CN106654221B - Three-dimensional porous carbon coating selenizing Zinc material and preparation method thereof for negative electrode of lithium ion battery - Google Patents
Three-dimensional porous carbon coating selenizing Zinc material and preparation method thereof for negative electrode of lithium ion battery Download PDFInfo
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- CN106654221B CN106654221B CN201710026565.0A CN201710026565A CN106654221B CN 106654221 B CN106654221 B CN 106654221B CN 201710026565 A CN201710026565 A CN 201710026565A CN 106654221 B CN106654221 B CN 106654221B
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- 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
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Abstract
The invention belongs to material, energy technology field, specially a kind of three-dimensional porous carbon coating selenizing Zinc material and preparation method thereof for negative electrode of lithium ion battery.Specifically it regard zinc-base zeolite imidazole ester metal-organic framework materials (ZIF-8) as presoma or template; it is sintered certain time at high temperature with selenium powder under the conditions of inert atmosphere protection; by the synchronous selenizing carried out and carbonisation, carbon-coated zinc selenide composite material is finally prepared.Composite process prepared by the present invention realizes the effective compound of zinc selenide and graphitic carbon, strong interface coupling effect is formd between each constituent, and it can be effectively relieved and inhibit Volumetric expansion of the selenizing Zinc material in charge and discharge process, improve the electric conductivity of material, therefore when the composite material is used as lithium ion battery negative material, very high specific capacity and excellent cyclical stability and high rate performance are had both.Preparation process of the invention is simple, and preparation condition is moderate, low in cost.
Description
Technical field
The invention belongs to materials, energy technology field, and in particular to a kind of for the three-dimensional porous of negative electrode of lithium ion battery
Carbon coating selenizing Zinc material and preparation method thereof.
Background technique
With the development of economy, the demand of the energy is also increasingly increased, people have had now been found that a variety of available
Clean energy resource, and develop energy conversion and memory technology is also particularly significant.Removable cycle charge-discharge battery is most extensive at present
Energy storage mode.Lithium ion battery is high with its energy density, has extended cycle life and environmentally friendly etc. advantage, wide
It is general to be applied to various portable electronic devices.With the increase of demand, people are higher and higher to the performance requirement of lithium ion battery,
How improving battery capacity, extending cycle life, improve high rate performance is the main target for studying lithium ion battery.Lithium-ion electric
Pond mainly includes battery case, negative electrode material, positive electrode, diaphragm and electrolyte, and the raising of performance depends primarily on positive and negative electrode
The raising of material property.
The cathode for the lithium ion battery commercially produced at present is mainly graphite material.But the reason of graphite-based negative electrode material
There was only 372mAh/g by capacity, has been unable to meet people for the demand of high capacity.And the higher silica-base material of theoretical capacity and
Transition metal oxide due to during removal lithium embedded enormousness change, and poorly conductive leads to low service life, easy decaying, circulation
Stability is poor.Therefore, it is badly in need of finding while meeting the lithium ion battery negative material of capacity height and good cycling stability.
Elemental selenium theoretical specific capacity with higher (weight ratio capacity 675mAh/g, volume and capacity ratio 3268mAh/
G), high conductivity (10-5S/cm is much higher than sulphur 10-30S/cm it) attracts extensive attention.Amine et al.
(J.Am.Chem.Soc.2012,134,4505-4508) first reported a kind of preparation method of lithium-selenium cell, but due to
Granules of selenium size is too big, can not be effectively compound, leads to capacity rapid decay in cyclic process.Guo et al.
(Angew.Chem.Int.ed.2013,52,8363-8367) prepares cyclic annular or chain selenium molecule using melting-diffusion method,
Its coulombic efficiency is close to 100%, but capacity only has 657mAh/g.
The study found that can effectively buffer the volume change during removal lithium embedded using selenium progress alloying, improve circulation
Performance.In recent years, metal selenide is widely used in lithium ion battery negative material.Zhang et al. (ELECTROCHIMICA
ACTA 2016,209,423-429) a kind of 1-dimention nano threadiness SnSe/C composite negative pole material is reported, in 200mA/g
Multiplying power under the capacity of initial 840mAh/g can be kept after 100 circulations.Although high rate performance is more prominent, its
Capacity still has to be hoisted.
