CN109817960A - A kind of anode material of lithium-ion battery, sodium-ion battery and preparation method thereof - Google Patents
A kind of anode material of lithium-ion battery, sodium-ion battery and preparation method thereof Download PDFInfo
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Abstract
The present invention discloses a kind of anode material of lithium-ion battery, sodium-ion battery and preparation method thereof, wherein the method includes the steps: it sulphur source and antimony source is dissolved in solvent is placed in homogeneous reactor and carry out primary heating, react and Sb is made2S3Nanometer rods；By Sb2S3Nanometer rods are scattered in alcohol, are added titanium salt and control system as neutral or alkalescent, are then carried out reheating, react and Sb is made2S3‑TiO2；By Sb2S3‑TiO2It is added in Tirs buffer solution with Dopamine hydrochloride, solid is taken after being sufficiently stirred and powder is made, is subsequently placed in inert gas atmosphere and calcines, carbon is restored and is wrapped in Sb2S3‑TiO2Surface obtains anode material of lithium-ion battery.Anode material of lithium-ion battery provided by the present invention not only increases the structural stability of material, it is suppressed that volume expansion, and the electric conductivity of material is also improved, so that the cyclical stability and high rate performance of material are improved.
Description
Technical field
The present invention relates to sodium-ion battery technical field more particularly to a kind of anode material of lithium-ion batteries, sodium ion electricity
Pond and preparation method thereof.
Background technique
Currently, it is abundant and cheap and have and lithium ion battery to have benefited from sodium content in the earth's crust for sodium-ion battery
Similar working principle and receive the concern of numerous scholars.In view of the research for developing promising positive electrode in recent years, promote
The cathode of suitable high capacity, high-speed, long-term cycle performance is a lack of into one of commercialized key challenge of sodium-ion battery
Material.People are to the carbonaceous materials such as hard carbon, hollow carbon sphere, carbon fiber and Sn, SnOx、SnO2、Bi0.94Sb1.06S3, the gold such as Sb
Category/metal chalcogenide compound has conducted extensive research as potential negative electrode material., operating potential unsafe carbonaceous low with energy storage
Negative electrode material is compared, and the cathode made of metal oxide/metal sulfide has been explored by more and more people, excellent to obtain
Different high rate performance and height ratio capacity, still, these negative electrode materials volume change in electrochemical reaction process is violent, is easy to lead
Structure is caused to be destroyed rapidly.
Therefore, the existing technology needs to be improved and developed.
Summary of the invention
In view of above-mentioned deficiencies of the prior art, the purpose of the present invention is to provide a kind of anode material of lithium-ion batteries, sodium
Ion battery and preparation method thereof, it is intended to solve in existing sodium-ion battery negative electrode material made of metal sulfide in electrochemistry
The problem of volume change is violent in reaction process, and material structure is easy to cause to be destroyed.
Technical scheme is as follows:
A kind of preparation method of anode material of lithium-ion battery, wherein comprising steps of
It sulphur source and antimony source is dissolved in solvent is placed in homogeneous reactor and carry out primary heating, react and Sb is made2S3Nanometer rods；
By Sb2S3Nanometer rods are scattered in alcohol, are added titanium salt and control system as neutral or alkalescent, are then carried out secondary add
Heat reacts and Sb is made2S3-TiO2；
By Sb2S3-TiO2It is added in Tirs buffer solution with Dopamine hydrochloride, solid is taken after being sufficiently stirred and powder is made, then
It is placed in inert gas atmosphere and calcines, carbon is restored and be wrapped in Sb2S3-TiO2Surface obtains sodium-ion battery cathode material
Material.
The preparation method of the anode material of lithium-ion battery, wherein the sulphur source is Sodium Sulphate Nine Hydroxide, thio second
One of amide, thiocarbamide and L-cysteine are a variety of.
The preparation method of the anode material of lithium-ion battery, wherein the antimony source is antimony trichloride or antimony acetate.
The preparation method of the anode material of lithium-ion battery, wherein the titanium salt is that butyl titanate or metatitanic acid are different
Propyl ester.
The preparation method of the anode material of lithium-ion battery, wherein the temperature of primary heating be 160-200 DEG C, when
Between be 8-16 h.
The preparation method of the anode material of lithium-ion battery, wherein the temperature of reheating is 35-55 DEG C, time
For 8-16 h.
