CN109473673A - A kind of preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material - Google Patents
A kind of preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material Download PDFInfo
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- CN109473673A CN109473673A CN201811405457.5A CN201811405457A CN109473673A CN 109473673 A CN109473673 A CN 109473673A CN 201811405457 A CN201811405457 A CN 201811405457A CN 109473673 A CN109473673 A CN 109473673A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a kind of preparation methods of carbon compound phosphoric acid vanadium sodium lithium anode material, which is characterized in that the positive electrode is LixNa(3‑x)V2(PO4)3/ C includes the following steps: step 1: lithium source, sodium source, phosphorus source, vanadium source and hexamethylenetetramine is added to the container wherein the x is greater than 0 and x less than 3, deionized water is added again, liquid is transferred in hydro-thermal liner by stirring and dissolving later, adds deionized water in liner；Step 2: step 1 liner being sealed and is transferred in hydro-thermal outer lining, after in convection oven 12~48h of hydro-thermal, natural cooling obtain presoma；Step 3: carbon source is placed in step 2 presoma, stirring and dissolving；Step 4: step 3 liquid is dried, rear grind into powder, 4~5.5h of pre-burning at 300~345 DEG C, and 6~10.5h is calcined at 650~850 DEG C, and carbon compound phosphoric acid vanadium sodium lithium anode material is obtained after natural cooling.Carbon compound phosphoric acid vanadium sodium lithium material, carbon made from this method are evenly distributed, and pattern is graininess, and partial size is smaller, there is preferable chemical property.
Description
Technical field
Sodium-ion battery technical field of the present invention, in particular to a kind of preparation side of carbon compound phosphoric acid vanadium sodium lithium anode material
Method.
Background technique
Lithium ion battery is excellent by feat of high-energy density, low self-discharge, environmentally friendly, ideal operating voltage etc.
Gesture has become the energy source of the portable electronic products such as mobile phone, plate and electric car.With the development of the times, Science and Technology Day is different
The moon is new, and market is increasing to the demand of lithium ion battery, and lithium resource deficiency is increasingly becoming limiting lithium ion cell future hair
The lethal factor of exhibition.Find lithium ion battery substitute products urgently to adapt to the needs of future market.
Sodium and lithium are in same main group, there is identical physico-chemical property, and sodium resource distribution is extensive, it is simple to extract, relatively
There are apparent superiority of reserves and price advantage for lithium resource.Sodium-ion battery has similar working principle, and many exists
When the electrode material that performance of lithium ion battery is excellent in is applied to sodium-ion battery, good electrochemistry can be equally shown
Performance, and sodium-ion battery production can also directly continue to use the production equipment of lithium ion battery.
Vanadium phosphate sodium lithium has NASICON structure, is a kind of fast-ionic conductor as a kind of sodium-ion battery positive material
Material has Three-dimensional Open ion transport channel, has good ion transmission performance, but poor electric conductivity causes its performance
Poor chemical property out.The most common way for enhancing electrode material electric conductivity is carbon material.And electrode material and carbon are micro-
The compound uniformity coefficient for seeing scale will determine the final electric conductivity of composite material.
Summary of the invention
In order to solve the above-mentioned technical problem, the embodiment of the invention provides a kind of carbon compound phosphoric acid vanadium sodium lithium anode materials
Preparation method, the positive electrode are LixNa(3-x)V2(PO4)3/ C includes the following steps: wherein the x is greater than 0 and x less than 3
Step 1: lithium source, sodium are weighed according to the molar ratio of lithium in the chemical formula of carbon compound phosphoric acid vanadium sodium lithium, sodium, phosphorus and vanadium
Weighed lithium source, sodium source, phosphorus source and vanadium source are placed in container by source, phosphorus source and vanadium source, hexamethylenetetramine are added, then add
Add deionized water, liquid is transferred in hydro-thermal liner by stirring and dissolving later, addition deionized water to the 80% of liner volume；
Step 2: step 1 liner being sealed and is transferred in hydro-thermal outer lining, and the hydro-thermal outer lining is transferred to 185 later
12~48h of hydro-thermal in convection oven at~240 DEG C, natural cooling obtain intermediate fluid phase precursor；
Step 3: it weighs carbon source and is placed in step 2 presoma, dissolution is sufficiently stirred, obtains mixed solution；
Step 4: step 3 mixed solution is dried, by the solid abrasive of drying at powder, the pre-burning at 300~345 DEG C
4~5.5h, and 6~10.5h is calcined at 650~850 DEG C, carbon compound phosphoric acid vanadium sodium lithium anode material is obtained after natural cooling.
