CN109585837A - A kind of preparation method and applications of the carbon-coated cobaltous selenide nano material in original position - Google Patents
A kind of preparation method and applications of the carbon-coated cobaltous selenide nano material in original position Download PDFInfo
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- CN109585837A CN109585837A CN201811560020.9A CN201811560020A CN109585837A CN 109585837 A CN109585837 A CN 109585837A CN 201811560020 A CN201811560020 A CN 201811560020A CN 109585837 A CN109585837 A CN 109585837A
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Abstract
A kind of preparation method and applications of original position carbon coating cobaltous selenide nano material.This method is not under conditions of adding any template, surfactant, using the rodlike presoma of method synthesizing one-dimensional of hydro-thermal, is then prepared for cobaltous selenide nano-bar material by the method for carbon coating and selenizing in situ simultaneously.The present invention solves the problems such as higher cost existing for common carbon coating, process are cumbersome, cladding is uneven, one layer of amorphous carbon has uniformly been coated around selenizing cobalt nano-particle in carbon-coated method in situ, improves the stability and electric conductivity of cobaltous selenide material.And the cobaltous selenide of preparation is club shaped structure, size length is controllable.Gained carbon coating cobaltous selenide nano material is used as anode material of lithium-ion battery, shows higher capacity, longer cycle life and outstanding high rate performance.The preparation method has the advantages that process is simple, low in cost, yield is higher, reproducible, has very high practical value.
Description
Technical field
The invention belongs to anode material of lithium-ion battery fields, and in particular to a kind of carbon-coated cobaltous selenide (CoSe in original position
C) the preparation and application of electrode material.
Background technique
With electric car, the arrival in smart grid epoch, demand of the people to electronic product is continuously increased, therefore is developed low
The electrical energy storage device of cost is particularly important.However the shortage of lithium resource and the soaring of price seriously constrain new energy production
The development of industry, this becomes the focus of people's research the energy-storage battery system for developing other cheap alternative lithium ion batteries.
Sodium and lithium belong to same main group, have similar physics and chemical property, and have similar coil insertion device in electrochemical reaction
Reason, makes it possible in the two systems with similar compound as electrode material.In addition, the storage of sodium on earth
Higher than lithium 4~5 orders of magnitude are measured, there are the mature advantages such as low with development cost of widely distributed, extraction process.Therefore, sodium from
Sub- battery is expected to meet the needs of extensive stored energy application, becomes the ideal chose of next-generation energy storage and power battery.
Currently, the negative electrode material of sodium-ion battery mainly includes carbon material, layered oxide, alloy and Transition Metal Sulfur
Belong to several classes of compound.Wherein, cobaltous selenide due to sodium storage volume with higher, extensive availability and high safety it is wide
The general electrode material applied to sodium-ion battery.But cobaltous selenide as anode material of lithium-ion battery when asked there are still some
Topic, such as volume expansion in charge and discharge process, material powder phenomenon-tion are serious, this causes material poor circulation and capacity occur
Decay fast problem, limits its application in practice.Common ameliorative way mainly includes by material nano and carbon packet
Cover two kinds.Electrode material nanosizing can reduce the influence of mechanical stress by the volume change reduced in telescopiny, and
Nano material has big specific surface area, is conducive to coming into full contact with for material and electrolyte, and then can effectively improve the benefit of material
With rate；The electric conductivity and mechanical performance of material can be improved in carbon coating.However, design synthesizes while having nanostructure and carbon packet
The cobaltous selenide material covered, experimentation is cumbersome, time-consuming, while higher cost, yield are lower.Therefore, a kind of easy, warp is developed
Ji, high yield, the experimental method without template have great importance to synthesis cobaltous selenide material.
Summary of the invention
It is an object of the invention to solve the above problem of the existing technology, provide a kind of simple experiment, it is low in cost,
The preparation method of higher, without template the carbon-coated cobaltous selenide nano material in original position of yield, to improve the electronic conduction of cobaltous selenide
Property and structural stability, to improve the chemical property of material.
