CN107317001A - A kind of artificial gold/N doping carbonization bacteria cellulose lithium ion battery negative material and preparation method thereof - Google Patents
A kind of artificial gold/N doping carbonization bacteria cellulose lithium ion battery negative material and preparation method thereof Download PDFInfo
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- CN107317001A CN107317001A CN201710456535.3A CN201710456535A CN107317001A CN 107317001 A CN107317001 A CN 107317001A CN 201710456535 A CN201710456535 A CN 201710456535A CN 107317001 A CN107317001 A CN 107317001A
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- bacteria cellulose
- artificial gold
- lithium ion
- ion battery
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- 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
- H01M4/581—Chalcogenides or intercalation compounds thereof
- H01M4/5815—Sulfides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of artificial gold/N doping carbonization bacteria cellulose lithium ion battery negative material and preparation method thereof.The preparation method of the present invention includes water-bath process, carbonation process, the present invention is raw material using bacteria cellulose, by water-bath process artificial gold is grown in bacteria cellulose surface in situ, after being dried by washing, the carbonization bacteria cellulose and vertical distribution for obtaining N doping in the step of carbonation process one uniformly vulcanize tin composite material.The materials application has height ratio capacity, high coulomb efficiency and stable cycle performance in lithium ion battery negative material, the lithium ion battery of assembling.Simple to operate, energy consumption of the invention is relatively low, preparation process controllable row is high.
Description
Technical field
The invention belongs to field of lithium ion battery, it is related to a kind of artificial gold/N doping carbonization bacteria cellulose lithium-ion electric
Pond negative material and preparation method thereof.
Background technology
With expanding economy, the energy increasingly exhaustion problem is badly in need of solving.Lithium ion battery is that current combination property is best
Secondary cell, be widely used in all kinds of portable sets.Lithium ion battery has that energy density is high, has extended cycle life,
The features such as operating voltage is high, but because traditional lithium rechargeable battery by the theoretical lithium storage content of positive electrode due to being restricted,
It is difficult to make a breakthrough in terms of energy density is lifted, such as the most widely used its theoretical energy of graphene negative material
Density is only 372Wh kg-1, also far from the high energy consumption demand for meeting current equipment.Therefore, new negative active core-shell material is found
It is particularly important.Artificial gold has larger interlamellar spacing, and theoretical specific capacity is up to 782mAh g-1, rich reserves, hypotoxicity,
But the poorly conductive of artificial gold, serious Volumetric expansion is there is during removal lithium embedded, active material is easily caused
Disengaging and crushing, so as to have a strong impact on the chemical property of battery.Compound with carbon material is to effectively improve vulcanization tin electrode material
The effective way of material, and traditional method is usually the method using Hydrothermal Synthesiss, preparation technology controllability is poor, energy consumption compared with
It is high.
Bacteria cellulose wide material sources, cheap and easy to get, pattern is homogeneous controllable, is a kind of reproducible environmentally friendly biology
Material.The bacteria cellulose that is carbonized is the char-forming material processed under an inert atmosphere through high annealing by bacteria cellulose.
In recent years, carbonization bacteria cellulose by three-dimensional netted nanofiber that its presoma bacteria cellulose has can be retained, it is excellent
The characteristic such as different electric conductivity and chemical stability, is received significant attention, especially in energy storage material field.Wang et al. (Bin
Wang et al.Small,2013,9(14):2399-2404.) preparing Ge/CBC composites first is used for lithium ion battery,
The battery shows poor high rate performance, and it is to influence the key factor of its battery performance to think electrical conductivity.In addition, high temperature
The CBC aperture contents obtained that are carbonized are relatively low, therefore to dissolubility polysulfide absorption and control ability in lithium ion battery operation
Relatively limited (Yang Huang et al.Journal of Materials Chemistry A, 2015,3:10910-
10918.).In addition, through char-forming material made from high annealing, less oxygen-containing functional group is contained on surface, hinders and enters one to it
Step application.
The content of the invention
It is an object of the invention to provide a kind of GND of artificial gold/N doping carbonization bacteria cellulose.