Further, the phosphorus source is at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate.
Further, the vanadium source is at least one of ammonium metavanadate, vanadyl oxalate, vanadic anhydride.
Further, the lithium source is at least one of lithium hydroxide, lithium carbonate, lithia, lithium peroxide.
Further, the sodium source is at least one of sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium oxide molybdena.
Further, the carbon source is citric acid, bad hematic acid, glucose, sucrose, maltose, at least one in starch
Kind.
Further, phosphorus: vanadium: lithium: the molar ratio of sodium and hexamethylenetetramine is 3:2:y:3-y:1~8, wherein the y
Greater than 0 and y is less than 3.
Further, the carbon source accounts for the 0~15% of gross mass.
The implementation of the embodiments of the present invention has the following beneficial effects:
1, preparation method is simply controllable, easily operated, reproducible, is easy to industrial production；
2, the prices of raw materials are cheap, from a wealth of sources；
3, vanadium phosphate sodium lithium consistency, the homogeneity for preparing out by intermediate liquid phase method are preferable；
4, the carbon compound phosphoric acid vanadium sodium lithium material prepared by intermediate fluid coupling carbon, carbon are evenly distributed；
5, the pattern of prepared carbon compound phosphoric acid vanadium sodium lithium is graininess, and partial size is smaller, there is preferable chemical property,
Preferable cyclicity, higher specific capacity and stable cycle life.
Detailed description of the invention
Fig. 1 is Li made in embodiment 22NaV2(PO4)3The SEM of/C-material schemes；
Fig. 2 is Li made in embodiment 22NaV2(PO4)3The cycle performance figure of/C-material；
Fig. 3 is Li made in embodiment 22NaV2(PO4)3The high rate performance figure of/C-material.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that the described embodiment is only a part of the embodiment of the present invention, instead of all the embodiments.Based on this
Embodiment in invention, those of ordinary skill in the art are obtained every other without making creative work
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1:
A kind of preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material, the positive electrode are LixNa(3-x)V2(PO4)3/
C includes the following steps: wherein the x is greater than 0 and x less than 3
Step 1: lithium source, sodium are weighed according to the molar ratio of lithium in the chemical formula of carbon compound phosphoric acid vanadium sodium lithium, sodium, phosphorus and vanadium
Weighed lithium source, sodium source, phosphorus source and vanadium source are placed in container by source, phosphorus source and vanadium source, hexamethylenetetramine are added, then add
Add deionized water, liquid is transferred in hydro-thermal liner by stirring and dissolving later, addition deionized water to the 80% of liner volume；
Step 2: step 1 liner being sealed and is transferred in hydro-thermal outer lining, and the hydro-thermal outer lining is transferred to 185 later
12~48h of hydro-thermal in convection oven at~240 DEG C, natural cooling obtain intermediate fluid phase precursor；
Step 3: it weighs carbon source and is placed in step 2 presoma, dissolution is sufficiently stirred, obtains mixed solution；
Step 4: step 3 mixed solution is dried, by the solid abrasive of drying at powder, the pre-burning at 300~345 DEG C
4~5.5h, and 6~10.5h is calcined at 650~850 DEG C, carbon compound phosphoric acid vanadium sodium lithium anode material is obtained after natural cooling.
Further, the phosphorus source is at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate.
Further, the vanadium source is at least one of ammonium metavanadate, vanadyl oxalate, vanadic anhydride.
Further, the lithium source is at least one of lithium hydroxide, lithium carbonate, lithia, lithium peroxide.
Further, the sodium source is at least one of sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium oxide molybdena.
Further, the carbon source is citric acid, bad hematic acid, glucose, sucrose, maltose, at least one in starch
Kind.
