CN108242541A - A kind of preparation method of multi-level nano-structure lithium sulfur battery anode material - Google Patents
A kind of preparation method of multi-level nano-structure lithium sulfur battery anode material Download PDFInfo
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- CN108242541A CN108242541A CN201810013939.XA CN201810013939A CN108242541A CN 108242541 A CN108242541 A CN 108242541A CN 201810013939 A CN201810013939 A CN 201810013939A CN 108242541 A CN108242541 A CN 108242541A
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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
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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
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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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- Y02E60/10—Energy storage using batteries
Abstract
The present invention is based on nano tube structure as support, oxide nano-slice is grown by hydro-thermal reaction in nanotube and forms multi-level nano-structure, so as to fulfill effectively sulphur structure, then by carbon disulfide note sulphur, sulphur is injected in nanotube and obtains the lithium sulfur battery anode material admittedly.There is preparation method of the present invention raw material to be easy to get, is of low cost, is simple for process, is easy to operate, advantages of environment protection, entire reaction process does not need to special installation, conducive to industrialized production, it is higher to finally obtain product quality, entire reaction process requires Preparation equipment low, conducive to industrialized production, the multi-level nano-structure of preparation can realize the electric conductivity for inhibiting polysulfide dissolving and raising material, the ion diffusion rates of material simultaneously so that material has excellent high rate performance, high coulombic efficiency and the cycle performance stablized.
Description
Technical field
Present invention relates particularly to a kind of preparation methods of multi-level nano-structure lithium sulfur battery anode material, belong to new energy material
The preparing technical field of material.
Background technology
Lithium-sulfur cell is as a kind of very promising high-energy chemistry power supply, with electric vehicle and portable electronic device
High speed development, because its high theoretical specific capacity (1675m Ah/g) and high theoretical energy density (2600Wh/kg) cause
The extensive concern of various circles of society.The challenge however, opportunity invariably accompanies.Lithium-sulfur cell in charge and discharge process, generation it is solvable
Cathode of lithium is diffused in the polysulfide ion of the higher valence state of electrolyte, polysulfide of the generation compared with lower valency is reacted with lithium metal,
Anode is returned in the polysulfide back-diffusion of these lower valencies, the polysulfide of high-valence state is generated, so as to generate shuttle effect.Shuttle is imitated
The generation answered directly results in the reduction of utilization efficiency and the corrosion of cathode of lithium, circulating battery stability is made to be deteriorated, coulomb
Efficiency reduces.In addition, the conductivity of sulphur it is extremely low (at 25 DEG C, Ω=5 × 10-30S/cm), insoluble Li in charge and discharge process2S exists
Cathode deposition, the generation of cathode of lithium dendrite, just easily the factors such as volume expansion can all cause lithium-sulfur cell cyclical stability to be deteriorated to sulphur,
So as to restrict the commercial applications of lithium-sulfur cell.
Therefore, how effectively to inhibit the generation of polysulfide and diffuse into improve lithium-sulfur cell cycle life
One big approach, wherein, the selection of the sulfur-donor of lithium sulfur battery anode material just seems most important.The sulfur-donor needs following
Several features：(1) there are one close structures to prevent the shuttle effect of polysulfide；(2) there are one preferable conductivity with
Make up the insulating properties of sulphur；(3) there are one limited spaces to inhibit the volume change of sulphur, provide quick ion transmission.Therefore,
A kind of preparation method for the lithium sulfur battery anode material for effectively consolidating sulphur is explored to have important practical significance.The present invention passes through nanometer
The space physics confinement of pipe forms a unique multi-level nano-structure with oxide nano-slice, strengthens gathering sulfur molecule and more sulphur
The constraint effect of object, so as to inhibit the shuttle effect of polysulfide, mitigates the reduction of sulfur content in cyclic process reaction system, has
Improve the stable circulation performance of lithium-sulfur cell in effect ground.
Invention content
The object of the invention is exactly to overcome the problems of the above-mentioned prior art, provides a kind of multi-level nano-structure lithium sulphur
Cell positive material strengthens the effect of the constraint to sulfur molecule and more thiamers, inhibits the method for the shuttle effect of polysulfide, should
Method effectively inhibits the shuttle effect of polysulfide, improves the lithium-sulfur cell cycle longevity by a kind of unique multi-level nano-structure
Life, to meet currently the needs of to new energy materials.
