385A (en) * | 2020-07-29 | 2020-11-06 | 肇庆市华师大光电产业研究院 | Novel negative electrode material of potassium ion battery and preparation method thereof |
| CN113511630A (en) * | 2021-07-28 | 2021-10-19 | 王秀丽 | Hydrogen chloride production equipment |
| CN113764659A (en) * | 2021-09-16 | 2021-12-07 | 河北工业大学 | Preparation method and application of iron-based selenide serving as negative electrode material of sodium-ion battery |
| CN115000361A (en) * | 2022-04-25 | 2022-09-02 | 齐鲁工业大学 | Fe 3 Se 4 Graphene sodium battery negative electrode material and preparation method thereof |
| CN115207344A (en) * | 2021-04-12 | 2022-10-18 | 南京工业大学 | Fe x Se y Preparation of @ CN composite material and electrochemical energy storage application thereof |
| CN115632112A (en) * | 2022-06-28 | 2023-01-20 | 四川大学 | Phosphorus-doped FeS 2 @ C negative electrode material and preparation and application thereof |
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| CN110459766A (en) * | 2019-07-11 | 2019-11-15 | 华南师范大学 | Micro- cube of composite material, electrode slice, sodium-ion battery with hierarchical structure and preparation method thereof |
| CN110534740A (en) * | 2019-08-25 | 2019-12-03 | 湘潭大学 | A kind of cellular porous carbon FeSe of compound N doping2The preparation method and product of/C |
| CN111092211A (en) * | 2019-12-31 | 2020-05-01 | 青岛科技大学 | Micro-cavity liquid state vulcanization preparation method of carbon and sulfide composite electrode material |
| CN111554874A (en) * | 2020-06-18 | 2020-08-18 | 电子科技大学 | FeS2-xSexSolid solution cathode material and preparation method thereof |
| CN111900385A (en) * | 2020-07-29 | 2020-11-06 | 肇庆市华师大光电产业研究院 | Novel negative electrode material of potassium ion battery and preparation method thereof |
| CN111900385B (en) * | 2020-07-29 | 2022-04-26 | 肇庆市华师大光电产业研究院 | Novel negative electrode material of potassium ion battery and preparation method thereof |
| CN115207344A (en) * | 2021-04-12 | 2022-10-18 | 南京工业大学 | Fe x Se y Preparation of @ CN composite material and electrochemical energy storage application thereof |
| CN113511630A (en) * | 2021-07-28 | 2021-10-19 | 王秀丽 | Hydrogen chloride production equipment |
| CN113764659A (en) * | 2021-09-16 | 2021-12-07 | 河北工业大学 | Preparation method and application of iron-based selenide serving as negative electrode material of sodium-ion battery |
| CN115000361A (en) * | 2022-04-25 | 2022-09-02 | 齐鲁工业大学 | Fe 3 Se 4 Graphene sodium battery negative electrode material and preparation method thereof |
| CN115632112A (en) * | 2022-06-28 | 2023-01-20 | 四川大学 | Phosphorus-doped FeS 2 @ C negative electrode material and preparation and application thereof |
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