Realize that the technical scheme of above-mentioned purpose is as follows：
A kind of GND of artificial gold/N doping carbonization bacteria cellulose, is prepared by following steps：
Step 1, water-bath process：Tin source, nitrogen sulphur source are dissolved in ethanol, after being uniformly dispersed, bacterial cellulose gel soaked
Stain is soaked in above-mentioned solution, at room temperature after 0.5-3h, and mixing liquid is reacted into 20-80min at 60~100 DEG C, is produced
After thing is scrubbed and dry, artificial gold and the bacteria cellulose composite material i.e. nano combined material of artificial gold/bacteria cellulose are obtained
Material；
Step 2, carbonation process：By artificial gold/bacterial cellulose nano composite material pressing processing, then in inert atmosphere
Under in being carbonized at 600-800 DEG C, obtain artificial gold/N doping carbonization bacteria cellulose aeroge；
In step 1, the thickness of described bacterial cellulose gel is 1.5-3.0mm,
In step 1, described pink salt is selected from one or both of butter of tin, stannous chloride, selected from thioacetamide,
Mass ratio 1 of the bacteria cellulose/pink salt/nitrogen sulphur source in mixed solution：1：3, wherein the concentration of thioacetamide be 70~
280mM。
In step 1, described washing is that the volume ratio of ethanol and deionized water is 1：1 mixed solution is washed, and drying is
Vacuum freeze drying；
In step 2, the pressure of described pressing processing is 0.2Mpa, and inert atmosphere is the mixing of nitrogen or hydrogen and argon gas
Gas, described carbonization time is 1-3h；
Compared with prior art, the present invention has following remarkable result：
(1) present invention is carrier using the bacteria cellulose of macroreticular structure, using difunctional dose, prepares artificial gold
N doping is carried out simultaneously, and completing a step by carburising step obtains artificial gold/N doping carbonization bacteria cellulose；
(2) preparation technology that uses of the present invention is simple to operate, energy consumption is relatively low, and Modulatory character is strong, with merchandized handling
Potentiality；
(3) composite prepared by the present invention is the artificial gold vertical distribution of small lamella in three-dimensional N doping carbonization bacterium fibre
Dimension element, artificial gold has the controllable nanostructured of granular size, significantly improves the load capacity of artificial gold, and effectively buffering Sn exists
Volume Changes in charge/discharge, the lithium ion battery that assembling is formed has height ratio capacity, high coulomb efficiency and stable circulation
Performance.
Brief description of the drawings
Fig. 1 is the SnS/NCBC composite XRD spectrums prepared in embodiment 1.
Fig. 2 is the SnS/NCBC composite SEM spectrums prepared in embodiment 1.
Fig. 3 be the SnS/NCBC composite material prepared in embodiment 1 as lithium ion battery negative material in 100mA/g
Cyclical stability test chart under current density.
Embodiment
Below by embodiment and accompanying drawing, the invention will be further described.
Embodiment 1
Step 1, it is 20 according to molar concentration by butter of tin, thioacetamide：70mM is scattered in alcohol solvent, has been treated
After fully dissolved, the BC gel moulds for taking thickness to be 3.0mm are impregnated in above-mentioned solution, are soaked after 0.5h, will be mixed at room temperature
Close liquid and react 20min at 80 DEG C, the volume ratio of product ethanol and deionized water is 1：After 1 mixed solution washing, warp
Vacuum freeze drying is crossed, artificial gold and bacteria cellulose composite material i.e. artificial gold/bacterial cellulose nano composite material is obtained；
Step 2, artificial gold/bacterial cellulose nano composite material is subjected to pressing processing with 0.2Mpa normal pressures, then
1h carbonizations are incubated in 600 DEG C under nitrogen atmosphere protection, artificial gold/N doping carbonization bacteria cellulose aeroge is obtained.
The performance characterization of artificial gold/N doping carbonization bacteria cellulose aeroge is shown in Fig. 1.After being contrasted according to standard reference card
Restrain, artificial gold/N doping carbonization bacteria cellulose composite material of this method synthesis is consistent with standard card.
Embodiment 2
The molar concentration of butter of tin in embodiment 1, thioacetamide is changed into 40：140mM, remaining equal be the same as Example 1.
Embodiment 3
Water-bath reaction temperature in embodiment 1 is changed into 100 DEG C, remaining equal be the same as Example 1.
Embodiment 4
The water-bath reaction time in embodiment 1 is changed into 40min, remaining equal be the same as Example 1.
Embodiment 5
Carburizing temperature in embodiment 1 is changed into 700 DEG C, remaining equal be the same as Example 1.
Embodiment 6
Carburizing temperature in embodiment 1 is changed into 800 DEG C, remaining equal be the same as Example 1.
The SEM performance characterizations of artificial gold/N doping carbonization bacteria cellulose aeroge are shown in Fig. 2.Vulcanize as can be seen from Figure 2
Tin is uniformly arranged vertically on CBC, and CBC is wrapped up, and the lamella of artificial gold is smaller, is interted arrangement, is conducive to electricity
Infiltration and the ion exchange of liquid are solved, contributes to the lifting of battery performance.
It regard the gained final product SnS/NCBC composites of embodiment 5 as the negative material of lithium ion battery, the material
Negative electrode of lithium ion battery can be used for directly as self-supporting material, then using lithium piece as to electrode, electrolyte is commercially available 1mol/L
LiPF6/EC+DMC solution, assembling obtains lithium ion battery, and charge-discharge performance test, products therefrom are carried out using cell tester
As cyclical stability test result of the lithium ion battery negative material under 100mA/g current densities as shown in Figure 3.By attached
Fig. 3 is visible, the good cycling stability of battery, and battery capacity is still stablized in 681mAh/g after circulating 100 times.