The object of the invention can be achieved through the following technical solutions：
A kind of preparation method of multi-level nano-structure lithium sulfur battery anode material, includes the following steps：
(1) a certain proportion of precipitating reagent and metal salt are placed in the short chain alcohol of certain volume, 10~30 points of ultrasonic disperse
It is bell then to add in nanotube ultrasound 10~30 minutes into clear solution, it reacts 8~24 hours, obtains at 140~220 DEG C
The nanotube of hydroxide nano piece B modifications.
(2) the above-mentioned nanotube of centrifuge washing obtains for 2~10 hours in tube furnace under oxygen atmosphere in 300~700 DEG C of annealing
The multi-level nano-structure nanotube modified to oxide nano-slice.
(3) elemental sulfur is dissolved in carbon disulfide, ultrasonic disperse forms suspension, will be above-mentioned outstanding by way of vacuumizing
Turbid is extracted into multi-level nano-structure nanotube, and 155~285 DEG C of Low Temperature Heat Treatments 12~24 in Muffle furnace are put into after solvent evaporated
After hour, the composite material is just obtained after cooled to room temperature.
Precipitating reagent described above is urea, sodium hydroxide, potassium hydroxide, hexa, one kind in ammonium oxalate or
It is several；Metal salt is nickel acetate, nickel sulfate, nickel nitrate, n-butanol nickel, ferric acetate, ferric sulfate, ferric nitrate, n-butanol iron, acetic acid
One or more of cobalt, cobaltous sulfate, cobalt nitrate, n-butanol cobalt, manganese acetate, manganese sulfate, manganese nitrate, n-butanol manganese；Short chain alcohol
For one or more of ethyl alcohol, ethylene glycol, normal propyl alcohol, isopropanol, n-butanol, isobutanol mixed solvent；Nanotube is received for carbon
One or more of mitron, titania nanotube, vanadium oxide nanometer tube, tantalum oxide nanotube, niobium oxide nanotube.
Obtained multi-level nano-structure lithium sulfur battery anode material produced according to the present invention, structure novel can effectively inhibit
The dissolving of polysulfide and alleviation volume expansion, improve its chemical property, improve lithium-sulfur cell cycle life.
The present invention is based on nano tube structure as supporting, oxide nano-slice shape is grown by hydro-thermal reaction in nanotube
Into multi-level nano-structure, so as to fulfill effectively sulphur structure, then by carbon disulfide note sulphur, sulphur is injected in nanotube and is somebody's turn to do admittedly
Lithium sulfur battery anode material.There is preparation method of the present invention raw material to be easy to get, is of low cost, is simple for process, is easy to operate, environment is friendly
The advantages that good, entire reaction process do not need to special installation, and conducive to industrialized production, it is higher to finally obtain product quality, entirely
Reaction process is low to Preparation equipment requirement, and conducive to industrialized production, the multi-level nano-structure of preparation can be realized simultaneously inhibits more
Sulfide dissolves and the electric conductivity of raising material, the ion diffusion rates of material so that material has excellent high rate performance, height
Coulombic efficiency with stablize cycle performance.
Description of the drawings
Multi-level nano-structures of the Fig. 1 prepared by embodiment 1 consolidates the X-ray diffracting spectrum of sulphur nanotube；
Multi-level nano-structures of the Fig. 2 prepared by embodiment 2 consolidates the scanning electron microscope diagram of sulphur nanotube；
Multi-level nano-structures of the Fig. 3 prepared by embodiment 3 consolidates the transmission electron microscope figure of sulphur nanotube；
Fig. 4 is that the multi-level nano-structure prepared by embodiment 4 consolidates charge and discharge of the sulphur nanotube in the case where current density is 0.1C
Specific volume spirogram.
Specific embodiment
Below in conjunction with attached drawing, the present invention is described in detail, helps to understand the present invention, but the present invention is not limited merely to
Following embodiment.
Embodiment 1
(1) it is 5 by molar ratio:1 urea and cobalt acetate are placed in the isopropanol of certain volume, and ultrasonic disperse is formed for 10 minutes
Clear solution, then adds in titania nanotube ultrasound 20 minutes, is reacted 10 hours at 170 DEG C, obtains cobalt hydroxide and receive
The titania nanotube of rice piece modification.
