CN109346646A - A kind of novel lithium sulphur battery diaphragm material, preparation method and application - Google Patents
A kind of novel lithium sulphur battery diaphragm material, preparation method and application Download PDFInfo
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- CN109346646A CN109346646A CN201811154611.6A CN201811154611A CN109346646A CN 109346646 A CN109346646 A CN 109346646A CN 201811154611 A CN201811154611 A CN 201811154611A CN 109346646 A CN109346646 A CN 109346646A
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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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 belongs to the technical fields of lithium-sulfur cell diaphragm material, it is related to the preparation method of lithium-sulfur cell sandwich material, relate more specifically to a kind of preparation method of bimetallic oxide doped graphene lithium-sulfur cell sandwich material, specially a kind of novel lithium sulphur battery diaphragm material, preparation method and application.The present invention is that one kind by one step hydro thermal method prepares NiMoO4, functional diaphragm material is prepared in conjunction with spray drying, to control the shuttle effect of more lithium sulfides in lithium-sulfur cell.It is prepared using simple test method and processing step with the bimetallic oxide doped graphene material that partial size is smaller and is evenly distributed, and using the rGO/NiMoO obtained of spray drying preparation4Material has novelty, rGO/NiMoO4With outstanding chemical property when film is as lithium-sulfur cell interlayer.
Description
Technical field
The invention belongs to the technical fields of lithium-sulfur cell diaphragm material, are related to the preparation method of lithium-sulfur cell sandwich material,
Relate more specifically to a kind of preparation method of bimetallic oxide doped graphene lithium-sulfur cell sandwich material, it is specially a kind of new
Type lithium-sulfur cell diaphragm material, preparation method and application.
Background technique
With the fast development in the fields such as mobile terminal, electric car and new energy development, the lithium that is widely used at present from
Sub- battery system has been increasingly difficult to meet various demands, in recent years the high-energy density secondary battery research based on lithium metal
Obtain unprecedented pay attention to.Lithium-sulfur cell is up to 2600wh kg due to theoretical energy density-1, resourceful and advantages of environment protection
It worldwide receives significant attention, is the main direction of studying of next-generation lithium battery.
Lithium-sulfur cell is made of sulphur anode composite, lithium anode and electrolyte between the two.Since elemental sulfur is electricity
The non-conductor of son, sulphur anode composite is generally made of elemental sulfur, conductive agent and polymeric binder, with commercial li-ion battery
The embedding lithium mechanism of the de- lithium-of anode is different, and lithium-sulfur cell sulphur anode is in charge and discharge process along with the solid-liquid of multistep complexity
Reaction, since elemental sulfur is in Charging state, lithium-sulfur cell brings into operation from electric discharge.Elemental sulfur is reduced into dissolves in first
The polysulfide S of electrolyten 2-(4≤n≤8), the chemical constituent of polysulfide not instead of single stable, by plurality of stable
The mixture of chemical constituent and the unstable component composition including free radical.It is vulcanize with the progress of discharge process more
Object is reduced further into the sulphion S of lower valency2-Or cross sulphion S2 2-, since over cure lithium and lithium sulfide are organic
Solubility in electrolyte is very low, therefore final discharging product can be in the form of solid-state lithium sulfide and over cure lithium in positive conductive
It is precipitated on skeleton.The change procedure of active material sulfur component is the inverse process of above-mentioned discharge process in charging process, this shows
A large amount of active materials are present in organic electrolyte in the form of soluble polysulfide in the charge and discharge process of lithium-sulfur cell.
Electrolyte (also known as " liquid anode ") containing polysulfide can not only occur in charge and discharge process in positive receiving and losing electrons
Electrochemical reaction can also be chemically reacted with the very strong lithium anode of reproducibility.It shows as putting certainly during discharge
Electric process causes active material utilization low；During the charging process, it is low to react generation with lithium anode for high-valence state polysulfide
Valence state polysulfide, lower valency polysulfide diffuse to anode be oxidized to high-valence state polysulfide spread back again cathode continue it is anti-
It answers.Whole process forms closed circulation, and external circuit shows apparent over-charging of battery process, and this phenomenon is referred to as " to shuttle and imitate
It answers ".
" shuttle effect " bring consequence be it is very serious, not only result in that battery capacity decaying is fast, and active material utilizes
Rate is low, and it is unstable to will cause the chemical property of volume expansion effect and battery in charge and discharge process.