The preparation method of the anode material of lithium-ion battery, wherein the solvent is the mixed of deionized water and ethyl alcohol
Bonding solvent.
The preparation method of the anode material of lithium-ion battery, wherein it is 8 ~ 9 that the Tirs, which buffers molten pH,.
The preparation method of the anode material of lithium-ion battery, wherein the control system is neutral or weakly alkaline
Step, including ammonium hydroxide, which is added, keeps system neutral or alkalescent.
The preparation method of the anode material of lithium-ion battery, wherein the calcination reaction temperature be 250-550 DEG C,
Time is 2-6 h.
A kind of anode material of lithium-ion battery, wherein be prepared by preparation method as described above.
A kind of sodium-ion battery, wherein including cathode, the cathode uses sodium-ion battery cathode material as described above
Material.
The utility model has the advantages that anode material of lithium-ion battery prepared by the present invention, in Sb2S3Surface is successively coated with TiO2And C
Layer, for the Sb with core-shell structure2S3-TiO2C composite has benefited from Sb2S3-TiO2The unique knot of C composite
Structure has excellent chemical property, coats Sb2S3TiO2Modified layer and carbon-coating not only increase the structural stability of material,
Volume expansion is inhibited, and also improves the electric conductivity of material, so that the cyclical stability and high rate performance of material are changed
It is kind.
Detailed description of the invention
Fig. 1 is Sb prepared by the embodiment of the present invention 12S3、Sb2S3-TiO2And Sb2S3-TiO2The Flied emission of C composite
Scanning electron microscope SEM figure；
Fig. 2 is Sb prepared by the embodiment of the present invention 12S3、Sb2S3-TiO2、Sb2S3-TiO2The XRD diagram of C composite；
Fig. 3 is Sb prepared by the embodiment of the present invention 12S3、Sb2S3-TiO2、Sb2S3-TiO2The cycle performance of C composite
Figure；
Fig. 4 is Sb prepared by the embodiment of the present invention 12S3、Sb2S3-TiO2、Sb2S3-TiO2The high rate performance of C composite
Figure.
Specific embodiment
The present invention provides a kind of anode material of lithium-ion battery, sodium-ion battery and preparation method thereof, of the invention to make
Purpose, technical solution and effect are clearer, clear, and the present invention is described in more detail below.It should be appreciated that this place is retouched
The specific embodiment stated is only used to explain the present invention, is not intended to limit the present invention.
The preparation method of anode material of lithium-ion battery of the present invention, comprising steps of
S1, it sulphur source and antimony source is dissolved in solvent is placed in homogeneous reactor and carry out primary heating, react and Sb is made2S3Nanometer
Stick；
S2, by Sb2S3Nanometer rods are scattered in alcohol, are added titanium salt and control system as neutral or alkalescent, are then carried out two
Secondary heating reacts and Sb is made2S3-TiO2；
S3, by Sb2S3-TiO2It is added in Tirs buffer solution with Dopamine hydrochloride, solid is taken after being sufficiently stirred and powder is made,
It is subsequently placed in inert gas atmosphere and calcines, carbon is restored and be wrapped in Sb2S3-TiO2Surface obtains sodium-ion battery cathode
Material.
The present invention generates antimonous sulfide nanometer rods first with sulphur source and the reaction of antimony source, then by Sb2S3Nanometer rods are uniformly divided
It dissipates in alcoholic solvent, recycles titanium salt and weak base reaction in Sb2S3Nanorod surfaces generate layer of titanium dioxide, to obtain
Sb2S3-TiO2, then using Dopamine hydrochloride in Sb2S3-TiO2Surface formed layer of surface carbon-coating, finally obtain with trithio
Change the Sb with core-shell structure that two antimony are core2S3-TiO2C composite.Wherein, antimonous sulfide (Sb2S3) because it often rubs
You are Sb2S3There are 946 mAh g containing 12 moles of sodium ions-1Reversible theoretical capacity, and due to Na2S phase is as buffering base
Matter and there is improved cycle performance, thus can be with volume expansion of the lightening material in cathode discharge and recharge reaction；And surface is wrapped
The TiO covered2The characteristic that modified layer and carbon-coating have stable structure, electric conductivity excellent, not only further enhances the knot of material
Structure stability inhibits volume expansion, and also improves the electric conductivity of material, so that the cyclical stability and high rate performance of material
Improved.