Further, phosphorus: vanadium: lithium: the molar ratio of sodium and hexamethylenetetramine is 3:2:y:3-y:1~8, wherein the y
Greater than 0 and y is less than 3.
Further, the carbon source accounts for the 0~15% of gross mass.
Embodiment 2:
A kind of preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material, the positive electrode are LixNa(3-x)V2(PO4)3/
C includes the following steps: wherein the x is greater than 0 and x less than 3
Step 1: the di(2-ethylhexyl)phosphate of 4mmol lithium hydroxide, 2mmol sodium bicarbonate, the ammonium metavanadate of 4mmol, 6mmol are weighed
Hydrogen ammonium, 4mmol hexamethylenetetramine into container, addition 30ml deionized water be sufficiently stirred 30min to its dissolution, later will
Liquid is transferred in hydro-thermal liner, addition deionized water to the 80% of liner volume；
Step 2: step 1 liner being sealed and is transferred in hydro-thermal outer lining, and the hydro-thermal outer lining is transferred to 185 later
Hydro-thermal 36h in convection oven at DEG C, natural cooling obtain intermediate fluid phase precursor；
Step 3: weighing 0.5g citric acid and be placed in step 2 presoma, and 30min is sufficiently stirred to its dissolution, is mixed
Close solution；
Step 4: step 3 mixed solution is placed in 70 DEG C of baking oven and is dried, by the solid abrasive of drying at powder
And place in the material boat, it moves into tube furnace, 345 DEG C of pre-burnings 4h, 750 DEG C of calcining 10h under the atmosphere of nitrogen.After natural cooling
Obtain Li2NaV2(PO4)3/ C-material.
Preferably, the y is 2, the phosphorus: vanadium: lithium: the molar ratio of sodium and hexamethylenetetramine is 3:2:2:1:2.
Further, the carbon source accounts for the 0~15% of gross mass.
To Li2NaV2(PO4)3/ C-material carry out SEM characterization, as seen from Figure 1, pattern be graininess, partial size compared with
It is small.By obtained Li2NaV2(PO4)3/ C-material, conductive agent acetylene black and binder Kynoar 7:2:1 in mass ratio
Ratio mixing, is made slurry by solvent of N-Methyl pyrrolidone, is coated uniformly on the aluminium foil of LITHIUM BATTERY, does at 60 DEG C
It is dry, it is cut into the disk that diameter is 14cm later, the dry 8h in 120 DEG C of vacuum drying oven.Positive plate is turned after natural cooling
It moves in argon gas glove box, is to electrode with metallic sodium, glass fibre membrane is diaphragm, is assembled into CR2025 button cell.It uses
LT2001A battery test system carries out electrochemical property test, and test voltage range is 3~3.9V.Fig. 2 shows 2 institute of embodiment
Li obtained2NaV2(PO4)3/ C is under the current density of 0.5C, first discharge specific capacity 103.3mAh/g, by preceding 3 circle
After the circulation of 0.5C, the 4th loop current is changed to 1C, and the specific discharge capacity for remaining 86.0mAh/g is recycled at the 50th time.Fig. 3 shows
Li obtained by embodiment 22NaV2(PO4)3/ C positive electrode material, after 0.5C, 1C, 2C, 5C return the circulation of 0.5C,
25th circulation also retains the specific discharge capacity of 99.2mAh/g, shows Li2NaV2(PO4)3The preferable electrochemistry of/C anode
Performance, preferable cyclicity and higher specific capacity.
Embodiment 3:
A kind of preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material, the positive electrode are LixNa(3-x)V2(PO4)3/
C includes the following steps: wherein the x is greater than 0 and x less than 3
Step 1: weigh 2mmol lithium hydroxide, 2mmol sodium carbonate, 2mmol V2O5,6mmol ammonium dihydrogen phosphate,
For the hexamethylenetetramine of 6mmol into container, 30min is sufficiently stirred to its dissolution, later by liquid in addition 30ml deionized water
It is transferred in hydro-thermal liner, addition deionized water to the 80% of liner volume；
Step 2: step 1 liner being sealed and is transferred in hydro-thermal outer lining, and the hydro-thermal outer lining is transferred to 185 later
Hydro-thermal 48h in convection oven at DEG C, natural cooling obtain intermediate fluid phase precursor；
Step 3: weighing 1g bad hematic acid and be placed in step 2 presoma, and 30min is sufficiently stirred to its dissolution, is mixed
Solution；
Step 4: step 3 mixed solution is placed in 65 DEG C of baking oven and is dried, by the solid abrasive of drying at powder
And place in the material boat, it moves into tube furnace, 300 DEG C of pre-burnings 4h, 850 DEG C of calcining 8h under the atmosphere of nitrogen.After natural cooling
Obtain LiNa2V2(PO4)3/ C-material.