In the prior art, the scheme for improving lithium-sulfur cell performance is by the method for filling, mixing or cladding by elemental sulfur
Mechanical compound, formation anode composite material, designed for thiopectic various is carried out with the porous material with high pore structure
Material of main part develops new electrolyte additive and other electrode protection strategies, so as to improve the lithium ion conductance of sulfur-based positive electrode
The cycle performance of rate and battery, however, shuttle effect is still inevitable.Moreover, in the production process, it is inevitable its it is high at
The harsh conditions such as this and complex process, this will seriously hinder the commercialization of lithium-sulfur cell.
Summary of the invention
It is an object of the present invention to provide a kind of bimetallic oxide doped graphene lithium sulphur for the problems in lithium-sulfur cell
The preparation method of battery sandwich material, specially a kind of novel lithium sulphur battery diaphragm material, preparation method and application.The present invention is
One kind preparing NiMoO by one step hydro thermal method4, functional diaphragm material is prepared in conjunction with spray drying, to control in lithium-sulfur cell
The shuttle effect of more lithium sulfides.
The technical solution of the present invention is as follows:
A kind of preparation method of novel lithium sulphur battery diaphragm material, the specific steps are as follows:
Step 1: preparing bimetallic oxide NiMoO4
Both 5-50mol/L nickel nitrate solution and 5-50mol/L sodium molybdate solution are mixed, it magnetic agitation 10-20 minutes, will be molten
Liquid is transferred to hydrothermal reaction kettle, sealing, in an oven 150-180 DEG C heat preservation 3-10 hours, after natural cooling, collects precipitating,
Rinsed with deionized water, in an oven 60-80 DEG C dry 6-12 hours to get arrive NiMoO4。
Step 2: preparation NiMoO4@rGO material
NiMoO after the first step is dried4Powder and 2mg/ml graphene are admixed together, by mixed solution ultrasound 1-2 hours,
And 10-20h is stirred, it is then spray-dried at 200-220 DEG C, collects the powder for being spray-dried out, NiMoO is made4@rGO
Material.
Step 3: preparation NiMoO4@rGO diaphragm material
By NiMoO made from second step4@rGO material and conductive black and PVDF, which are blended in nmp solution, grinds 30-60 points
Clock is subsequently coated on clean diaphragm, and 50-70 DEG C dries to get NiMoO4@rGO diaphragm material is arrived.
The features of the present invention is also:
The stirring is magnetic agitation, and revolving speed is 100~300r/min.
Preferably, in the first step, nickel nitrate: sodium molybdate is that molar ratio is 1:1-1:2.
Preferably, in second step, NiMoO4The molar ratio of powder and graphene is 2:1-3:1.
Preferably, in third step, by NiMoO4@rGO material and conductive black and PVDF are blended in nmp solution, quality
Than for NiMoO4@rGO material: conductive black: PVDF=6:1:1-9:1:1.
Preferably, in third step, wherein conductive black: the mass ratio of PVDF is 1:1.
Above-mentioned NiMoO4The preparation method of@rGO lithium-sulfur cell diaphragm material, wherein involved raw material pass through quotient
Purchase obtains.
A kind of novel lithium sulphur battery diaphragm material obtained using above-mentioned preparation method.
Application of the novel lithium sulphur battery diaphragm material that the present invention obtains in lithium-sulfur cell as lithium sulphur diaphragm.
The invention has the benefit that creativeness of the invention is to prepare using simple test method and processing step
Provide the bimetallic oxide doped graphene material that partial size is smaller and is evenly distributed, and being made using spray drying preparation
RGO/ NiMoO4Material has novelty, rGO/ NiMoO4With outstanding electrochemistry when film is as lithium-sulfur cell interlayer
Energy.
Detailed description of the invention
Present invention will be further explained below with reference to the attached drawings and examples.
Fig. 1 is that the scanning electron microscope of bimetallic oxide spray dosing grapheme material obtained by embodiment 1 is shone
Piece.
Charging and discharging capacity curve when Fig. 2 is the circulation of NiMoO4@rGO diaphragm cell 0.2C obtained by embodiment 1.
Fig. 3 is the NiMoO that comparative test one obtains4Specific discharge capacity circulation of diaphragm material when as battery diaphragm
Figure.