(2) the above-mentioned titania nanotube of centrifuge washing obtains for 6 hours in tube furnace under oxygen atmosphere in 400 DEG C of annealing
The multi-level nano-structure titania nanotube modified to cobalt oxide nanometer sheet.
(3) elemental sulfur is dissolved in carbon disulfide, ultrasonic disperse forms suspension, will be above-mentioned outstanding by way of vacuumizing
Turbid is extracted into multi-level nano-structure titania nanotube, and 155 DEG C of Low Temperature Heat Treatments 12 in Muffle furnace are put into after solvent evaporated
After hour, the composite material is just obtained after cooled to room temperature.
Multi-level nano-structures of the Fig. 1 obtained by the present embodiment consolidates the X-ray diffracting spectrum of sulphur nanotube, can from figure
To find out that obtained material as pure phase, occurs without other phases and other impurity, and the well-crystallized of material.
Embodiment 2
(1) it is 6 by molar ratio:1 sodium hydroxide and manganese acetate are placed in the normal propyl alcohol of certain volume, ultrasonic disperse 10 minutes
Clear solution is formed, then adds in titania nanotube ultrasound 20 minutes, is reacted 14 hours at 190 DEG C, obtains hydroxide
The titania nanotube of manganese nanometer sheet modification.
(2) the above-mentioned titania nanotube of centrifuge washing obtains for 5 hours in tube furnace under oxygen atmosphere in 600 DEG C of annealing
The multi-level nano-structure titania nanotube modified to manganese oxide nanometer sheet.
(3) elemental sulfur is dissolved in carbon disulfide, ultrasonic disperse forms suspension, will be above-mentioned outstanding by way of vacuumizing
Turbid is extracted into multi-level nano-structure titania nanotube, and 185 DEG C of Low Temperature Heat Treatments 12 in Muffle furnace are put into after solvent evaporated
After hour, the composite material is just obtained after cooled to room temperature.
Multi-level nano-structures of the Fig. 2 obtained by the present embodiment consolidates the scanning electron microscope diagram of sulphur nanotube, from figure
As it can be seen that resulting materials are ordered arrangement structure.
Embodiment 3
(1) it is 5 by molar ratio:1 sodium hydroxide and cobalt acetate are placed in the ethylene glycol of certain volume, ultrasonic disperse 10 minutes
Clear solution is formed, then adds in carbon nanotube ultrasound 30 minutes, is reacted 8 hours at 200 DEG C, obtains cobalt hydroxide nanometer sheet
The carbon nanotube of modification.
(2) the above-mentioned carbon nanotube of centrifuge washing is aoxidized for 6 hours in tube furnace under oxygen atmosphere in 550 DEG C of annealing
The multi-level nano-structure carbon nanotube of cobalt nanometer sheet modification.
(3) elemental sulfur is dissolved in carbon disulfide, ultrasonic disperse forms suspension, will be above-mentioned outstanding by way of vacuumizing
Turbid is extracted into multi-level nano-structure carbon nanotube, and 155 DEG C of Low Temperature Heat Treatments are put into Muffle furnace after solvent evaporated after 24 hours,
Just the composite material is obtained after cooled to room temperature.
Multi-level nano-structures of the Fig. 3 obtained by the present embodiment consolidates the scanning electron microscope diagram of sulphur nanotube, from figure
As it can be seen that sulphur has been supported in nanotube, contemplated nanostructured is realized.
Embodiment 4
(1) it is 3 by molar ratio:1 ammonium oxalate and ferric nitrate are placed in the ethyl alcohol of certain volume, and ultrasonic disperse is formed for 20 minutes
Clear solution, then adds in vanadium oxide nanometer tube ultrasound 20 minutes, is reacted 8 hours at 220 DEG C, obtains iron hydroxide nanometer sheet
The vanadium oxide nanometer tube of modification.
(2) the above-mentioned vanadium oxide nanometer tube of centrifuge washing obtains for 4 hours in tube furnace under oxygen atmosphere in 700 DEG C of annealing
The multi-level nano-structure vanadium oxide nanometer tube of ferric oxide nano piece modification.