Technical solution of the present invention:
A kind of preparation method of the carbon-coated cobaltous selenide nano material in original position, this method are not adding any template, table
Under conditions of the activating agent of face, first with the rodlike presoma of method synthesizing one-dimensional of hydro-thermal, then pass through carbon coating in situ simultaneously
Cobaltous selenide nano material is prepared with the method for selenizing.Specific step is as follows:
1) cobalt source and nitrilotriacetic acid (NTA) are dissolved in the mixed solution of water and isopropanol, are stirred evenly, obtain pink
Solution；
2) above-mentioned solution is transferred in stainless steel autoclave, is put into constant temperature oven, the hydro-thermal at 150-180 DEG C
After being cooled to room temperature, products therefrom is filtered by 6-12h, and is washed for several times with distilled water and dehydrated alcohol, in vacuum drying oven
Middle drying finally obtains the presoma of pink；
3) presoma and selenium powder that step 2) obtains are put in tube furnace after mixing, in argon gas or nitrogen atmosphere
Under, 500-600 DEG C of calcining 2-4h obtains carbon-coated selenizing cobalt composite material in situ.
The cobalt source is cobalt chloride hexahydrate or cabaltous nitrate hexahydrate, the quality amount ratio of cobalt source and nitrilotriacetic acid (NTA)
It is 2.5:1, the volume ratio of the mixed solution of water and isopropanol is 1:3,1:1 or 3:1, mole matter of presoma and selenium powder when calcining
Amount is than being 1:1.5.
The carbon coating cobaltous selenide nano material of the method for the present invention preparation can be used as anode material of lithium-ion battery.
The advantages of the present invention:
The present invention by simple mild experimental method, solve higher cost existing for common carbon coating, process it is cumbersome,
Coat the problems such as uneven, with carbon-coated method in situ uniformly coated around selenizing cobalt nano-particle one layer it is amorphous
Carbon improves the stability and electric conductivity of cobaltous selenide material.And the cobaltous selenide material of preparation is club shaped structure, it is molten by adjusting
Agent ratio, the size length of controllable prepared material.Simultaneously preferably selenium powder be selenium source, instead of highly toxic selenous acid, hydrazine hydrate with
And sodium selenite etc., there is very high practical value.By the cobaltous selenide of preparation be used as anode material of lithium-ion battery, show compared with
High capacity, longer cycle life and outstanding high rate performance.
Detailed description of the invention
Fig. 1 is the XRD spectrum of carbon-coated selenizing cobalt composite material prepared by embodiment 1.
Fig. 2 is the SEM figure and TEM figure of carbon-coated selenizing cobalt composite material prepared by embodiment 1, in which: (a) SEM figure,
(b) TEM schemes.
Fig. 3 is the carbon-coated selenizing cobalt composite material of the preparation of embodiment 1 in 0.1A g-1Current density under charge and discharge
Curve graph.
Fig. 4 is the carbon-coated selenizing cobalt composite material of the preparation of embodiment 1 in 0.1A g-1Current density under cyclicity
It can figure and corresponding coulombic efficiency.
Specific embodiment
The present invention is described further below with reference to embodiment.
Embodiment 1:
A kind of preparation method of the carbon-coated cobaltous selenide nano material in original position, this method are not adding any template, table
Under conditions of the activating agent of face, first with the rodlike presoma of method synthesizing one-dimensional of hydro-thermal, then pass through carbon coating in situ simultaneously
Cobaltous selenide nano material is prepared with the method for selenizing.Specific step is as follows:
1) 1.5g cobalt chloride hexahydrate (CoCl is weighed2·6H2O) with 0.6g nitrilotriacetic acid (NTA) be dissolved in 30mL distilled water and
It in the mixed solution of 10mL isopropanol, stirs evenly, obtains pink solution.
2) above-mentioned mixed solution is transferred in 50mL stainless steel autoclave, is put into 180 DEG C of hydro-thermals in constant temperature oven
After being cooled to room temperature, products therefrom is filtered by 6h, and is washed for several times with distilled water and dehydrated alcohol, in vacuum drying oven
It is dry, finally obtain the presoma of pink.
3) presoma and selenium powder that step 2) obtains are put in tube furnace after mixing in the ratio of 1:1.5, in argon
Atmosphere enclose under with 2 DEG C of min-1Heating rate be raised to 600 DEG C, and keep the temperature 2h, obtain target product.
The XRD spectrum of the carbon-coated cobaltous selenide material of preparation in figure as shown in Figure 1, show: products therefrom is hexagonal crystal
The cobaltous selenide of system, and without other impurities.
Fig. 2 is SEM and the TEM figure of the carbon-coated selenizing cobalt composite material of preparation, in which: (a) SEM figure, (b) TEM schemes,
Show in figure: the cobaltous selenide of preparation is club shaped structure, while 0.15nm thickness is uniformly coated with around selenizing cobalt nano-particle
Amorphous carbon.
Fig. 3 is the carbon-coated selenizing cobalt composite material of preparation in 0.1A g-1Current density under charging and discharging curve figure,
Show in figure: material has preferable capacity retention ratio.
