CN106654221A - Three-dimensional porous carbon-coated zinc selenide material for lithium ion battery anodes and preparation method of material - Google Patents
Three-dimensional porous carbon-coated zinc selenide material for lithium ion battery anodes and preparation method of material Download PDFInfo
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- CN106654221A CN106654221A CN201710026565.0A CN201710026565A CN106654221A CN 106654221 A CN106654221 A CN 106654221A CN 201710026565 A CN201710026565 A CN 201710026565A CN 106654221 A CN106654221 A CN 106654221A
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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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- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention belongs to the technical field of material and energy and particularly relates to three-dimensional porous carbon-coated zinc selenide material for lithium ion battery anodes and a preparation method of the material. The preparation method comprises the specific steps of sintering zinc-based zeolite imidazate metal organic framework material (ZIF-8) as a precursor or template with selenium powder under the protection of an inert atmosphere at high temperature for a certain time, and carrying out synchronous selenization and carbonization to finally prepare the carbon-coated zinc selenide composite material. The composite material prepared herein and the preparation method thereof provide effective composition of zinc selenide and graphite carbon, the component ingredients generate great interfacial coupling effect, volume expansion effect of the zinc selenide material during charging and discharging can be effectively relieved and inhibited, the conductivity of the material is improved, and accordingly the composite material has very high specific capacity and excellent cycle stability and rate performance when applied as lithium ion battery anode material. The preparation process is simple, the preparation conditions are mild, and the cost is low.
Description
Technical field
The invention belongs to material, energy technology field, and in particular to a kind of for the three-dimensional porous of lithium ion battery negative
Carbon coating selenizing Zinc material and preparation method thereof.
Background technology
With expanding economy, the demand of the energy is also increasingly increased, people have had now been found that various available
Clean energy resource, and development energy conversion and memory technology are also particularly significant.Removable cycle charge-discharge battery is most extensive at present
Energy storage mode.Lithium ion battery with its energy density it is high, have extended cycle life and the aspect such as environmentally friendly advantage, it is wide
It is general to be applied to various portable electric appts.With the increase of demand, performance requirement more and more higher of the people to 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 material, positive electrode, barrier film and electrolyte, and the raising of its performance depends primarily on positive and negative electrode
The raising of material property.
The negative pole of the lithium ion battery commercially produced at present is mainly graphite material.But the reason of graphite-based negative material
There was only 372mAh/g by capacity, demand of the people for high power capacity can not have been met.And the higher silica-base material of theoretical capacity and
Transition metal oxide causes low life-span, easy decay, circulation due to enormousness change, and poorly conductive during removal lithium embedded
Stability is poor.Therefore, it is badly in need of finds and meet simultaneously high and good cycling stability the lithium ion battery negative material of capacity.
Elemental selenium has higher theoretical specific capacity（Weight ratio capacity is 675mAh/g, and volume and capacity ratio is 3268mAh/
g）, high electrical conductivity（10-5S/cm, far above sulphur 10-30S/cm）Cause extensive concern.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, it is impossible to effectively compound, causes capacity rapid decay in cyclic process.Guo et al.
（Angew.Chem.Int.ed.2013,52,8363-8367）The selenium molecule of ring-type or chain is prepared using melting-diffusion method,
Its coulombic efficiency close 100%, but capacity only has 657mAh/g.
Research finds that carrying out alloying using selenium can effectively buffer Volume Changes during removal lithium embedded, 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 wire 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 projected, its
Capacity still has to be hoisted.
The content of the invention
In order to overcome the above-mentioned technology cannot be while meet the shortcoming of high power capacity, long-life and excellent high rate performance, the present invention
There is provided a kind of economical and efficient, stable performance, can industrialized production three-dimensional porous carbon coating selenizing Zinc material and its preparation side
Method and the application in field of lithium ion battery.