Claims (6)
1. a kind of artificial gold/N doping carbonization bacteria cellulose lithium ion battery negative material, it is characterised in that the artificial gold/
N doping carbonization bacteria cellulose lithium ion battery negative material is made by following specific steps：
Step 1, water-bath process：Pink salt, nitrogen sulphur source are dissolved in ethanol, after being uniformly dispersed, bacterial cellulose gel are impregnated in
In above-mentioned solution；At room temperature after immersion 0.5-3h, mixing liquid is reacted into 20-80min, product warp at 60~100 DEG C
After washing and drying, artificial gold and bacteria cellulose composite material i.e. artificial gold/bacterial cellulose nano composite material are obtained；
Step 2, carbonation process：By the processing of artificial gold/bacterial cellulose nano composite material pressing, then under an inert atmosphere in
It is carbonized at 600-800 DEG C, obtains artificial gold/N doping carbonization bacteria cellulose aeroge.
2. artificial gold as claimed in claim 1/N doping carbonization bacteria cellulose lithium ion battery negative material, its feature exists
In in step 1, the thickness of described bacterial cellulose gel is 1.5-3.0mm.
3. artificial gold as claimed in claim 1/N doping carbonization bacteria cellulose lithium ion battery negative material, its feature exists
In, in step 1, pink salt is selected from one or both of butter of tin, stannous chloride, selected from thioacetamide, and bacteria cellulose/
Mass ratio 1 of the pink salt/nitrogen sulphur source in mixed solution：1：3, the wherein concentration of thioacetamide is 70~280mM.
4. artificial gold as claimed in claim 1/N doping carbonization bacteria cellulose lithium ion battery negative material, its feature exists
In in step 1, the washing is that the volume ratio of ethanol and deionized water is 1：1 mixed solution washing, it is vacuum refrigeration to dry
Dry.
5. artificial gold as claimed in claim 1/N doping carbonization bacteria cellulose lithium ion battery negative material, its feature exists
In in step 2, the pressure of described pressing processing is 0.2Mpa, and inert atmosphere is the gaseous mixture of nitrogen or hydrogen and argon gas, institute
The carbonization time stated is 1-3h.
The preparation of bacteria cellulose lithium ion battery negative material 6. artificial gold/N doping as described in claim 1-5 is carbonized
Method.
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Cited By (5)
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|---|---|---|---|---|
| CN107895786A (en) * | 2017-11-15 | 2018-04-10 | 晋中学院 | Flexible self-supporting SnS/ carbon foam composites and its preparation method and application |
| CN108598424A (en) * | 2018-04-25 | 2018-09-28 | 新疆大学 | A kind of SnS2Mesoporous carbon compound cathode materials of N doping and preparation method thereof |
| CN109776851A (en) * | 2019-01-04 | 2019-05-21 | 浙江工业大学 | A kind of bacteria cellulose/metal sulfide plural gel and preparation method thereof and conductive processing method |
| CN109841825A (en) * | 2019-03-29 | 2019-06-04 | 华南理工大学 | A kind of method that tin prepares lithium ion battery negative material in recycling electroplating sludge |
| CN112490449A (en) * | 2020-11-30 | 2021-03-12 | 胡冲丽 | Three-dimensional tubular molybdenum disulfide composite bacterial cellulose membrane electrode material and preparation method thereof |
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| CN106299385A (en) * | 2016-08-26 | 2017-01-04 | 南京理工大学 | N doping carbonization bacterial cellulose loaded nanometer platinum electrode material and preparation method thereof |
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| CN106552629A (en) * | 2016-11-01 | 2017-04-05 | 北京理工大学 | A kind of preparation method of the oxide/carbon nanofiber composite aerogel of cobalt |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107895786A (en) * | 2017-11-15 | 2018-04-10 | 晋中学院 | Flexible self-supporting SnS/ carbon foam composites and its preparation method and application |
| CN108598424A (en) * | 2018-04-25 | 2018-09-28 | 新疆大学 | A kind of SnS2Mesoporous carbon compound cathode materials of N doping and preparation method thereof |
| CN109776851A (en) * | 2019-01-04 | 2019-05-21 | 浙江工业大学 | A kind of bacteria cellulose/metal sulfide plural gel and preparation method thereof and conductive processing method |
| CN109841825A (en) * | 2019-03-29 | 2019-06-04 | 华南理工大学 | A kind of method that tin prepares lithium ion battery negative material in recycling electroplating sludge |
| CN109841825B (en) * | 2019-03-29 | 2021-10-26 | 华南理工大学 | Method for preparing lithium ion battery cathode material by recycling tin in electroplating sludge |
| CN112490449A (en) * | 2020-11-30 | 2021-03-12 | 胡冲丽 | Three-dimensional tubular molybdenum disulfide composite bacterial cellulose membrane electrode material and preparation method thereof |
| CN112490449B (en) * | 2020-11-30 | 2021-11-05 | 江苏日御光伏新材料科技有限公司 | Three-dimensional tubular molybdenum disulfide composite bacterial cellulose membrane electrode material and preparation method thereof |
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Application publication date: 20171103 |