CN106549145A - A kind of application of vanadium phosphate cathode material of doping sulphur in lithium ion battery - Google Patents
A kind of application of vanadium phosphate cathode material of doping sulphur in lithium ion battery Download PDFInfo
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- CN106549145A CN106549145A CN201510591162.1A CN201510591162A CN106549145A CN 106549145 A CN106549145 A CN 106549145A CN 201510591162 A CN201510591162 A CN 201510591162A CN 106549145 A CN106549145 A CN 106549145A
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- lithium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
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Abstract
The present invention relates to a kind of application of the vanadium phosphate cathode material in lithium ion battery of doping sulphur, the positive electrode consists of Li3V2-xSx(PO4)3, wherein 0.01≤x≤0.15.As sulphur atom radius is more than vanadium, doping sulphur latter aspect can expand lithium ion transport channel, promote ion diffusion, on the other hand can maintain structural stability of the material in charge and discharge process.The positive electrode of the phosphoric acid vanadium lithium of doping sulphur electronic conductivity and ionic conductivity compared with the pure vanadium phosphate cathode material without doping are greatly improved；As the initial discharge specific capacity of lithium ion anode material, cycle performance and high rate performance are also greatly improved.
Description
Technical field
The present invention relates to a kind of vanadium phosphate cathode material of doping sulphur, belongs to electrochmical power source material and lithium
Ion battery field.
Background technology
Lithium ion battery has that specific energy is high, self discharge coefficient is little, has extended cycle life, lightweight
And advantages of environment protection, become the strong competition of electric automobile and hybrid vehicle power supply
Person.Common lithium ion power positive electrode has spinel lithium manganate, cobalt acid lithium and polyanion
Class positive electrode (LiMPO4, M=Mn, Fe, V etc.).Wherein, polyanionic ferric phosphate
Lithium (LiFePO4) have extended cycle life, it is safe, cheap, but there is electronic and ionic and lead
The defect such as electrically poor, lithium ion diffusion coefficient is low and heavy-current discharge characteristic is poor.It is all poly- the moon
Phosphoric acid vanadium lithium (the Li of ionic structure3V2(PO4)3) theoretical energy density reach 500mWh/g, compare
LiFePO4 has higher ion-electron electric conductivity, theoretical charge/discharge capacity and charging/discharging voltage
Platform, therefore there is in becoming lithium ion battery the positive electrode of very big application prospect.
But phosphoric acid vanadium lithium has the disadvantages that and hinders its practical application：(1) in synthesizing
V3+V is oxidized to easily5+It is difficult to obtain single-phase Li3V2(PO4)3；(2) lithium ion exists
Li3V2(PO4)3Middle diffusion difficulty causes the utilization rate of active material low；(3)Li3V2(PO4)3Itself
Electrical conductivity very low cause its heavy-current discharge performance poor；(4) high voltage cycle stability is poor.
Existing research improves Li by following approach3V2(PO4)3Performance：(1) adopt inertia
Gas shield V3+；(2) synthesize the Li of small particle3V2(PO4)3Come the Li for improving+Diffusivity；
(3) coated with carbon improves electronic conductivity；(4) doping improves the steady of electrical conductivity and structure
It is qualitative.
The content of the invention
It is an object of the invention to it is new modified just to have synthesized a kind of phosphoric acid vanadium lithium of sulfur doping
Pole material, and probe into its application in lithium ion battery.Technical problem to be solved is to provide
A kind of particle is uniform, electrical conductivity is high, discharge capacity is high, cycle performance is excellent, high-multiplying power discharge
The vanadium phosphate cathode material of the good doping of performance.
To realize object above, technical scheme is as follows：
The vanadium phosphate cathode material of doping sulphur consists of Li3V2-xSx(PO4)3, wherein 0.01≤x
≤0.15.Replace the V in phosphoric acid vanadium lithium using S as doped chemical part.
