CN110492074A - A method of preparing lithium ion battery carbon fiber/antimony trisulfide composite negative pole - Google Patents
A method of preparing lithium ion battery carbon fiber/antimony trisulfide composite negative pole Download PDFInfo
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- CN110492074A CN110492074A CN201910780520.1A CN201910780520A CN110492074A CN 110492074 A CN110492074 A CN 110492074A CN 201910780520 A CN201910780520 A CN 201910780520A CN 110492074 A CN110492074 A CN 110492074A
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- carbon fiber
- antimony trisulfide
- negative pole
- composite negative
- lithium ion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01M4/362—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
- 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
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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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- 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 present invention, which discloses, a kind of prepares lithium ion battery carbon fiber/antimony trisulfide composite negative pole method, it can be directly electrode active material, carbon fiber as conducting base using natural stibnite, and the novel anode material of carbon fiber substrates is coated by melt-synthesizing nanoscale antimony trisulfide, the structure has been released effectively the stress variation of antimony trisulfide intra-die in process of intercalation, while shortening Li+With electronics in the path that material internal transmits, carbon fiber substrate provides excellent conductive network for composite material, and due to that can eliminate high energy consumption, the metallurgy purification process of high pollution using natural stibnite as the direct material of electrode active material；Nanocomposite is prepared using solid phase mixing fusion method, eliminates offal treatment technique.
Description
Technical field
The present invention relates to technical field of lithium ion, and in particular to a kind of to prepare lithium ion battery carbon fiber/antimony trisulfide
The method of composite negative pole.
Background technique
In lithium ion battery, the performance of electrode material directly determines the energy density, service life and sale of battery
Price.As one of storage lithium main body, the superiority and inferiority of the comprehensive performance of cathode is most important.When graphite type material is as cathode, have
The advantages that stable structure, first effect are high, and electric conductivity is good.But its lower theoretical specific capacity has been unable to meet future market to high ratio
The needs of energy lithium ion battery.And in numerous novel cathode, antimony trisulfide is by its high theoretical specific capacity, moderate platform electricity
Position, resource reserve abundant cause the extensive concern of researcher.
However, due to the semiconductor properties of itself, ion/electronic conductivity relatively low (10 of antimony trisulfide-8-10-9S·cm-1), and cause its electrode kinetics process slow, material is easy to crack to fall off with more serious volume change in process of intercalation
Loss of activity, overall performance go out the feature that cycle life is short, high rate performance is poor.For this main problem, many nano shapes
Antimony trisulfide and antimony trisulfide composite material are used to improve electric conductivity, alleviate volume expansion.Including antimony sulfide nano piece
(Energy Storage Materials, 2018), nanometer rods (Materials Letters, 2009,63,1258-1261),
Nanometer bouquet (Journal of Alloys and Compounds, 2013,572,56-61), antimony trisulfide/reduction-oxidation graphite
Alkene (Adv.Mater.Interfaces, 2018,1701481) etc..Although above-mentioned antimony trisulfide and its composite material improve vulcanization
The circulation and high rate performance of antimony, but its solwution method preparation process is tediously long, waste liquid amount is big, repeatability is poor, is not conducive to industry popularization
Using.
Carbon fiber is a kind of high conductive carbon material, is used for combination electrode material as conductive improved component extensively
In.Conventional composite materials preparation based on carbon fiber, often through means such as hydro-thermal, solvent heat, collosol and gels, to be commercialized height
Pure reagent obtains for raw material, by certain process regulation.Although changing as described above, nano active substance can be prepared
The electric conductivity of kind composite material, but this process is often more tediously long, the place of heavy metal, acid, alkali, organic matter in waste liquid etc.
Reason considerably increases preparation cost, is not conducive to be mass produced.Secondly, the preparation of business high purity reagent is also required to complicated, high consumption
Metallurgical process.