Preferably, the y is 1, the phosphorus: vanadium: lithium: the molar ratio of sodium and hexamethylenetetramine is 3:2:1:2:3.
Further, the carbon source accounts for the 0~15% of gross mass.
By obtained LiNa2V2(PO4)3/ C-material, conductive agent acetylene black and binder Kynoar in mass ratio 7:
The ratio of 2:1 mixes, and slurry is made by solvent of N-Methyl pyrrolidone, is coated uniformly on the aluminium foil of LITHIUM BATTERY, at 60 DEG C
Lower drying is cut into the disk that diameter is 14cm later, the dry 8h in 120 DEG C of vacuum drying oven.It will be positive after natural cooling
Piece is transferred in argon gas glove box, is to electrode with metallic sodium, glass fibre membrane is diaphragm, is assembled into CR2025 button cell.
Electrochemical property test is carried out using LT2001A battery test system, test voltage range is 3~3.9V, in the electric current of 0.5C
Under density, first discharge specific capacity 100.3mAh/g, after the circulation of preceding 3 circle 0.5C, the 4th loop current is changed to 1C, the
It recycles for 50 times and to remain the specific discharge capacity of 83.0mAh/g, after 0.5C, 1C, 2C, 5C return the circulation of 0.5C, the
25 circulations also retain the specific discharge capacity of 97.2mAh/g, show LiNa2V2(PO4)3The preferable electrochemistry of/C anode
Can, preferable cyclicity and higher specific capacity.
Embodiment 4:
A kind of preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material, the positive electrode are LixNa(3-x)V2(PO4)3/
C includes the following steps: wherein the x is greater than 0 and x less than 3
Step 1: the V of 1.5mmol lithia, 1.5mmol sodium carbonate, 2mmol are weighed2O5, 6mmol diammonium hydrogen phosphate,
For the hexamethylenetetramine of 5mmol into container, 30min is sufficiently stirred to its dissolution, later by liquid in addition 30ml deionized water
It is transferred in hydro-thermal liner, addition deionized water to the 80% of liner volume；
Step 2: step 1 liner being sealed and is transferred in hydro-thermal outer lining, and the hydro-thermal outer lining is transferred to 200 later
For 24 hours, natural cooling obtains intermediate fluid phase precursor to hydro-thermal in convection oven at DEG C；
Step 3: weighing 0.5g sucrose and be placed in step 2 presoma, and 30min is sufficiently stirred to its dissolution, is mixed
Solution；
Step 4: step 3 mixed solution is placed in 65 DEG C of baking oven and is dried, by the solid abrasive of drying at powder
And place in the material boat, it moves into tube furnace, 340 DEG C of pre-burning 5.5h, 800 DEG C of calcining 10h, natural cooling under the atmosphere of nitrogen
After obtain Li1.5Na1.5V2(PO4)3/ C-material.
Preferably, the y is 1.5, the phosphorus: vanadium: lithium: the molar ratio of sodium and hexamethylenetetramine is 3:2:1.5:1.5:
2.5。
Further, the carbon source accounts for the 0~15% of gross mass.