(3) elemental sulfur is dissolved in carbon disulfide, ultrasonic disperse forms suspension, will be above-mentioned outstanding by way of vacuumizing
Turbid is extracted into multi-level nano-structure vanadium oxide nanometer tube, and it is small that 165 DEG C of Low Temperature Heat Treatments 12 in Muffle furnace are put into after solvent evaporated
Shi Hou just obtains the composite material after cooled to room temperature.
Fig. 4 is that the multi-level nano-structure obtained by the present embodiment is consolidated the charge and discharge when current density is 0.1C of sulphur nanotube and followed
Ring performance map tests first discharge specific capacity 1245.6mAh g under 0.1C current densities-1, 30 times cycle after specific discharge capacity
It is maintained at 958.1mAh g-1。
Embodiment 5
(1) it is 8 by molar ratio:1 potassium hydroxide and nickel nitrate are placed in the ethyl alcohol of certain volume and isopropanol (v：V=1:1)
In, ultrasonic disperse forms clear solution in 10 minutes, then adds in tantalum oxide nanotube ultrasound 20 minutes, reacts 18 at 140 DEG C
Hour, obtain the tantalum oxide nanotube of nickel hydroxide nano piece modification.
(2) the above-mentioned tantalum oxide nanotube of centrifuge washing obtains for 10 hours in tube furnace under oxygen atmosphere in 300 DEG C of annealing
The multi-level nano-structure tantalum oxide nanotube of nickel oxide nano piece modification.
(3) elemental sulfur is dissolved in carbon disulfide, ultrasonic disperse forms suspension, will be above-mentioned outstanding by way of vacuumizing
Turbid is extracted into multi-level nano-structure tantalum oxide nanotube, and it is small that 160 DEG C of Low Temperature Heat Treatments 12 in Muffle furnace are put into after solvent evaporated
Shi Hou just obtains the composite material after cooled to room temperature.
Embodiment 6
(1) it is 7 by molar ratio:1 hexa and nickel nitrate are placed in the ethylene glycol of certain volume and isopropanol (v：v
=2:1) in, ultrasonic disperse forms clear solution in 10 minutes, then adds in nanotube ultrasound 20 minutes, and it is small that 8 are reacted at 220 DEG C
When, obtain the carbon nanotube of nickel hydroxide nano piece modification.
(2) the above-mentioned carbon nanotube of centrifuge washing is aoxidized for 7 hours in tube furnace under oxygen atmosphere in 600 DEG C of annealing
The multi-level nano-structure carbon nanotube of nickel nano film modification.
(3) elemental sulfur is dissolved in carbon disulfide, ultrasonic disperse forms suspension, will be above-mentioned outstanding by way of vacuumizing
Turbid is extracted into multi-level nano-structure carbon nanotube, and 245 DEG C of Low Temperature Heat Treatments are put into Muffle furnace after solvent evaporated after 12 hours,
Just the composite material is obtained after cooled to room temperature.
In conclusion a kind of preparation method of multi-level nano-structure lithium sulfur battery anode material of the present invention, this method are led to
The multi-level nano-structure nanotube for synthesizing nanometer sheet modification is crossed as sulfur-donor, strengthens the beam to sulfur molecule and more thiamers
Effect is tied up, effectively inhibit the dissolving of polysulfide and alleviates volume expansion, alleviates reaction system sulfur content in cyclic process
Reduction, improve its chemical property, further apply new energy field.
Claims (9)
1. a kind of preparation method of multi-level nano-structure lithium sulfur battery anode material, includes the following steps：
(1) a certain proportion of precipitating reagent and metal salt are placed in the short chain alcohol of certain volume, 10~30 minutes shapes of ultrasonic disperse
Into clear solution, nanotube ultrasound is then added in 10~30 minutes, reacted 8~24 hours at 140~220 DEG C, obtain hydrogen-oxygen
The nanotube of compound nanometer sheet B modifications.
(2) the above-mentioned nanotube of centrifuge washing obtains oxygen in 2~10 hours under oxygen atmosphere in tube furnace in 300~700 DEG C of annealing
The multi-level nano-structure nanotube of compound nanometer sheet modification.