Specifically, in the step S1, sulphur source and antimony source are dissolved in the in the mixed solvent of deionized water and ethyl alcohol first,
It is then transferred into ptfe autoclave, progress primary heating reaction in homogeneous reactor is subsequently placed into, so that sulphur and antimony
Reaction generates Sb2S3Nanometer rods.Wherein, the temperature of primary heating is 160-200 DEG C, the time is 8-16 h, is more preferably 180 DEG C
And 12h is kept the temperature, to allow the sulphur in sulphur source sufficiently to react into Sb with the antimony in antimony source2S3, and control the Sb generated2S3In nanoscale.
The sulphur source is one of Sodium Sulphate Nine Hydroxide, thioacetamide, thiocarbamide and L-cysteine or a variety of, and the antimony source is three
Antimony chloride or antimony acetate；And the mixed solvent for dissolving sulphur source with antimony source simultaneously, it is preferable that control deionized water and second
The volume ratio of alcohol is (0-40): (40-0).
In the step S2, by Sb2S3Nanometer rods are dispersed in the alcoholic solvents such as ethyl alcohol, add titanium salt and control system is
Neutral or weak base state, then 35-55 DEG C at a temperature of carry out reheating and continue 8-16 h so that titanium salt is oxidized
And in Sb2S3Nanorod surfaces superscribe layer of titanium dioxide.Wherein, system can be made for neutral or weak base by the way that ammonium hydroxide is added
State；Preferably, a small amount of H is added in neutral or weak base condition2O or NaOH, to promote titanium salt to decompose.Preferably, the titanium salt
For butyl titanate or isopropyl titanate.In addition, in order to more fully by Sb2S3Nanometer rods are dispersed in the alcoholic solvents such as ethyl alcohol, can
30 ~ 60min is acted on to carry out ultrasonic disperse to system.
In the step S3, by Sb2S3-TiO2It is added in Tirs buffer solution with Dopamine hydrochloride, is taken after being sufficiently stirred
Surface aggregation has the Sb of poly-dopamine2S3-TiO2Solid, then the powder that diameter is 100-200 nm is made in grinding, then by powder
It is placed in inert gas atmosphere and calcines, the carbon in poly-dopamine is restored and be wrapped in Sb2S3-TiO2Surface obtains sodium ion
Cell negative electrode material.Preferably, first solid is cleaned and is dried before the milling, specifically respectively with deionized water and anhydrous
Ethyl alcohol cleans three times, and to remove the excessive poly-dopamine in surface, 8 h are then dried in 70 DEG C of air dry ovens.
Wherein, the buffer solution is three (methylol) aminomethane deionized water solutions, and adjust solution be pH be 8 ~
9, it can sufficiently allow poly-dopamine (PDA) in Sb2S3-TiO2The surface of solids carries out uniform self aggregation.Preferably, pH value of solution is adjusted
It is 8.5.
Calcination reaction temperature in the step S3 is 250-550 DEG C, the time is 2-6 h, and nano bar-shape can be made
Sb2S3-TiO2C composite, nanorod diameter are 100-200 nm.
Based on the above method, the present invention also provides a kind of anode material of lithium-ion batteries, wherein by making as described above
Preparation Method is prepared.
Based on the above method, the present invention also provides a kind of sodium-ion batteries, wherein including cathode, the cathode is used
Anode material of lithium-ion battery as described above.
It is described further combined with specific embodiments below.
Embodiment 1
(1) Sb2S3The preparation of nanometer rods: 0.9 g Sodium Sulphate Nine Hydroxide and 0.4 g antimony trichloride are dissolved in mixed solvent first
In 25 mL deionized waters and 15 mL ethyl alcohol, it is then transferred into ptfe autoclave, is subsequently placed into homogeneous reactor
180 DEG C of high temperature 12 h of reaction, obtain Sb2S3Nanometer rods；
(2) Sb is prepared2S3-TiO2Composite material: by 0.1 g Sb2S3Nanometer rods dispersion in ethanol ultrasound 30 minutes, then plus
Enter 0.4 mL butyl titanate and 0.2 mL ammonium hydroxide, 12 h are reacted at 45 DEG C, obtain Sb2S3-TiO2；
(3) Sb is prepared2S3-TiO2C composite: by 0.1 g Sb2S3-TiO2100 mL are dissolved in 0.2 g Dopamine hydrochloride
In 10mM Tirs buffer solution, 24 h are stirred, are centrifuged, are cleaned, it is dry；Product grind into powder is placed in tube furnace lazy
450 DEG C of high temperature 4 h of calcining under property atmosphere, obtain Sb2S3-TiO2C composite is the anode material of lithium-ion battery.