Concretely comprise the following steps：
(1) oxide or salt of oxalic acid and vanadium certain mol ratio is added equipped with deionized water
Beaker in, and stir under 70-80 DEG C of constant temperature to blue-tinted transparent solution, Ran Houyi
The secondary phosphoric acid vanadium lithium precursor sol for adding phosphorus source, sulphur source, lithium source to obtain doping sulphur；
Wherein：Li:V:S:PO3 4-Mol ratio be (3-3.3)：2：x：(3-x)(0.01≤x≤0.15)；
(2) colloidal sol of gained in (1) is put in 80-120 DEG C of baking oven and dries 5-10h,
Obtain xerogel；
(3) xerogel of presoma is calcined into 3-5h under the conditions of 300-400 DEG C, obtains pre- place
Reason material；
(4) material previously treated is calcined into 6-10h under the conditions of 700-850 DEG C, obtains sulfur doping
Phosphoric acid vanadium lithium；
Step (3) (4) is carried out in inert gas, and described inert gas is argon gas or nitrogen
One kind in gas.
The mol ratio of the oxide or salt of step (1) mesoxalic acid and vanadium is (3-5)：1；It is described
The oxide or salt of vanadium is the one kind in vanadic anhydride, ammonium vanadate or vanadium phosphate；Phosphorus source
For the one kind in diammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium phosphate, sodium phosphate；The sulphur source is
Ammonium sulfate or lithium sulfate；The lithium source be lithium carbonate, lithium hydroxide, lithium acetate, lithium nitrate,
One kind in lithium fluoride, lithium oxalate, described inert gas are nitrogen or the one kind in argon gas.
Beneficial effect
Sulphur atom radius is more than vanadium, and doping sulphur latter aspect can expand lithium ion transport channel, promote
Enter ion diffusion, on the other hand can maintain structural stability of the material in charge and discharge process.Mix
The positive electrode of the phosphoric acid vanadium lithium of miscellaneous sulphur and the pure vanadium phosphate cathode material phase without doping
It is more many than having the advantages that：(1) electronic conductivity and ionic conductivity are greatly improved；(2)
As the initial discharge specific capacity of lithium ion anode material, cycle performance and high rate performance are all obtained
Very big raising；
In preparation method, the method for modifying of this doping sulphur is simple, easy to operate, low cost,
And effect is substantially, with industrial prospect.
Description of the drawings
Fig. 1 is the sample and control sample of case study on implementation 1,2,3,4,5 in 3-4.8V conditions
100 cycle performance figures.
Specific embodiment
Embodiment 1
By the dissolving oxalic acid of 0.003mol in the beaker equipped with deionized water, it is subsequently adding
The vanadic anhydride of 0.001mol, stirs in blue solution in 70-80 DEG C of water bath with thermostatic control,
It is subsequently adding 0.00299mol ammonium dihydrogen phosphates, the ammonium sulfate of 0.00001mol, 0.0015mol
Lithium carbonate, continues the phosphoric acid vanadium lithium colloidal sol (Li that stirring forms glaucous doping:V:S:PO4 3-=3:2:
0.01:2.99).The colloidal sol is placed in baking 10h or so in 80 DEG C of baking ovens and obtains blue puffy forerunner
Body, is placed in tube furnace after the presoma is ground in powder, under argon atmosphere, with 3 DEG C
The programming rate of/min is warmed up to 350 DEG C and is incubated 4h, takes out grinding, continue with 3 DEG C after cooling
The programming rate of/min is raised to 750 DEG C and is incubated 10h, obtains the phosphoric acid vanadium lithium of 1% sulphur of doping
Composite powder.
Embodiment 2
By the dissolving oxalic acid of 0.003mol in the beaker equipped with deionized water, it is subsequently adding
The vanadic anhydride of 0.001mol, stirs in blue solution in 70-80 DEG C of water bath with thermostatic control,
It is subsequently adding 0.00297mol ammonium dihydrogen phosphates, the ammonium sulfate of 0.00003mol, 0.0015mol
Lithium carbonate, continues the phosphoric acid vanadium lithium colloidal sol that stirring forms glaucous doping
(Li:V:S:PO4 3-=3:2:0.03:2.97).The colloidal sol is placed in baking 10h or so in 80 DEG C of baking ovens to obtain
To blue puffy presoma, it is placed in tube furnace after the presoma is ground in powder, in argon
Under atmosphere is enclosed, 350 DEG C are warmed up to the programming rate of 3 DEG C/min and are incubated 4h, taken after cooling
Go out grinding, continue 750 DEG C to be warmed up to the programming rate of 3 DEG C/min and be incubated 10h, obtain
Adulterate the phosphoric acid vanadium lithium composite powder of 3% sulphur.