Summary of the invention
The shortcomings that in order to overcome above-mentioned technology that can not meet high capacity, long-life and excellent high rate performance simultaneously, the present invention
Provide a kind of economical and efficient, performance it is stable, can industrialized production three-dimensional porous carbon coating selenizing Zinc material and its preparation side
Method and application in field of lithium ion battery.
The preparation method of the porous carbon coating zinc selenide material of three-dimensional polyhedron provided by the invention, is had using zinc-base metal
Machine frame (ZIF-8) carries out selenylation reaction with selenium powder using hydrogen-argon-mixed as protective atmosphere as template at high temperature,
It is prepared in situ to obtain three-dimensional porous carbon coating selenizing Zinc material.In the material of preparation, by zinc selenide quantum dot in porous carbon,
With meso-hole structure and higher specific surface area, and completely maintain very much the polyhedron pattern of ZIF-8, as lithium from
During sub- cell negative electrode material use, excellent performance is shown.
The preparation method of the porous carbon coating zinc selenide material of three-dimensional polyhedron of the present invention, specific steps are as follows:
(1) 1.35-1.66 grams of zinc nitrate hexahydrate and 1.45-1.85 grams of 2-methylimidazole are weighed, is dissolved in 15-35 milli respectively
In the methanol solution risen, then stirring and dissolving is poured into 2-methylimidazole solution in zinc nitrate solution；It mixes to uniformly
(5-10 minutes) stand 18-24 hours at room temperature, product are centrifugated, is cleaned 2-4 times with ethanol solution, is finally placed in
In 55-80 degrees Celsius of drying box, products therefrom is polyhedron shape ZIF-8；Product is white, mostly granatohedron shape
Looks, particle size are mainly distributed between 600 to 900 nanometers；
(2) 100 to 300 milligrams of ZIF-8 and 100 to 300 milligrams three-dimensional porous carbon coating selenizing Zinc material and preparation: are weighed
Selenium powder be respectively placed in the both ends of porcelain boat, porcelain boat is put into tube furnace, be passed through it is hydrogen-argon-mixed, with 1-3 centigrade per minute
Heating rate be heated to 400 to 600 degrees Celsius, at this temperature keep the temperature 2 to 4 hours to get arrive three-dimensional porous carbon coating
Selenizing Zinc material.
Three-dimensional porous selenizing Zinc material prepared by the present invention have microcellular structure and higher specific surface area, can be used for lithium from
Sub- battery cathode active material, material capacity with higher, and three-dimensional porous structure can effectively buffer removal lithium embedded mistake
Volume change in journey improves cycle performance.Anode is done with lithium piece, microporous polypropylene membrane (Celgard 2400) makees diaphragm, adopts
With business electrolyte (LiPF6For electrolyte, EC and DMC is solvent and volume ratio is 1:1), be assembled into CR2032 type battery progress
Test.
Present invention has an advantage that (1) three-dimensional porous selenizing Zinc material maintains the three-dimensional multi-panel of original ZIF-8 well
Bodily form looks, and there is microcellular structure and biggish specific surface area, it shows to be substantially better than at present in fields such as lithium ion batteries
The capacity and cycle performance for the selenizing Zinc material known；(2) raw material relate only to zinc nitrate hexahydrate, 2-methylimidazole, selenium powder and
The common agents such as methanol, ethyl alcohol, safe and non-toxic, low in cost, product purity is high；(3) three-dimensional porous selenium is prepared using one-step method
Change Zinc material, simple process is easy to industrialized production；(4) this method has good applicability, can be extended to other metals
In the preparation method of selenides.
In conclusion the present invention provides a kind of capacity high, stability and good cycle, easy to operate, safety is good,
The preparation method of three-dimensional porous selenizing Zinc material at low cost, high-efficient, easy to industrialized production.
Detailed description of the invention
Fig. 1 is scanning electron microscope (SEM) figure of three-dimensional porous selenizing Zinc material prepared by the embodiment of the present invention 1.
Fig. 2 is transmission electron microscope (TEM) figure of three-dimensional porous selenizing Zinc material prepared by the embodiment of the present invention 1.