Sb prepared by embodiment 12S3、Sb2S3-TiO2、Sb2S3-TiO2- C carries out field emission scanning electron microscope respectively
Analysis, result are as shown in Figure 1.Fig. 1 (a, b) is Sb2S3Shape appearance figure under different amplification therefrom can significantly be seen
To Sb2S3Pattern be nanometer rods, diameter is about 100 nm；Fig. 1 (c, d) is Sb2S3-TiO2Composite material is in different times magnifications
Shape appearance figure under several therefrom can significantly see there is granular TiO2It is supported on Sb2S3In nanometer rods；Fig. 1 (e, f) is
Sb2S3-TiO2Shape appearance figure of the C composite under different amplification, therefrom it can clearly be seen that there is one layer of carbon-coating to be coated on
Sb2S3-TiO2Outside, diameter is about 200 nm.
Sb prepared by the present embodiment 12S3、Sb2S3-TiO2、Sb2S3-TiO2C composite carries out XRD analysis respectively,
As a result as shown in Figure 2.Sb obtained can be obviously observed in Fig. 22S3、Sb2S3-TiO2、Sb2S3-TiO2C composite exists
11.22°、15.64°、17.52°、22.27°、25.01°、29.24°、32.35°、33.39°、34.34°、35.52°、36.99°、
Diffraction maximum at 43.03 °, 53.04 ° and 54.19 ° respectively corresponds Sb2S3(1 1 0) of standard card PDF#42-1393,
( 0 2 0)、( 1 2 0)、( 2 2 0)、( 3 1 0) 、( 2 1 1)、( 2 2 1)、( 3 0 1)、( 3 1 1)、( 2
4 0), (2 3 1), (2 5 0), (5 3 1) and (1 3 2) crystal face；Sb2S3-TiO241.94 ° in C composite,
Diffraction maximum at 51.59 °, 65.91 ° and 68.53 ° respectively corresponds (1 1 0) of Sb standard card PDF#35-0732, (2
0 2), (1 1 6) and (1 2 2) crystal face, this is the reason of thermal reduction；Sb2S3-TiO2And Sb2S3-TiO2In C composite
TiO is not found2Peak be because of TiO2It is amorphous and content is seldom, the available verifying in XPS test；In general,
Sb obtained by embodiment 12S3、Sb2S3-TiO2And Sb2S3-TiO2Required by C composite is exactly us.
To Sb prepared by the present embodiment 12S3、Sb2S3-TiO2、Sb2S3-TiO2C composite carries out cycle performance respectively
Test, result is as shown in figure 3, by can see Sb in Fig. 32S3-TiO2C composite is in 200 mAg-1Current density under
Reversible specific capacity after 100 circle of circulation is 533.1 mAhg-1, hence it is evident that it is better than Sb2S3-TiO221.4 mAhg-1And Sb2S3's
30.1 mAhg-1.This is because Sb2S3-TiO2The special structure of C composite enhances the electric conductivity and stability of material.
To Sb prepared by the present embodiment 12S3、Sb2S3-TiO2、Sb2S3-TiO2The carry out high rate performance survey of C composite
Examination, result is schemed as shown in Figure 4, by can obviously observe Sb in 42S3-TiO2C composite and Sb2S3-TiO2And Sb2S3
It compares, 10 circles are recycled under different current densities higher capacity, and returns again after different current densities circulation
To 50 mAg-1When, capacity retention ratio 92% presents good high rate performance.TiO2It is swollen that modified layer alleviates material volume
Swollen, carbon-coating enhances the electric conductivity of material, this makes material show excellent performance in charge and discharge process.