Fig. 4 is specific discharge capacity circulation figure of the obtained rGO diaphragm material of comparative test two when as battery diaphragm.
Specific embodiment
Below in conjunction with specific embodiments of the present invention, apparent and completion is carried out to technical solution of the present invention and is explained
It states.Described embodiment is only a part of the embodiments of the present invention, and is not whole, all in spirit and original of the invention
Within then, any modification, equivalent substitution, improvement and etc. done be should all be included in the protection scope of the present invention.
Graphene oxide (GO) of the present invention is to be synthesized using improved Hummers method from natural graphite, is passed through
GO is dispersed 1 hour in deionized water by ultrasonic treatment, concentration 2mg/ml.
Embodiment 1
Step 1: preparing bimetallic oxide NiMoO4
2mmol nickel nitrate is dissolved in 30mL deionized water, 2mmol sodium molybdate is dissolved in 30mL deionized water, the two mixing, magnetic force
Stirring 10 minutes, transfers the solution into 100mL hydrothermal reaction kettle, seals, and 6 hours is kept the temperature for 150 DEG C in an oven, to naturally cold
But after, precipitating is collected, is rinsed with deionized water, 60 DEG C of drying 12 hours are in an oven to get to NiMoO4。
Step 2: preparation NiMoO4@rGO
Powder (1g) and the graphene (concentration 2mg/ml) of 200mL after the first step is dried is admixed together.By above-mentioned mixing
Solution ultrasound 1 hour, and stir 10h and then be spray-dried at 200 DEG C.The powder for being spray-dried out is collected, is made
NiMoO4@rGO material.
Step 3: preparation NiMoO4@rGO diaphragm material
The pvdf of the conductive black and 0.1 g of NiMoO4@rGO material made from 0.7g second step and 0.1g is blended in NMP
It grinds 30 minutes, is subsequently coated on clean diaphragm in solution, 50 DEG C dry to get NiMoO is arrived4@rGO diaphragm material.
It is that lithium sulphur electrolyte, NiMoO are added to electrode and reference electrode with lithium metal using bright sulfur as positive electrode4@rGO
Diaphragm material is diaphragm, and CR2025 button cell is assembled in the glove box full of argon gas.
Fig. 1 is that the scanning electron microscope of bimetallic oxide spray dosing grapheme material obtained by embodiment 1 is shone
Piece.It can be clearly seen that from Fig. 1, bimetallic oxide is oxidized graphene and coats completely, rGO/ NiMoO4Material
For nanoscale microballoon, this will provide good lead for the transmission of lithium-sulfur cell intermediate ion to (NiMoO4@rGO diaphragm material) shape
Electrically, while bimetallic ion can also cooperate with, and adsorb polysulfide together, play to the shuttle effect of lithium-sulfur cell polysulfide
Good inhibiting effect.
Fig. 2 is NiMoO4Charging and discharging capacity curve when@rGO diaphragm cell 0.2C is recycled.From figure 2 it can be seen that
In this rGO/ NiMoO4When material is as lithium-sulfur cell diaphragm material, initial capacity is up to 1410mAg h-1, coulombic efficiency is also several
It is 100%.It is readily apparent that, NiMoO4@rGO interlayer plays the role of inhibiting well the shuttle of polysulfide, improves electricity
The chemical property in pond.
Embodiment 2
Step 1: preparing bimetallic oxide NiMoO4
3 mmol nickel nitrates are dissolved in 40 mL deionized waters, 3 mmol sodium molybdates are dissolved in 35mL deionized water, and the two mixes,
Magnetic agitation 15 minutes, 100mL hydrothermal reaction kettle is transferred the solution into, is sealed, 5 hours are kept the temperature for 165 DEG C in an oven, to certainly
After so cooling, precipitating is collected, is rinsed with deionized water, 70 DEG C of drying 8 hours are in an oven to get to NiMoO4。
Step 2: preparation NiMoO4@rGO material
Powder (1.5g) and the graphene (concentration 2mg/ml) of 350mL after the first step is dried is admixed together.It will be above-mentioned mixed
It closes solution ultrasound 1.5 hours, and stirs 15h and then be spray-dried at 210 DEG C.The powder for being spray-dried out is collected, is made
NiMoO4@rGO material.