The preparation method of the three-dimensional polyhedron porous carbon coating zinc selenide material that the present invention is provided, is had using zinc-base metal
Machine frame（ZIF-8）As template, selenylation reaction is carried out at high temperature with selenium powder as protective atmosphere by the use of hydrogen-argon-mixed,
Original position prepares three-dimensional porous carbon coating selenizing Zinc material.In the material of preparation, it is embedded in porous carbon by zinc selenide quantum dot,
With meso-hole structure and higher specific surface area, and intactly 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 three-dimensional polyhedron porous carbon coating zinc selenide material of the present invention, concretely comprises the following steps：
（1）1.35-1.66 gram of zinc nitrate hexahydrate and 1.45-1.85 gram of 2-methylimidazole are weighed, 15-35 milliliters are dissolved in respectively
In methanol solution, then stirring and dissolving is poured 2-methylimidazole solution in zinc nitrate solution into；Mix to uniform（5-10
Minute）, 18-24 hours are stood at room temperature, product centrifugation is cleaned 2-4 time with ethanol solution, finally it is placed in 55-80
In degree Celsius drying box, products therefrom is polyhedron shape ZIF-8；Product is white, mostly granatohedron pattern, particle
Size is mainly distributed between 600 to 900 nanometers；
（2）Three-dimensional porous carbon coating selenizing Zinc material and preparation：Weigh the selenium of 100 to 300 milligrams of ZIF-8 and 100 to 300 milligrams
Powder is respectively placed in the two ends of porcelain boat, and porcelain boat is put in tube furnace, be passed through it is hydrogen-argon-mixed, with the liter of 1-3 centigrade per minutes
Warm speed is heated to 400 to 600 degrees Celsius, is incubated 2 to 4 hours at this temperature, that is, obtain three-dimensional porous carbon coating selenizing
Zinc material.
The present invention prepare three-dimensional porous selenizing Zinc material there is microcellular structure and higher specific surface area, can be used for lithium from
Sub- GND active material, the material has higher capacity, and three-dimensional porous structure can effectively buffer removal lithium embedded mistake
Volume Changes in journey, improve cycle performance.Positive pole, microporous polypropylene membrane are done with lithium piece（Celgard 2400）Barrier film is made, is adopted
Use business electrolyte（LiPF6For electrolyte, EC and DMC is solvent and volume ratio is 1:1）, being assembled into CR2032 types battery is carried out
Test.
Advantage of the invention is that：（1）Three-dimensional porous selenizing Zinc material maintains well the three-dimensional multiaspect of original ZIF-8
Bodily form looks, and with microcellular structure and larger specific surface area, show to be substantially better than at present in fields such as lithium ion batteries
The capacity and cycle performance of the selenizing Zinc material known；（2）Raw material relate only to zinc nitrate hexahydrate, 2-methylimidazole, selenium powder and
The common agents such as methyl alcohol, ethanol, safety non-toxic is with low cost, and product purity is high；（3）Three-dimensional porous selenium is prepared using one-step method
Change Zinc material, process is simple, it is easy to industrialized production；（4）This method has good applicability, can be extended to other metals
In the preparation method of selenides.
In sum, the invention provides a kind of capacity is high, stability and good cycle, simple to operate, security it is good,
Low cost, efficiency high, be easy to industrialized production three-dimensional porous selenizing Zinc material preparation method.
Description of the drawings
Fig. 1 is the ESEM of the three-dimensional porous selenizing Zinc material prepared by the embodiment of the present invention 1（SEM）Figure.
Fig. 2 is the transmission electron microscope of the three-dimensional porous selenizing Zinc material prepared by the embodiment of the present invention 1（TEM）Figure.
Fig. 3 is the X-ray diffraction of the three-dimensional porous selenizing Zinc material prepared by the embodiment of the present invention 1（XRD）Figure.
Fig. 4 is the specific surface area analysis of three-dimensional porous selenizing Zinc material prepared by the embodiment of the present invention 1（BET）Figure.
Fig. 5 be the lithium that 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 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, with reference to example and accompanying drawing, the present invention is further described.