Summary of the invention
Complicated in view of preparation process of the existing technology, at high cost and antimony trisulfide negative conductive is poor, embedding lithium volume becomes
Change the problems such as serious, the present invention proposes a kind of to prepare lithium ion battery carbon fiber/antimony trisulfide composite negative pole method.
In order to achieve the above objectives, proposed by the present invention a kind of to prepare lithium ion battery carbon fiber/antimony trisulfide composite negative pole
Method, comprising the following steps:
Antimony trisulfide and carbon fiber are mixed and dried；
Above-mentioned dry pack is placed in heating melting in inert atmosphere, and held for some time, is quickly cooled down or natural
After cooling, the stibnite of melting is attached on carbon fiber, and recrystallization forms nanoscale antimony trisulfide crystal grain, and thus obtains carbon fiber
Dimension/antimony trisulfide composite negative pole；Wherein the diameter of carbon fiber is 50-150nm, and length is 1-10 μm；Antimony trisulfide with nano particle or
Nanometer sheet is coated on carbon fiber, and the size of antimony sulfide nano grain diameter or nanometer sheet is in 150nm or less.
Preferably, antimony trisulfide used is the sulfide mineral or high-purity antimony trisulfide of stibnite or other metallic antimonies.
Preferably, antimony trisulfide, carbon fiber mixed method be ball milling, grinding or solution stirring.
Preferably, ball milling and process of lapping include dry grinding and wet-milling, and dry grinding medium includes air or argon gas, wet-milling and solution
Agitated medium includes water or alcohol.
When preferably, using ball milling mixing, ratio of grinding media to material 10:1-20:1, revolving speed 300-1200r/min, Ball-milling Time
For 0.5-10h；When being stirred using solution, speed of agitator 300-1000r/min, time 0.5-10h.
Preferably, the mass ratio that antimony trisulfide, carbon fiber mix is 95:5-10:90.
Preferably, antimony trisulfide and the temperature of carbon fiber mixed material heating melting are 550-700 DEG C, soaking time 0.5-
10h。
In the present invention, nanocomposite is prepared using fusion method, pattern, the performance repeatability of material are high, and make
Standby process is simple, and the use without other reagents does not generate waste and pollution；Using natural stibnite as raw material, high-purity quotient is saved
The use of industry reagent, eliminates the metallurgical process of feedstock purification, and enriches the application field of antimony resource；It is conduction with carbon fiber
Substrate improves the electric conductivity of material, may advantageously facilitate electrode kinetics process；Stibnite after recombination with nano particle or is received
The form of rice piece exists, and partial size in 150nm hereinafter, embedding lithium volumetric stress can effectively be discharged, and shorten lithium ion and
Electronically transmission path, recycles and high rate performance with improving antimony trisulfide.
Detailed description of the invention
Fig. 1 is carbon fiber scanning electron microscope (SEM) photograph；
Fig. 2 is composite negative pole (the carbon fibers Sb that antimony trisulfide coats carbon fiber2S3) scanning electron microscope (SEM) photograph；
Fig. 3 is composite negative pole (the carbon fibers Sb that antimony trisulfide coats carbon fiber2S3) XRD spectrum；
Fig. 4 is carbon fibers@Sb2S3Voltage-specific capacity curve；
Fig. 5 is carbon fibers@Sb2S3Cycle performance.
Specific embodiment
Below in conjunction with attached drawing and specific embodiment, the present invention is described in further detail, but the present invention is not limited to
Following embodiment.
Embodiment 1
Stibnite and carbon fiber are weighed according to mass ratio 1:1, is added in ball grinder, ball is added by ball material mass ratio 20:1
Pearl is ground, and ball-milling medium is added according to alcohol, material mass ratio 2:1.Start ball mill, 450r/min ball milling 4h is filtered after stopping
It is dry, obtain mixture.Fig. 1 is the scanning electron microscope (SEM) photograph of electric conduction of carbon fiber matrix used, it can be seen that the diameter of carbon fiber is
50-150nm, length are 1-10 μm.