Embodiment 2
(1) Sb2S3The preparation of nanometer rods: 0.9 g Sodium Sulphate Nine Hydroxide and 0.4 g antimony trichloride are dissolved in mixed solvent first
In 25 mL deionized waters and 15 mL ethyl alcohol, it is then transferred into ptfe autoclave, is subsequently placed into homogeneous reactor
180 DEG C of high temperature 12 h of reaction, obtain Sb2S3Nanometer rods；
(2) Sb is prepared2S3-TiO2Composite material: by 0.1g Sb2S3Nanometer rods dispersion in ethanol ultrasound 30 minutes, then plus
Enter 0.4 mL butyl titanate and 0.2 mL ammonium hydroxide, 12 h are reacted at 45 DEG C, obtain Sb2S3-TiO2；
(3) Sb is prepared2S3-TiO2C composite: by 0.1 g Sb2S3-TiO2100ml is dissolved in 0.2 g Dopamine hydrochloride
In 10mM Tirs buffer solution, 24 h are stirred, are centrifuged, are cleaned, it is dry；Product grind into powder is placed in tube furnace lazy
250 DEG C of high temperature 4 h of calcining under property atmosphere, obtain Sb2S3-TiO2C composite is the anode material of lithium-ion battery.
It is found through sem analysis, XRD analysis, cycle performance test and high rate performance test analysis, obtained by the present embodiment
Sb2S3-TiO2C composite equally has Sb2S3、TiO2, C three-decker, have good high rate performance, electric conductivity and
Height ratio capacity can alleviate the volume expansion of the material in charge and discharge process.
Embodiment 3
(1) Sb2S3The preparation of nanometer rods: 0.9 g Sodium Sulphate Nine Hydroxide and 0.4 g antimony trichloride are dissolved in mixed solvent first
In 25 mL deionized waters and 15 mL ethyl alcohol, it is then transferred into ptfe autoclave, is subsequently placed into homogeneous reactor
180 DEG C of high temperature 12 h of reaction, obtain Sb2S3Nanometer rods；
(2) Sb is prepared2S3-TiO2Composite material: by 0.1 g Sb2S3Nanometer rods dispersion in ethanol ultrasound 30 minutes, then plus
Enter 0.4 mL butyl titanate and 0.2 mL ammonium hydroxide, 12 h are reacted at 45 DEG C, obtain Sb2S3-TiO2；
(3) Sb is prepared2S3-TiO2C composite: by 0.1 g Sb2S3-TiO2100 mL are dissolved in 0.2 g Dopamine hydrochloride
In 10 mM Tirs buffer solutions, 24 h are stirred, are centrifuged, are cleaned, it is dry；Product grind into powder is placed in tube furnace lazy
350 DEG C of high temperature 4 h of calcining under property atmosphere, obtain Sb2S3-TiO2C composite is the anode material of lithium-ion battery.
It is found through sem analysis, XRD analysis, cycle performance test and high rate performance test analysis, obtained by the present embodiment
Sb2S3-TiO2C composite equally has Sb2S3、TiO2, C three-decker, have good high rate performance, electric conductivity and
Height ratio capacity can alleviate the volume expansion of the material in charge and discharge process.
Embodiment 4
(1) Sb2S3The preparation of nanometer rods: 0.9 g Sodium Sulphate Nine Hydroxide and 0.4 g antimony trichloride are dissolved in mixed solvent first
In 25 mL deionized waters and 15 mL ethyl alcohol, it is then transferred into ptfe autoclave, is subsequently placed into homogeneous reactor
180 DEG C of high temperature 12 h of reaction, obtain Sb2S3Nanometer rods；
(2) Sb is prepared2S3-TiO2Composite material: by 0.1 g Sb2S3Nanometer rods dispersion in ethanol ultrasound 30 minutes, then plus
Enter 0.4 mL butyl titanate and 0.2 mL ammonium hydroxide, 12 h are reacted at 45 DEG C, obtain Sb2S3-TiO2；
(3) Sb is prepared2S3-TiO2C composite: by 0.1 g Sb2S3-TiO2100 mL are dissolved in 0.2g Dopamine hydrochloride
In 10mM Tirs buffer solution, 24 h are stirred, are centrifuged, are cleaned, it is dry；Product grind into powder is placed in tube furnace lazy
550 DEG C of high temperature 4 h of calcining under property atmosphere, obtain Sb2S3-TiO2C composite is the anode material of lithium-ion battery.
It is found through sem analysis, XRD analysis, cycle performance test and high rate performance test analysis, obtained by the present embodiment
Sb2S3-TiO2C composite equally has Sb2S3、TiO2, C three-decker, have good high rate performance, electric conductivity and
Height ratio capacity can alleviate the volume expansion of the material in charge and discharge process.