Embodiment 1：Three-dimensional porous carbon coating selenizing Zinc material and its preparation method and application, comprises the following steps：
（1）It is prepared by the ZIF-8 templates with polyhedron pattern：Weigh 1.45 grams of zinc nitrate hexahydrates and 1.66 grams of 2- methyl miaows
Azoles, during 20 milliliters of methanol solution is dissolved in respectively, after dissolving to be mixed, 2-methylimidazole solution is poured in zinc nitrate solution；
Stirring 5 minutes, stands 24 hours at room temperature, and product centrifugation is cleaned 4 times with ethanol solution, is finally placed in 55 Celsius
In degree drying box, products therefrom is polyhedron shape ZIF-8；Product is white, mostly granatohedron pattern, particle size
It is mainly distributed between 600 to 900 nanometers；
（2）Three-dimensional porous selenizing Zinc material and preparation：The selenium powder for weighing 200 milligrams ZIF-8 and 200 milligram is respectively placed in porcelain boat
Two ends, porcelain boat is put in tube furnace, is passed through hydrogen-argon-mixed, is heated to 600 with the heating rate of 3 centigrade per minutes Celsius
Degree, is incubated 2 hours at this temperature, that is, obtain three-dimensional porous carbon coating selenizing Zinc material.
Three-dimensional porous carbon coating selenizing Zinc material is used as into lithium ion battery negative pole active materials, positive pole is done with lithium piece, gathered
Propylene microcellular film（Celgard 2400）Barrier film is made, using business electrolyte（LiPF6For electrolyte, EC and DMC is solvent and body
Product is than being 1:1）, it is assembled into CR2032 type batteries and is tested.Shown in its pattern and characteristic as Fig. 1-Fig. 5.
Advantage of the invention is that：（1）Three-dimensional porous selenizing Zinc material maintains well the three-dimensional multiaspect of original ZIF-8
Bodily form looks, and with microcellular structure and larger specific surface area, show to be substantially better than at present in fields such as lithium ion batteries
The capacity of the selenizing Zinc material known（Fig. 4, under the current density of 600mA/g, circulates 500 times, and capacity is maintained at 1134mAh/g）
And cycle performance（Fig. 5,200, under the current density of 400,800,1600,3200,6400,12800 mA/g, capacity is respectively
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 methyl alcohol, ethanol, safety non-toxic is with low cost, and product purity is high；（3）Using one-step method system
Standby three-dimensional porous selenizing Zinc material, process is simple is easy to industrialized production.
Embodiment 2：Three-dimensional porous carbon coating selenizing Zinc material and its preparation method and application, comprises the following steps：
（1）It is prepared by the ZIF-8 templates with polyhedron pattern：Weigh 1.45 grams of zinc nitrate hexahydrates and 1.66 grams of 2- methyl miaows
Azoles, during 20 milliliters of methanol solution is dissolved in respectively, after dissolving to be mixed, 2-methylimidazole solution is poured in zinc nitrate solution；
Stirring 5 minutes, stands 24 hours at room temperature, and product centrifugation is cleaned 4 times with ethanol solution, is finally placed in 55 Celsius
In degree drying box, products therefrom is polyhedron shape ZIF-8；Product is white, mostly granatohedron pattern, particle size
It is mainly distributed between 600 to 900 nanometers；
（2）Three-dimensional porous selenizing Zinc material and preparation：The selenium powder for weighing 200 milligrams ZIF-8 and 200 milligram is respectively placed in porcelain boat
Two ends, porcelain boat is put in tube furnace, is passed through hydrogen-argon-mixed, is heated to 500 with the heating rate of 3 centigrade per minutes Celsius
Degree, is incubated 2 hours at this temperature, that is, obtain three-dimensional porous carbon coating selenizing Zinc material.
Three-dimensional porous carbon coating selenizing Zinc material is used as into lithium ion battery negative pole active materials, positive pole is done with lithium piece, gathered
Propylene microcellular film（Celgard 2400）Barrier film is made, using business electrolyte（LiPF6For electrolyte, EC and DMC is solvent and body
Product is than being 1:1）, it is assembled into CR2032 type batteries and is tested.Its pattern and characteristic are similar with embodiment 1.