Step 3: preparation NiMoO4@rGO diaphragm material
The NiMoO4@rGO material and the conductive black of 0.1g and the pvdf of 0.1g of 0.8g are blended in nmp solution and are ground
It 40 minutes, is subsequently coated on clean diaphragm, 60 DEG C dry to get NiMoO is arrived4@rGO diaphragm material.
It is that lithium sulphur electrolyte, NiMoO are added to electrode and reference electrode with lithium metal using bright sulfur as positive electrode4@rGO
Diaphragm material is diaphragm, and CR2025 button cell is assembled in the glove box full of argon gas.
Embodiment 3
Step 1: preparing bimetallic oxide NiMoO4
4 mmol nickel nitrates are dissolved in 50 mL deionized waters, 4 mmol sodium molybdates are dissolved in 40mL deionized water, and the two mixes,
Magnetic agitation 20 minutes, 100mL hydrothermal reaction kettle is transferred the solution into, is sealed, 4 hours are kept the temperature for 180 DEG C in an oven, to certainly
After so cooling, precipitating is collected, is rinsed with deionized water, 80 DEG C of drying 6 hours are in an oven to get to NiMoO4。
Step 2: preparation NiMoO4@rGO material
Powder (2g) and the graphene (concentration 2mg/ml) of 500mL after the first step is dried is admixed together.By above-mentioned mixing
Solution ultrasound 2 hours, and stir 10h and then be spray-dried at 220 DEG C.The powder for being spray-dried out is collected, is made
NiMoO4@rGO material.
Step 3: preparation NiMoO4@rGO diaphragm material
The NiMoO4@rGO material and the conductive black of 0.1g and the pvdf of 0.1g of 0.9g are blended in nmp solution and are ground
It 60 minutes, is subsequently coated on clean diaphragm, 70 DEG C dry to get NiMoO is arrived4@rGO barrier material film.
It is that lithium sulphur electrolyte, NiMoO are added to electrode and reference electrode with lithium metal using bright sulfur as positive electrode4@rGO
Diaphragm material is diaphragm, and CR2025 button cell is assembled in the glove box full of argon gas.
In order to protrude the outstanding advantages of material of the invention, following two comparative experiments is provided.
Comparative test one: NiMoO4Diaphragm and NiMoO4@rGO diaphragm compares.
2mmol nickel nitrate is dissolved in 30mL deionized water, 2 mmol sodium molybdates are dissolved in 30mL deionized water, and the two is mixed
It closes, magnetic agitation 10 minutes, transfers the solution into 100mL hydrothermal reaction kettle, seal, keep the temperature 6 hours for 150 DEG C in an oven, to
After natural cooling, precipitating is collected, is rinsed with deionized water, 60 DEG C of drying 12 hours are in an oven to get to NiMoO4。
The pvdf of the conductive black and 0.1 g of the NiMoO4 material of 0.7g and 0.1g is blended in nmp solution and is ground
It 30 minutes, is subsequently coated on clean diaphragm, 50 DEG C dry to get NiMoO is arrived4Diaphragm material.
It is that lithium sulphur electrolyte, NiMoO are added to electrode and reference electrode with lithium metal using bright sulfur as positive electrode4Diaphragm
Material is diaphragm, and CR2025 button cell is assembled in the glove box full of argon gas.
It can be seen in figure 3 that NiMoO4Effect is very bad in terms of shuttle in inhibiting to vulcanize more for diaphragm material, at the beginning of battery
Beginning capacity only 610mAh/g, well below NiMoO4The capacity of the 1400mAh/g of@rGO diaphragm, this also illustrates do not restoring
Under conditions of graphene oxide provides high conductivity, simple NiMoO4The channel that the transmission of lithium ion may be blocked, leads to capacity
It is not high.
Two: rGO diaphragm of comparative test and NiMoO4@rGO diaphragm compares.
By graphene (concentration 2mg/ml) solution ultrasound 2 hours of 500mL, and stirs 10h and then done by spraying at 220 DEG C
It is dry.Collect the powder for being spray-dried out, as rGO material.
The pvdf of the conductive black and 0.1 g of the rGO material of 0.7g and 0.1g is blended in nmp solution and grinds 30 points
Clock is subsequently coated on clean diaphragm, and 50 DEG C dry to get rGO diaphragm material is arrived.