Embodiment 3
By the dissolving oxalic acid of 0.003mol in the beaker equipped with deionized water, it is subsequently adding
The vanadic anhydride of 0.001mol, stirs in blue solution in 70-80 DEG C of water bath with thermostatic control,
It is subsequently adding 0.00295mol ammonium dihydrogen phosphates, the ammonium sulfate of 0.00005mol, 0.0015mol
Lithium carbonate, continues the phosphoric acid vanadium lithium colloidal sol that stirring forms glaucous doping
(Li:V:S:PO4 3-=3:2:0.05:2.95).The colloidal sol is placed in baking 10h or so in 80 DEG C of baking ovens to obtain
To blue puffy presoma, it is placed in tube furnace after the presoma is ground in powder, in argon
Under atmosphere is enclosed, 350 DEG C are warmed up to the programming rate of 3 DEG C/min and are incubated 4h, taken after cooling
Go out grinding, continue 750 DEG C to be warmed up to the programming rate of 3 DEG C/min and be incubated 10h, obtain
Adulterate the phosphoric acid vanadium lithium composite powder of 5% sulphur.
Embodiment 4
By the dissolving oxalic acid of 0.003mol in the beaker equipped with deionized water, it is subsequently adding
The vanadic anhydride of 0.001mol, stirs in blue solution in 70-80 DEG C of water bath with thermostatic control,
It is subsequently adding 0.00293mol ammonium dihydrogen phosphates, the ammonium sulfate of 0.00003mol, 0.0015mol
Lithium carbonate, continues the phosphoric acid vanadium lithium colloidal sol that stirring forms glaucous doping
(Li:V:S:PO4 3-=3:2:0.07:2.93).The colloidal sol is placed in baking 10h or so in 80 DEG C of baking ovens to obtain
To blue puffy presoma, it is placed in tube furnace after the presoma is ground in powder, in argon
Under atmosphere is enclosed, 350 DEG C are warmed up to the programming rate of 3 DEG C/min and are incubated 4h, taken after cooling
Go out grinding, continue 750 DEG C to be warmed up to the programming rate of 3 DEG C/min and be incubated 10h, obtain
Adulterate the phosphoric acid vanadium lithium composite powder of 7% sulphur.
Embodiment 5
By the dissolving oxalic acid of 0.00285mol in the beaker equipped with deionized water, it is subsequently adding
The vanadic anhydride of 0.0095mol, stirs in blue molten in 70-80 DEG C of water bath with thermostatic control
Liquid, is subsequently adding the ammonium sulfate of 0.003mol ammonium dihydrogen phosphates, 0.0010mol, 0.0015mol
Lithium carbonate, continues the phosphoric acid vanadium lithium colloidal sol that stirring forms glaucous doping
(Li:V:S:PO4 3-=3:1.90:0.10:3).The colloidal sol is placed in baking 10h or so in 80 DEG C of baking ovens to obtain
To blue puffy presoma, it is placed in tube furnace after the presoma is ground in powder, in argon
Under atmosphere is enclosed, 350 DEG C are warmed up to the programming rate of 3 DEG C/min and are incubated 4h, taken after cooling
Go out grinding, continue 750 DEG C to be warmed up to the programming rate of 3 DEG C/min and be incubated 10h, adulterate
The phosphoric acid vanadium lithium composite powder of 10% sulphur.
Comparative example
By the dissolving oxalic acid of 0.003mol in the beaker equipped with deionized water, it is subsequently adding
The vanadic anhydride of 0.01mol, stirs in blue solution in 70-80 DEG C of water bath with thermostatic control,
0.03mol ammonium dihydrogen phosphates, 0.015mol lithium carbonates are subsequently adding, are continued stirring and is formed bluish-green
Phosphoric acid vanadium lithium colloidal sol (the Li of color:V:PO4 3-=3:2:3).The colloidal sol is placed in 80 DEG C of baking ovens and is dried
10h or so obtains blue puffy presoma, is placed in tubular type after the presoma is ground in powder
In stove, under argon atmosphere, 350 DEG C are warmed up to the programming rate of 3 DEG C/min and are incubated 4h,
Grinding is taken out after cooling, continues 750 DEG C to be warmed up to the programming rate of 3 DEG C/min and be incubated
10h, obtains Li in theory3V2(PO4)3Powder.