(3) elemental sulfur is dissolved in carbon disulfide, ultrasonic disperse forms suspension, by above-mentioned suspension by way of vacuumizing
It is extracted into multi-level nano-structure nanotube, 155~285 DEG C of Low Temperature Heat Treatments is put into Muffle furnace after solvent evaporated 12~24 hours
Afterwards, the composite material is just obtained after cooled to room temperature.
2. preparation method as described in claim 1, it is characterised in that：The precipitating reagent be urea, sodium hydroxide, hydroxide
One or more of potassium, hexa, ammonium oxalate.
3. preparation method as described in claim 1, it is characterised in that：The metal salt be nickel acetate, nickel sulfate, nickel nitrate,
N-butanol nickel, ferric acetate, ferric sulfate, ferric nitrate, n-butanol iron, cobalt acetate, cobaltous sulfate, cobalt nitrate, n-butanol cobalt, manganese acetate,
One or more of manganese sulfate, manganese nitrate, n-butanol manganese.
4. preparation method as described in claim 1, it is characterised in that：The molar ratio of the precipitating reagent and metal salt for (3~
8):1。
5. preparation method as described in claim 1, it is characterised in that：The short chain alcohol is ethyl alcohol, and ethylene glycol, normal propyl alcohol is different
One or more of propyl alcohol, n-butanol, isobutanol mixed solvent.
6. preparation method as described in claim 1, it is characterised in that：The nanotube be carbon nanotube, nano titania
One or more of pipe, vanadium oxide nanometer tube, tantalum oxide nanotube, niobium oxide nanotube mixed solvent.
7. preparation method as described in claim 1, it is characterised in that：The reaction temperature is 140~220 DEG C；During reaction
Between be 8~24 hours.
8. preparation method as described in claim 1, it is characterised in that：The annealing temperature is 300~700 DEG C；During reaction
Between be 2~10 hours.
9. preparation method as described in claim 1, it is characterised in that：Reaction temperature is 155~285 in the Muffle furnace
℃；Drying time is 12~24 hours.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108987729A (en) * | 2018-08-29 | 2018-12-11 | 武汉科技大学 | A kind of lithium sulfur battery anode material and preparation method thereof and lithium-sulfur cell |
| CN109686953A (en) * | 2018-12-27 | 2019-04-26 | 杭州电子科技大学 | A kind of lithium-sulfur battery composite cathode material and preparation method thereof |
| CN110156081A (en) * | 2019-05-22 | 2019-08-23 | 合肥学院 | A kind of porous flake TiNb of negative electrode of lithium ion battery2O7Nanocrystalline preparation method |
| CN112103563A (en) * | 2020-08-11 | 2020-12-18 | 威海广泰空港设备股份有限公司 | Lithium-sulfur battery for airport service vehicle in alpine region and preparation method |
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2018
- 2018-01-08 CN CN201810013939.XA patent/CN108242541A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108987729A (en) * | 2018-08-29 | 2018-12-11 | 武汉科技大学 | A kind of lithium sulfur battery anode material and preparation method thereof and lithium-sulfur cell |
| CN108987729B (en) * | 2018-08-29 | 2020-07-21 | 武汉科技大学 | Lithium-sulfur battery positive electrode material, preparation method thereof and lithium-sulfur battery |
| CN109686953A (en) * | 2018-12-27 | 2019-04-26 | 杭州电子科技大学 | A kind of lithium-sulfur battery composite cathode material and preparation method thereof |
| CN110156081A (en) * | 2019-05-22 | 2019-08-23 | 合肥学院 | A kind of porous flake TiNb of negative electrode of lithium ion battery2O7Nanocrystalline preparation method |
| CN110156081B (en) * | 2019-05-22 | 2021-05-14 | 合肥学院 | Porous flaky TiNb for lithium ion battery cathode2O7Method for preparing nanocrystalline |
| CN112103563A (en) * | 2020-08-11 | 2020-12-18 | 威海广泰空港设备股份有限公司 | Lithium-sulfur battery for airport service vehicle in alpine region and preparation method |
| CN112103563B (en) * | 2020-08-11 | 2021-04-16 | 威海广泰空港设备股份有限公司 | Lithium-sulfur battery for airport service vehicle in alpine region and preparation method |
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Application publication date: 20180703 |