It is that lithium sulphur electrolyte, rGO diaphragm material are added to electrode and reference electrode with lithium metal using bright sulfur as positive electrode
Material is diaphragm, and CR2025 button cell is assembled in the glove box full of argon gas.
It can be seen from figure 4 that effect is very bad in terms of shuttle in inhibiting to vulcanize more for rGO diaphragm material, battery is initial
Capacity only 580mAh/g, well below NiMoO4The capacity of the 1400mAh/g of@rGO diaphragm, this also illustrates in no NiMoO4
Under conditions of providing in efficient absorption vulcanizes more, simple rGO is difficult to adsorb staying lithiums well more, leads to sulfur electrode active matter
The utilization rate of matter reduces, and more lithium sulfides cannot be dissolved in electrolyte to be deposited on lithium anode surface, further reduces lithium
The performance of sulphur battery.
Claims (8)
1. a kind of preparation method of novel lithium sulphur battery diaphragm material, the specific steps are as follows:
Step 1: preparing bimetallic oxide NiMoO4
Both 5-50mol/L nickel nitrate solution and 5-50mol/L sodium molybdate solution are mixed, it magnetic agitation 10-20 minutes, will be molten
Liquid is transferred to hydrothermal reaction kettle, sealing, in an oven 150-180 DEG C heat preservation 3-10 hours, after natural cooling, collects precipitating,
Rinsed with deionized water, in an oven 60-80 DEG C dry 6-12 hours to get arrive NiMoO4；
Step 2: preparation NiMoO4@rGO material
NiMoO after the first step is dried4Powder and 2mg/ml graphene are admixed together, by mixed solution ultrasound 1-2 hours,
And 10-20h is stirred, it is then spray-dried at 200-220 DEG C, collects the powder for being spray-dried out, NiMoO is made4@rGO
Material；
Step 3: preparation NiMoO4@rGO diaphragm material
By NiMoO made from second step4@rGO material and conductive black and PVDF, which are blended in nmp solution, grinds 30-60 points
Clock is subsequently coated on clean diaphragm, and 50-70 DEG C dries to get NiMoO4@rGO diaphragm material is arrived.
2. the preparation method of novel lithium sulphur battery diaphragm material according to claim 1, which is characterized in that the stirring
It is magnetic agitation, revolving speed is 100~300r/min.
3. the preparation method of novel lithium sulphur battery diaphragm material according to claim 1, which is characterized in that in the first step,
Nickel nitrate: sodium molybdate is that molar ratio is 1:1-1:2.
4. the preparation method of novel lithium sulphur battery diaphragm material according to claim 1, which is characterized in that in second step,
NiMoO4The molar ratio of powder and graphene is 2:1-3:1.
5. the preparation method of novel lithium sulphur battery diaphragm material according to claim 1, which is characterized in that in third step,
By NiMoO4@rGO material and conductive black and PVDF are blended in nmp solution, mass ratio NiMoO4@rGO material: conductive
Carbon black: PVDF=6:1:1-9:1:1.
6. the preparation method of novel lithium sulphur battery diaphragm material according to claim 5, which is characterized in that in third step,
Wherein conductive black: the mass ratio of PVDF is 1:1.
7. a kind of preparation method using novel lithium sulphur battery diaphragm material described in the claims 1-6 any claim
Obtained novel lithium sulphur battery diaphragm material.
8. the preparation method of novel lithium sulphur battery diaphragm material according to any claim from 1 to 6 obtains new
Application of the type lithium-sulfur cell diaphragm material in lithium-sulfur cell as lithium sulphur diaphragm.
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| CN109950508A (en) * | 2019-04-08 | 2019-06-28 | 朱焕光 | A kind of carbon cloth flexible lithium ion battery negative electrode material and preparation method thereof |
| CN110739428A (en) * | 2019-10-29 | 2020-01-31 | 肇庆市华师大光电产业研究院 | Preparation method of functional diaphragm of lithium-sulfur battery |
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| CN109950508A (en) * | 2019-04-08 | 2019-06-28 | 朱焕光 | A kind of carbon cloth flexible lithium ion battery negative electrode material and preparation method thereof |
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| CN110739428A (en) * | 2019-10-29 | 2020-01-31 | 肇庆市华师大光电产业研究院 | Preparation method of functional diaphragm of lithium-sulfur battery |
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| CN109346646B (en) | 2021-12-28 |
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