Fig. 4 is the carbon-coated selenizing cobalt composite material of preparation in 0.1A g-1Current density under cycle performance figure with
And corresponding coulombic efficiency, show in figure: carbon-coated cobaltous selenide shows good as the negative electrode material of sodium-ion battery
Cyclical stability.
Embodiment 2:
A kind of preparation method of the carbon-coated cobaltous selenide nano material in original position, this method are not adding any template, table
Under conditions of the activating agent of face, first with the rodlike presoma of method synthesizing one-dimensional of hydro-thermal, then pass through carbon coating in situ simultaneously
Cobaltous selenide nano material is prepared with the method for selenizing.Specific step is as follows:
1) 1.5g cobalt chloride hexahydrate (CoCl is weighed2·6H2O) with 0.6g nitrilotriacetic acid (NTA) be dissolved in 20mL distilled water and
It in the mixed solution of 20mL isopropanol, stirs evenly, obtains pink solution.
2) above-mentioned mixed solution is transferred in 50mL stainless steel autoclave, is put into 180 DEG C of hydro-thermals in constant temperature oven
After being cooled to room temperature, products therefrom is filtered by 6h, and is washed for several times with distilled water and dehydrated alcohol, in vacuum drying oven
It is dry, finally obtain the presoma of pink.
3) presoma and selenium powder that step 2) obtains are put in tube furnace after mixing in the ratio of 1:1.5, in argon
Atmosphere enclose under with 2 DEG C of min-1Heating rate be raised to 600 DEG C, and keep the temperature 2h, obtain target product.
Embodiment 3:
A kind of preparation method of the carbon-coated cobaltous selenide nano material in original position, this method are not adding any template, table
Under conditions of the activating agent of face, first with the rodlike presoma of method synthesizing one-dimensional of hydro-thermal, then pass through carbon coating in situ simultaneously
Cobaltous selenide nano material is prepared with the method for selenizing.Specific step is as follows:
1) 1.5g cobalt chloride hexahydrate (CoCl is weighed2·6H2O) with 0.6g nitrilotriacetic acid (NTA) be dissolved in 10mL distilled water and
It in the mixed solution of 30mL isopropanol, stirs evenly, obtains pink solution.
2) above-mentioned mixed solution is transferred in 50mL stainless steel autoclave, is put into 180 DEG C of hydro-thermals in constant temperature oven
After being cooled to room temperature, products therefrom is filtered by 6h, and is washed for several times with distilled water and dehydrated alcohol, in vacuum drying oven
It is dry, finally obtain the presoma of pink.
3) presoma and selenium powder that step 2) obtains are put in tube furnace after mixing in the ratio of 1:1.5, in argon
Atmosphere enclose under with 2 DEG C of min-1Heating rate be raised to 600 DEG C, and keep the temperature 2h, obtain target product.
Embodiment 4:
A kind of preparation method of the carbon-coated cobaltous selenide nano material in original position, this method are not adding any template, table
Under conditions of the activating agent of face, first with the rodlike presoma of method synthesizing one-dimensional of hydro-thermal, then pass through carbon coating in situ simultaneously
Cobaltous selenide nano material is prepared with the method for selenizing.Specific step is as follows:
1) 1.5g cabaltous nitrate hexahydrate (Co (NO) is weighed2·6H2O) 30mL distilled water is dissolved in 0.6g nitrilotriacetic acid (NTA)
In the mixed solution of 10mL isopropanol, stirs evenly, obtain pink solution.
2) above-mentioned mixed solution is transferred in 50mL stainless steel autoclave, is put into 150 DEG C of hydro-thermals in constant temperature oven
After being cooled to room temperature, products therefrom is filtered by 12h, and is washed for several times with distilled water and dehydrated alcohol, in vacuum drying oven
It is dry, finally obtain the presoma of pink.
3) presoma and selenium powder that step 2) obtains are put in tube furnace after mixing in the ratio of 1:1.5, in argon
Atmosphere enclose under with 2 DEG C of min-1Heating rate be raised to 500 DEG C, and keep the temperature 4h, obtain target product.