In conclusion anode material of lithium-ion battery provided by the present invention, in Sb2S3Surface is successively coated with TiO2And C
Layer, for the Sb with core-shell structure2S3-TiO2C composite has benefited from Sb2S3-TiO2The unique knot of C composite
Structure has excellent chemical property, coats Sb2S3TiO2Modified layer and carbon-coating not only increase the structural stability of material,
Volume expansion is inhibited, and also improves the electric conductivity of material, so that the cyclical stability and high rate performance of material are changed
It is kind.
It should be understood that the application of the present invention is not limited to the above for those of ordinary skills can
With improvement or transformation based on the above description, all these modifications and variations all should belong to the guarantor of appended claims of the present invention
Protect range.
Claims (10)
1. a kind of preparation method of anode material of lithium-ion battery, which is characterized in that comprising steps of
It sulphur source and antimony source is dissolved in solvent is placed in homogeneous reactor and carry out primary heating, react and Sb is made2S3Nanometer rods；
By Sb2S3Nanometer rods are scattered in alcohol, are added titanium salt and control system as neutral or alkalescent, are then carried out secondary add
Heat reacts and Sb is made2S3-TiO2；
By Sb2S3-TiO2It is added in Tirs buffer solution with Dopamine hydrochloride, solid is taken after being sufficiently stirred and powder is made, then
It is placed in inert gas atmosphere and calcines, carbon is restored and be wrapped in Sb2S3-TiO2Surface obtains sodium-ion battery cathode material
Material.
2. the preparation method of anode material of lithium-ion battery according to claim 1, which is characterized in that the sulphur source is nine
One of hydrated sodium sulfide, thioacetamide, thiocarbamide and L-cysteine are a variety of, and the antimony source is antimony trichloride or acetic acid
Antimony, the titanium salt are butyl titanate or isopropyl titanate.
3. the preparation method of anode material of lithium-ion battery according to claim 1, which is characterized in that the temperature of primary heating
Degree is 160-200 DEG C, the time is 8-16 h.
4. the preparation method of anode material of lithium-ion battery according to claim 1, which is characterized in that the temperature of reheating
Degree is 35-55 DEG C, the time is 8-16 h.
5. the preparation method of anode material of lithium-ion battery according to claim 1, which is characterized in that the solvent is to go
The mixed solvent of ionized water and ethyl alcohol.
6. the preparation method of anode material of lithium-ion battery according to claim 1, which is characterized in that the Tirs buffering
Molten pH is 8 ~ 9.
7. the preparation method of anode material of lithium-ion battery according to claim 1, which is characterized in that the control system
Keep system neutral or alkalescent for neutral or weakly alkaline step, including addition ammonium hydroxide.
8. the preparation method of anode material of lithium-ion battery according to claim 1, which is characterized in that the calcination reaction
Temperature is 250-550 DEG C, the time is 2-6 h.
9. a kind of anode material of lithium-ion battery, which is characterized in that by any preparation method preparation of claim 1 ~ 8
At.
10. a kind of sodium-ion battery, which is characterized in that including cathode, the cathode uses sodium ion as claimed in claim 9
Cell negative electrode material.
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| CN110611087A (en) * | 2019-07-18 | 2019-12-24 | 山东大学 | Composite material with antimony or bismuth uniformly distributed in titanium-based compound and preparation method and application thereof |
| CN111525112A (en) * | 2020-04-30 | 2020-08-11 | 青岛尚东新能源科技有限责任公司 | Negative electrode material of sodium ion battery |
| CN112072107A (en) * | 2020-08-28 | 2020-12-11 | 中南大学 | Antimony sulfide-based composite material and preparation method and application thereof |
| CN116425139A (en) * | 2023-02-07 | 2023-07-14 | 江苏大学 | High-first-efficiency high-magnification hard carbon material and preparation method and application thereof |
| WO2023165041A1 (en) * | 2022-05-07 | 2023-09-07 | 常州大学 | Preparation method for porous tio2-based nanomaterial, and porous tio2-based nanomaterial and sodium-ion battery |
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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 |
| WO2023165041A1 (en) * | 2022-05-07 | 2023-09-07 | 常州大学 | Preparation method for porous tio2-based nanomaterial, and porous tio2-based nanomaterial and sodium-ion battery |
| CN116425139A (en) * | 2023-02-07 | 2023-07-14 | 江苏大学 | High-first-efficiency high-magnification hard carbon material and preparation method and application thereof |
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