Fig. 3 is the X-ray diffraction (XRD) figure of three-dimensional porous selenizing Zinc material prepared by the embodiment of the present invention 1.
Fig. 4 is specific surface area analysis (BET) figure of three-dimensional porous selenizing Zinc material prepared by the embodiment of the present invention 1.
Fig. 5 be the lithium that is prepared with three-dimensional porous zinc selenide material as cathode active material prepared by the embodiment of the present invention 1 from
The capacity curve of sub- battery.
Fig. 6 be the lithium that is prepared with three-dimensional porous zinc selenide material as cathode active material prepared by the embodiment of the present invention 1 from
The high rate performance curve of sub- battery.
Specific embodiment
For a further understanding of the present invention, below with reference to example and attached drawing, the present invention is further described.
Embodiment 1: three-dimensional porous carbon coating selenizing Zinc material and its preparation method and application, comprising the following steps:
(1) prepared by the ZIF-8 template with polyhedron pattern: weighing 1.45 grams of zinc nitrate hexahydrates and 1.66 grams of 2- methyl
Imidazoles is dissolved in respectively in 20 milliliters of methanol solution, and after dissolution to be mixed, 2-methylimidazole solution is poured into zinc nitrate solution
In；Stirring 5 minutes stands 24 hours at room temperature, product is centrifugated, is cleaned 4 times with ethanol solution, 55 is finally placed in and takes the photograph
In family name's degree drying box, products therefrom is polyhedron shape ZIF-8；Product is white, mostly granatohedron pattern, particle ruler
It is very little to be mainly distributed between 600 to 900 nanometers；
(2) it three-dimensional porous selenizing Zinc material and preparation: weighs 200 milligrams ZIF-8 and 200 milligram of selenium powder and is respectively placed in porcelain
The both ends of boat, porcelain boat is put into tube furnace, is passed through hydrogen-argon-mixed, is heated to 600 with the heating rate of 3 centigrade per minutes
Degree Celsius, 2 hours are kept the temperature at this temperature to get three-dimensional porous carbon coating selenizing Zinc material is arrived.
Three-dimensional porous carbon coating selenizing Zinc material is used as lithium ion battery negative pole active materials, anode is done with lithium piece, is gathered
Propylene microcellular film (Celgard 2400) makees diaphragm, using business electrolyte (LiPF6For electrolyte, EC and DMC are solvent and body
Product is than being 1:1), it is assembled into CR2032 type battery and is tested.Its pattern and characteristic are as shown in Fig. 1-Fig. 5.
Present invention has an advantage that (1) three-dimensional porous selenizing Zinc material maintains the three-dimensional multi-panel of original ZIF-8 well
Bodily form looks, and there is microcellular structure and biggish specific surface area, it shows to be substantially better than at present in fields such as lithium ion batteries
The capacity for the selenizing Zinc material known (Fig. 4 is recycled 500 times, capacity is maintained at 1134mAh/g under the current density of 600mA/g)
(Fig. 5, under 200,400,800,1600,3200,6400,12800mA/g current density, capacity is respectively with cycle performance
1162,1157,1127,1029,811,696, and 474 mAh/g)；(2) raw material relates only to zinc nitrate hexahydrate, diformazan
The common agents such as base imidazoles, selenium powder and methanol, ethyl alcohol, safe and non-toxic, low in cost, product purity is high；(3) one-step method system is used
Standby three-dimensional porous selenizing Zinc material, simple process are easy to industrialized production.
Embodiment 2: three-dimensional porous carbon coating selenizing Zinc material and its preparation method and application, comprising the following steps:
(1) prepared by the ZIF-8 template with polyhedron pattern: weighing 1.45 grams of zinc nitrate hexahydrates and 1.66 grams of 2- methyl
Imidazoles is dissolved in respectively in 20 milliliters of methanol solution, and after dissolution to be mixed, 2-methylimidazole solution is poured into zinc nitrate solution
In；Stirring 5 minutes stands 24 hours at room temperature, product is centrifugated, is cleaned 4 times with ethanol solution, 55 is finally placed in and takes the photograph
In family name's degree drying box, products therefrom is polyhedron shape ZIF-8；Product is white, mostly granatohedron pattern, particle ruler
It is very little to be mainly distributed between 600 to 900 nanometers；
(2) it three-dimensional porous selenizing Zinc material and preparation: weighs 200 milligrams ZIF-8 and 200 milligram of selenium powder and is respectively placed in porcelain
The both ends of boat, porcelain boat is put into tube furnace, is passed through hydrogen-argon-mixed, is heated to 500 with the heating rate of 3 centigrade per minutes
Degree Celsius, 2 hours are kept the temperature at this temperature to get three-dimensional porous carbon coating selenizing Zinc material is arrived.