Above-mentioned dry pack is placed in argon atmosphere, is warming up to 620 DEG C with 3 DEG C/min, and keep the temperature 5h, natural cooling
Afterwards, the stibnite of melting is attached on carbon fiber, and recrystallization forms nanoscale antimony trisulfide crystal grain, and thus obtains carbon fiber@
Stibnite composite negative pole.
Fig. 2 shows the scanning electron microscope (SEM) photograph of carbon fiber@stibnite composite negative pole, and by melting cooling procedure, stibnite exists
Carbon fiber surface recrystallizes to form nano particle or nanometer sheet, is coated on carbon fiber, and the partial size of nano particle and nanometer sheet
Less than 150nm.Carbon fiber substrate used, carbon fiber@stibnite composite negative pole X-ray diffraction detection (XRD) as shown in figure 3,
It can be seen that carbon fiber have apparent carbonaceous material peak position, obtained carbon fiber@stibnite composite negative pole have carbon peak and
Sb2S3Impurity component SiO in peak and stibnite2Peak.
Obtained carbon fiber@stibnite composite material is mixed with conductive agent, bonding agent according to mass ratio 9:0.5:0.5,
It prepares slurry and is fabricated to pole piece, be assembled into button cell with metal lithium sheet, test chemical property after standing a few houres.Fig. 4 is
Voltage-specific capacity curve of carbon fiber@stibnite composite negative pole, it can be seen that all there are two apparent in electric discharge and charging process
Platform, and platform stable illustrate that cathode electrochemical reversibility prepared by the present invention is good.Fig. 5 is carbon fiber@stibnite Compound Negative
The cycle performance figure of pole, the cathode first circle coulombic efficiency reach 83.3%, imitate already close to the head of commercial graphite.In 5Ag-1's
Under current density, 260 circle capacity of circulation can still reach 252.3mAhg-1, it is far superior to current that coulombic efficiency is maintained at 99.6
Commercialization graphite cathode.
Embodiment 2
High-purity antimony trisulfide and carbon fiber are weighed according to mass ratio 80:20, is added in ball grinder, by ball material mass ratio 15:1
Ball milling pearl is added, in air medium with 600r/min ball milling 1h, filtration drying after stopping obtains mixture.
Above-mentioned dry pack is placed in argon atmosphere, is warming up to 580 DEG C with 1 DEG C/min, and keep the temperature 10h, it is naturally cold
But after, the stibnite of melting is attached on carbon fiber, and recrystallization forms nanoscale antimony trisulfide crystal grain, and thus obtains carbon fiber
Tie up@stibnite composite negative pole.
Embodiment 3
Stibnite and carbon fiber are weighed according to mass ratio 10:90, is added in ball grinder, is added by ball material mass ratio 20:1
Ball milling pearl, with 400r/min ball milling 5h in argon medium, filtration drying after stopping obtains mixture.
Above-mentioned dry pack is placed in argon atmosphere, is warming up to 650 DEG C with 10 DEG C/min, and keep the temperature 5h, it is naturally cold
But after, the stibnite of melting is attached on carbon fiber, and recrystallization forms nanoscale antimony trisulfide crystal grain, and thus obtains carbon fiber
Tie up@stibnite composite negative pole.
Embodiment 4
Stibnite and carbon fiber are weighed according to mass ratio 80:20, water is added and is stirred, speed of agitator 500r/min,
Filtration drying after stirring 2h, obtains mixture.