Claims (5)
1. a kind of preparation method of the carbon-coated cobaltous selenide nano material in original position, which is characterized in that this method do not add it is any
Under conditions of template, surfactant, first with the rodlike presoma of method synthesizing one-dimensional of hydro-thermal, then by former simultaneously
Position carbon coating and the method for selenizing are prepared for selenizing cobalt nanorod, the specific steps are as follows:
1) cobalt source and nitrilotriacetic acid (NTA) are dissolved in the mixed solution of water and isopropanol, are stirred evenly, it is molten to obtain pink
Liquid；
2) above-mentioned solution is transferred in stainless steel autoclave, is put into constant temperature oven the hydro-thermal 6- at 150-180 DEG C
After being cooled to room temperature, products therefrom is filtered by 12h, washing, dry in vacuum drying oven, before finally obtaining pink
Drive body；
3) presoma and selenium powder that step 2) obtains are put in tube furnace after mixing, under argon gas or nitrogen atmosphere,
500-600 DEG C of calcining 2-4h obtains carbon-coated selenizing cobalt composite material in situ.
2. the preparation method of carbon-coated cobaltous selenide nano material in situ according to claim 1, it is characterised in that: the cobalt
Source is the mixing of one or more of cobalt chloride hexahydrate, cabaltous nitrate hexahydrate or four acetate hydrate cobalts arbitrary proportion
The volume ratio of the mixed solution of object, water and isopropanol is 1:3,1:1 or 3:1.
3. the preparation method of the carbon-coated cobaltous selenide nano material in original position according to claim 1 or claim 2, it is characterised in that: institute
The amount ratio of the cobalt source and nitrilotriacetic acid (NTA) stated is 2.5:1.
4. the preparation method of the carbon-coated cobaltous selenide nano material in original position according to claim 1 or claim 2, it is characterised in that: institute
The amount ratio of the presoma and selenium powder stated is 1:1.5.
5. the carbon-coated cobaltous selenide applications to nanostructures of claim 1 the method preparation, the application is by carbon coating
Cobaltous selenide nano material be used as anode material of lithium-ion battery.
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| CN110492081A (en) * | 2019-08-27 | 2019-11-22 | 合肥工业大学 | A kind of preparation method and applications of cobaltous selenide/porous carbon nanotube of zinc selenide N doping |
| CN111349915A (en) * | 2020-02-20 | 2020-06-30 | 齐鲁工业大学 | CoSe with controllable appearance2/Ti composite material and preparation method thereof |
| CN114229805A (en) * | 2021-11-03 | 2022-03-25 | 深圳市本征方程石墨烯技术股份有限公司 | Preparation method and application of nitrogen-doped porous carbon-coated cobalt diselenide composite material |
| CN114388753A (en) * | 2021-12-13 | 2022-04-22 | 安徽大学 | Preparation method of edge nitrogen-doped porous hollow carbon nanorod material, prepared material and application thereof |
| CN114430043A (en) * | 2022-01-21 | 2022-05-03 | 山东大学 | Carbon-coated cobalt nickel selenide nanosphere material, preparation method and application of aluminum battery |
| CN114937761A (en) * | 2022-04-25 | 2022-08-23 | 多助科技(武汉)有限公司 | Nobaltosulfide/manganese sulfide/nitrogen-carbon composite material and preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110492081A (en) * | 2019-08-27 | 2019-11-22 | 合肥工业大学 | A kind of preparation method and applications of cobaltous selenide/porous carbon nanotube of zinc selenide N doping |
| CN110492081B (en) * | 2019-08-27 | 2021-03-23 | 合肥工业大学 | Preparation method and application of cobalt selenide/zinc selenide @ nitrogen-doped porous carbon nanotube |
| CN111349915A (en) * | 2020-02-20 | 2020-06-30 | 齐鲁工业大学 | CoSe with controllable appearance2/Ti composite material and preparation method thereof |
| CN114229805A (en) * | 2021-11-03 | 2022-03-25 | 深圳市本征方程石墨烯技术股份有限公司 | Preparation method and application of nitrogen-doped porous carbon-coated cobalt diselenide composite material |
| CN114388753A (en) * | 2021-12-13 | 2022-04-22 | 安徽大学 | Preparation method of edge nitrogen-doped porous hollow carbon nanorod material, prepared material and application thereof |
| CN114430043A (en) * | 2022-01-21 | 2022-05-03 | 山东大学 | Carbon-coated cobalt nickel selenide nanosphere material, preparation method and application of aluminum battery |
| CN114937761A (en) * | 2022-04-25 | 2022-08-23 | 多助科技(武汉)有限公司 | Nobaltosulfide/manganese sulfide/nitrogen-carbon composite material and preparation method and application thereof |
| CN114937761B (en) * | 2022-04-25 | 2023-10-13 | 多助科技(武汉)有限公司 | Nine cobalt octasulfide/manganese sulfide/nitrogen carbon composite material and preparation method and application thereof |
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