Advantage of the invention is that：（1）Three-dimensional porous selenizing Zinc material maintains well the three-dimensional multiaspect of original ZIF-8
Bodily form looks, and with microcellular structure and larger specific surface area, show to be substantially better than at present in fields such as lithium ion batteries
The capacity and cycle performance of the selenizing Zinc material known；（2）Raw material relate only to zinc nitrate hexahydrate, methylimidazole, selenium powder and
The common agents such as methyl alcohol, ethanol, safety non-toxic is with low cost, and product purity is high；（3）Three-dimensional porous selenium is prepared using one-step method
Change Zinc material, process is simple is easy to industrialized production.
Claims (3)
1. a kind of preparation method of three-dimensional porous carbon coating selenizing Zinc material, it is characterised in that using zinc-base metal organic frame
（ZIF-8）As template, by the use of hydrogen-argon-mixed as protective atmosphere, selenylation reaction, original position system are carried out at high temperature with selenium powder
It is standby to obtain three-dimensional porous carbon coating selenizing Zinc material；Concretely comprise the following steps：
（1）It is prepared by the ZIF-8 templates with polyhedron pattern：
1.35-1.66 gram of zinc nitrate hexahydrate and 1.45-1.85 gram of 2-methylimidazole are weighed, the first of 15-35 milliliters is dissolved in respectively
In alcoholic solution, then stirring and dissolving is poured 2-methylimidazole solution in zinc nitrate solution into；Mix to uniformly, in room temperature
Lower standing 18-24 hours, product centrifugation is cleaned 2-4 time with ethanol solution, is finally placed in 55-80 degree Celsius of drying box
In, products therefrom is polyhedron shape ZIF-8；Product is white, mostly granatohedron pattern, and particle size is mainly distributed
Between 600 to 900 nanometers；
（2）Polyhedron shape selenizing Zinc material and preparation：
Weigh 100 to 300 milligrams of ZIF-8 and 100 to 300 milligrams of selenium powder is respectively placed in the two ends of porcelain boat, put porcelain boat into pipe
In formula stove, it is passed through hydrogen-argon-mixed, with the heating rate of 1-3 centigrade per minutes 500-600 degree Celsius is heated to, in this temperature
The lower insulation 2-4 hours of degree, that is, obtain the zinc selenide quantum dot material of three-dimensional porous carbon coating.
2. a kind of selenizing Zinc material of the three-dimensional porous carbon coating obtained by preparation method described in claim 1.
3. a kind of selenizing Zinc material of the three-dimensional porous carbon coating by described in claim 2, active as lithium ion cell electrode
The application of material.
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| CN107516734A (en) * | 2017-08-10 | 2017-12-26 | 福建师范大学 | A kind of preparation method of carbon-coating nickel tin alloy nanosphere and its application in lithium battery |
| CN107640783A (en) * | 2017-10-16 | 2018-01-30 | 广州质量监督检测研究院 | Porous regular dodecahedron ZnO and its application as lecithin sorbing material |
| CN108054020A (en) * | 2017-11-22 | 2018-05-18 | 江苏大学 | A kind of preparation method and application of nitrogen-doped carbon particle/graphitized carbon nitrogen composite material |
| CN108525679A (en) * | 2018-05-22 | 2018-09-14 | 南开大学 | A method of preparing ZnS quantum dots and redox graphene compound by presoma of metal organic frame |
| CN108532290A (en) * | 2018-02-07 | 2018-09-14 | 南通大学 | A kind of preparation method and applications of photocatalytic functional fabric |
| CN109360986A (en) * | 2018-09-28 | 2019-02-19 | 桂林电子科技大学 | Application of the zinc selenide as aluminium ion cell positive material |
| CN109638266A (en) * | 2018-12-26 | 2019-04-16 | 山东大学 | A kind of carbon coating selenium indium lithium material and the preparation method and application thereof |
| CN109755527A (en) * | 2019-01-04 | 2019-05-14 | 中南大学 | A kind of preparation method and applications of zinc selenide/carbon fiber energy storage material |
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| CN107516734B (en) * | 2017-08-10 | 2020-03-17 | 福建师范大学 | Preparation method of carbon-coated nickel-tin alloy nanospheres and application of nanospheres in lithium battery |
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