By obtained Li1.5Na1.5V2(PO4)3/ C-material, conductive agent acetylene black and binder Kynoar press quality
Ratio mixing than 7:2:1, is made slurry by solvent of N-Methyl pyrrolidone, is coated uniformly on the aluminium foil of LITHIUM BATTERY,
It is dry at 60 DEG C, it is cut into the disk that diameter is 14cm later, the dry 8h in 120 DEG C of vacuum drying oven.It will after natural cooling
Positive plate is transferred in argon gas glove box, is to electrode with metallic sodium, and glass fibre membrane is diaphragm, is assembled into CR2025 button electricity
Pond.Electrochemical property test is carried out using LT2001A battery test system, test voltage range is 3~3.9V, in the electricity of 0.5C
Under current density, first discharge specific capacity 101.3mAh/g, after the circulation of preceding 3 circle 0.5C, the 4th loop current is changed to 1C,
50th circulation remains the specific discharge capacity of 82.9mAh/g, after 0.5C, 1C, 2C, 5C return the circulation of 0.5C,
25th circulation also retains the specific discharge capacity of 96.8mAh/g, shows Li1.5Na1.5V2(PO4)3The preferable electrification of/C anode
Learn performance, preferable cyclicity and higher specific capacity.
Above description sufficiently discloses a specific embodiment of the invention.It should be pointed out that being familiar with the field
Range of any change that technical staff does a specific embodiment of the invention all without departing from claims of the present invention.
Correspondingly, the scope of the claims of the invention is also not limited only to previous embodiment.
Claims (8)
1. a kind of preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material, which is characterized in that the positive electrode is
LixNa(3-x)V2(PO4)3/ C includes the following steps: wherein the x is greater than 0 and x less than 3
Step 1: lithium source, sodium source, phosphorus are weighed according to the molar ratio of lithium in the chemical formula of carbon compound phosphoric acid vanadium sodium lithium, sodium, phosphorus and vanadium
Weighed lithium source, sodium source, phosphorus source and vanadium source are placed in container by source and vanadium source, be added hexamethylenetetramine, then add from
Liquid is transferred in hydro-thermal liner by sub- water, stirring and dissolving later, addition deionized water to the 80% of liner volume；
Step 2: step 1 liner being sealed and is transferred in hydro-thermal outer lining, the hydro-thermal outer lining is transferred to 185 later~
12~48h of hydro-thermal in convection oven at 240 DEG C, natural cooling obtain intermediate fluid phase precursor；
Step 3: it weighs carbon source and is placed in step 2 presoma, dissolution is sufficiently stirred, obtains mixed solution；
Step 4: step 3 mixed solution is dried, by the solid abrasive of drying at powder, at 300~345 DEG C pre-burning 4~
5.5h, and 6~10.5h is calcined at 650~850 DEG C, carbon compound phosphoric acid vanadium sodium lithium anode material is obtained after natural cooling.
2. the preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material according to claim 1, which is characterized in that described
Phosphorus source is at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate, ammonium phosphate.
3. the preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material according to claim 1, which is characterized in that described
Vanadium source is at least one of ammonium metavanadate, vanadyl oxalate, vanadic anhydride.
4. the preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material according to claim 1, which is characterized in that described
Lithium source is at least one of lithium hydroxide, lithium carbonate, lithia, lithium peroxide.
5. the preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material according to claim 1, which is characterized in that described
Sodium source is at least one of sodium hydroxide, sodium carbonate, sodium bicarbonate, sodium oxide molybdena.
6. the preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material according to claim 1, which is characterized in that described
Carbon source is at least one of citric acid, bad hematic acid, glucose, sucrose, maltose, starch.
7. the preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material according to claim 1, which is characterized in that phosphorus: vanadium:
Lithium: the molar ratio of sodium and hexamethylenetetramine is 3:2:y:3-y:1~8, wherein the y is greater than 0 and y less than 3.
8. the preparation method of carbon compound phosphoric acid vanadium sodium lithium anode material according to claim 1, which is characterized in that the carbon
Source accounts for the 0~15% of gross mass.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114156470A (en) * | 2021-11-30 | 2022-03-08 | 电子科技大学 | Sodium-rich phase zinc vanadium sodium phosphate composite material, preparation and application thereof |
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2018
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114156470A (en) * | 2021-11-30 | 2022-03-08 | 电子科技大学 | Sodium-rich phase zinc vanadium sodium phosphate composite material, preparation and application thereof |
| CN114156470B (en) * | 2021-11-30 | 2023-04-25 | 电子科技大学 | Sodium-rich phase zinc-vanadium-sodium phosphate composite material, preparation and application |
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