Three-dimensional porous carbon coating selenizing Zinc material is used as lithium ion battery negative pole active materials, anode is done with lithium piece, is gathered
Propylene microcellular film (Celgard 2400) makees diaphragm, using business electrolyte (LiPF6For electrolyte, EC and DMC are solvent and body
Product is than being 1:1), it is assembled into CR2032 type battery and is tested.Its pattern and characteristic and embodiment 1 are similar.
Present invention has an advantage that (1) three-dimensional porous selenizing Zinc material maintains the three-dimensional multi-panel of original ZIF-8 well
Bodily form looks, and there is microcellular structure and biggish specific surface area, it shows to be substantially better than at present in fields such as lithium ion batteries
The capacity and cycle performance for the selenizing Zinc material known；(2) raw material relate only to zinc nitrate hexahydrate, methylimidazole, selenium powder and
The common agents such as methanol, ethyl alcohol, safe and non-toxic, low in cost, product purity is high；(3) three-dimensional porous selenium is prepared using one-step method
Change Zinc material, simple process is easy to industrialized production.
Claims (3)
1. a kind of preparation method of three-dimensional porous carbon coating selenizing Zinc material, which is characterized in that utilize zinc-base metal organic frame
(ZIF-8) it is used as template, using hydrogen-argon-mixed as protective atmosphere, carries out selenylation reaction at high temperature with selenium powder, it is in situ to make
It is standby to obtain three-dimensional porous carbon coating selenizing Zinc material；Specific steps are as follows:
(1) prepared by the ZIF-8 template with polyhedron pattern:
1.35-1.66 grams of zinc nitrate hexahydrate and 1.45-1.85 grams of 2-methylimidazole are weighed, is dissolved in 15-35 milliliters of first respectively
In alcoholic solution, then stirring and dissolving is poured into 2-methylimidazole solution in zinc nitrate solution；It mixes to uniformly, in room temperature
Lower standing 18-24 hours, product is centrifugated, is cleaned 2-4 times with ethanol solution, is finally placed in 55-80 degrees Celsius of drying box
In, products therefrom is polyhedron shape ZIF-8；Product is white, and mostly granatohedron pattern, particle size are mainly distributed
Between 600 to 900 nanometers；
(2) polyhedron shape selenizing Zinc material and preparation:
It weighs 100 to 300 milligrams of ZIF-8 and 100 to 300 milligrams of selenium powder is respectively placed in the both ends of porcelain boat, put porcelain boat into pipe
It in formula furnace, is passed through hydrogen-argon-mixed, is heated to 500-600 degrees Celsius with the heating rate of 1-3 centigrade per minute, in this temperature
Degree is lower to keep the temperature 2-4 hours to get three-dimensional porous carbon-coated zinc selenide quantum dot material is arrived.
2. the three-dimensional porous carbon-coated selenizing Zinc material that a kind of preparation method as described in claim 1 obtains.
3. it is a kind of by three-dimensional porous carbon-coated selenizing Zinc material as claimed in claim 2, as lithium ion cell electrode activity
The application of material.
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| CN111180725A (en) * | 2020-01-22 | 2020-05-19 | 河北大学 | Method for preparing aluminum battery anode material by utilizing MOF (metal organic framework) to induce metal selenide |
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| CN113912026B (en) * | 2021-09-13 | 2022-12-20 | 三峡大学 | Preparation method of double-carbon-modified zinc selenide layered multistage microspheres |
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| CN115064702B (en) * | 2022-07-22 | 2022-12-13 | 哈尔滨工业大学 | Sodium-philic 3D carbon current collector, preparation method and application thereof, and preparation method of non-negative solid sodium battery |
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