By embodiment 1,2,3,4,5 and composite obtained by comparative example, according to active material,
Conductive black, the mass ratio of binding agent three are 8:1:1 is dissolved in appropriate 1-METHYLPYRROLIDONE
Be well mixed, the electrode film that thickness is 0.15mm, vacuum drying are coated into wet film maker
It is cut into the electrode slice of a diameter of 12mm afterwards with slicer, weighs and calculate the matter of active material
Amount.Simultaneously using lithium piece as positive pole, using Clogard 2500 as barrier film, the LiPF of 1mol/L6
EC+DMC (volume ratio is 1:1) solution is electrolyte, in the glove box full of argon gas
In dress up button cell.Then the battery of assembling is carried out into electro-chemical test, in 3-4.3V and
Carry out electro-chemical test under 3-4.8V constant current conditions respectively.
The cyclical stability of the phosphoric acid vanadium lithium of doping sulphur is carried in right amount as can be seen from Figure 1
Height, the sulphur that reason is mainly adulterated are not involved in chemistry and appraise at the current rate, and can maintain stablizing for structure well
Property.
Claims (3)
1. application of a kind of vanadium phosphate cathode material of doping sulphur in lithium ion battery, its
It is characterised by：The vanadium phosphate cathode material of doping sulphur consists of Li3V2-xSx(PO4)3, wherein
0.01≤x≤0.15。
2. application according to claim 1, it is characterised in that concretely comprise the following steps
(1) by oxalic acid and the oxide or salt (3-5) of vanadium：1 mol ratio add equipped with go from
In the beaker of sub- water, and stir under 70-80 DEG C of constant temperature to blue-tinted transparent solution, so
The phosphoric acid vanadium lithium precursor sol that phosphorus source, sulphur source, lithium source obtain doping sulphur is sequentially added afterwards；
Wherein：Li:V:S:PO3 4-Mol ratio be (3-3.3)：2：x：(3-x)(0.01≤x≤0.15)；
(2) colloidal sol of gained in (1) is put in 80-120 DEG C of baking oven and dries 5-10h,
Obtain xerogel；
(3) xerogel of presoma is calcined into 3-5h under the conditions of 300-400 DEG C, obtains pre- place
Reason material；
(4) material previously treated is calcined into 6-10h under the conditions of 700-850 DEG C, obtains sulfur doping
Phosphoric acid vanadium lithium；
Step (3) (4) is carried out in inert gas, and described inert gas is argon gas or nitrogen
One kind in gas.
3. application according to claim 2, it is characterised in that：Step (1) vanadium
Oxide or salt be vanadic anhydride, ammonium vanadate or vanadium phosphate in one kind；Phosphorus source is
One kind in diammonium hydrogen phosphate, ammonium dihydrogen phosphate, potassium phosphate, sodium phosphate；The sulphur source is sulphur
Sour ammonium or lithium sulfate；The lithium source is lithium carbonate, lithium hydroxide, lithium acetate, lithium nitrate, fluorine
Change the one kind in lithium, lithium oxalate.
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Cited By (3)
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| CN108598473A (en) * | 2018-04-24 | 2018-09-28 | 电子科技大学 | Anion doped high-voltage charge and discharge vanadium phosphate cathode material and preparation method thereof |
| CN110504422A (en) * | 2019-07-29 | 2019-11-26 | 全球能源互联网研究院有限公司 | A kind of cell positive material and preparation method thereof |
| CN115050931A (en) * | 2022-05-24 | 2022-09-13 | 新疆师范大学 | Preparation method of nitrogen and sulfur co-doped carbon layer for coating positive electrode of sodium ion battery |
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| CN110504422A (en) * | 2019-07-29 | 2019-11-26 | 全球能源互联网研究院有限公司 | A kind of cell positive material and preparation method thereof |
| CN110504422B (en) * | 2019-07-29 | 2021-10-15 | 全球能源互联网研究院有限公司 | Battery positive electrode material and preparation method thereof |
| CN115050931A (en) * | 2022-05-24 | 2022-09-13 | 新疆师范大学 | Preparation method of nitrogen and sulfur co-doped carbon layer for coating positive electrode of sodium ion battery |
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Application publication date: 20170329 |