Above-mentioned dry pack is placed in argon atmosphere, is warming up to 580 DEG C with 1 DEG C/min, and keep the temperature 10h, it is naturally cold
But after, the stibnite of melting is attached on carbon fiber, and recrystallization forms nanoscale antimony trisulfide crystal grain, and thus obtains carbon fiber
Tie up@stibnite composite negative pole.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (7)
1. a kind of prepare lithium ion battery carbon fiber/antimony trisulfide composite negative pole method, which comprises the following steps:
Antimony trisulfide and carbon fiber are mixed and dried；
Above-mentioned dry pack is placed in heating melting in inert atmosphere, and held for some time, rapid cooling or natural cooling
Afterwards, the stibnite of melting is attached on carbon fiber, recrystallization form nanoscale antimony trisulfide crystal grain, and thus obtain carbon fiber/
Antimony trisulfide composite negative pole；Wherein the diameter of carbon fiber is 50-150nm, and length is 1-10 μm；Antimony trisulfide is with nano particle or nanometer
Piece is coated on carbon fiber, and the size of antimony sulfide nano grain diameter or nanometer sheet is in 150nm or less.
2. according to claim 1 prepare lithium ion battery carbon fiber/antimony trisulfide composite negative pole method, feature exists
In antimony trisulfide used is the sulfide mineral or high-purity antimony trisulfide of stibnite or other metallic antimonies.
3. according to claim 1 prepare lithium ion battery carbon fiber/antimony trisulfide composite negative pole method, feature exists
In the mixed method of, antimony trisulfide, carbon fiber be ball milling, grinding or solution stirring.
4. according to claim 3 prepare lithium ion battery carbon fiber/antimony trisulfide composite negative pole method, feature exists
In ball milling and process of lapping include dry grinding and wet-milling, and dry grinding medium includes air or argon gas, and wet-milling and solution agitated medium include
Water or alcohol.
5. according to claim 4 prepare lithium ion battery carbon fiber/antimony trisulfide composite negative pole method, feature exists
In, when using ball milling mixing, ratio of grinding media to material 10:1-20:1, revolving speed 300-1200r/min, Ball-milling Time 0.5-10h；It adopts
When being stirred with solution, speed of agitator 300-1000r/min, time 0.5-10h.
6. according to claim 1 prepare lithium ion battery carbon fiber/antimony trisulfide composite negative pole method, feature exists
In the mass ratio that antimony trisulfide, carbon fiber mix is 95:5-10:90.
7. according to claim 1 prepare lithium ion battery carbon fiber/antimony trisulfide composite negative pole method, feature exists
In the temperature of antimony trisulfide and the melting of carbon fiber mixed material heating is 550-700 DEG C, soaking time 0.5-10h.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112072107A (en) * | 2020-08-28 | 2020-12-11 | 中南大学 | Antimony sulfide-based composite material and preparation method and application thereof |
| CN112186161A (en) * | 2020-09-30 | 2021-01-05 | 青岛科技大学 | Semi-filled one-dimensional nano longitudinal hole composite fiber membrane flexible electrode material and preparation method thereof |
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Cited By (4)
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|---|---|---|---|---|
| CN112072107A (en) * | 2020-08-28 | 2020-12-11 | 中南大学 | Antimony sulfide-based composite material and preparation method and application thereof |
| CN112072107B (en) * | 2020-08-28 | 2022-07-05 | 中南大学 | Antimony sulfide-based composite material and preparation method and application thereof |
| CN112186161A (en) * | 2020-09-30 | 2021-01-05 | 青岛科技大学 | Semi-filled one-dimensional nano longitudinal hole composite fiber membrane flexible electrode material and preparation method thereof |
| CN112186161B (en) * | 2020-09-30 | 2021-05-18 | 青岛科技大学 | Semi-filled one-dimensional nano longitudinal hole composite fiber membrane flexible electrode material and preparation method thereof |
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Effective date of registration: 20220525 Address after: 410000 block a, building 13, country garden wisdom Park, Xuehua village, bachelor street, Yuelu District, Changsha City, Hunan Province Patentee after: Hunan Enjie frontier New Material Technology Co.,Ltd. Address before: Yuelu District City, Hunan province 410083 Changsha Lushan Road No. 932 Patentee before: CENTRAL SOUTH University |