CN101339992A - Preparation of lithium ionic cell positive electrode material vanadium lithium silicate - Google Patents
Preparation of lithium ionic cell positive electrode material vanadium lithium silicate Download PDFInfo
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- CN101339992A CN101339992A CNA2008101177018A CN200810117701A CN101339992A CN 101339992 A CN101339992 A CN 101339992A CN A2008101177018 A CNA2008101177018 A CN A2008101177018A CN 200810117701 A CN200810117701 A CN 200810117701A CN 101339992 A CN101339992 A CN 101339992A
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Abstract
The invention discloses a preparation method of lithium vanadium silicate of anode material of a lithium-ion battery, which belongs to the technical field of energy material preparation. The preparation method comprises the following steps: a lithium source, a vanadium source, a silicon source and a carbon source are made into a precursor by sol-gel reaction, after being dried, the precursor is made into lithium vanadium silicate powder after heat treatment for 8-48 hours at the high temperature of 600-900 DEG C under the protection of inert gas and reducing gas atmosphere. The lithium vanadium silicate powder consists of nano-grade particles, and has good conductivity and high specific capacity. When the lithium vanadium silicate is in 1C multiplying factor, in the charging and discharging range of 3-4.8V, the reversible specific capacity is larger than 160mAh/g, and in the charging and discharging range of 1.5-4.8V, the reversible specific capacity is larger than 285mAh/g. The lithium vanadium silicate has good cycle performance and application prospect.
Description
Technical field
The invention belongs to the energy and material technical field.Be particularly related to a kind of preparation method of lithium ionic cell positive electrode material vanadium lithium silicate.
Background technology
Lithium ion battery is the green high-capacity battery of a new generation, numerous advantages such as have that voltage height, energy density are big, good cycle, self discharge are little, memory-less effect, operating temperature range are wide, be widely used in mobile phone, notebook computer, UPS, video camera, various portable power tool, electronic instrument, weaponry etc., in electric automobile, also have a good application prospect, be considered to be in 21st century national economy and the significant new high-tech product of people's lives.
Positive electrode is the important component part of lithium ion battery.At present, most research work concentrate on the lithium intercalation compound of period 4 Ti, V, Mn, Fe, Co, six kinds of variable valency transition metals of Ni.First generation positive electrode is a metal sulfide, as TiS
2, MoS
2Deng.Second generation positive electrode is lithium-compound transition metal oxide, with LiCoO
2For representative, comprise LiNiO
2, LiMnO
2, LiMn
2O
4, LiV
3O
8, LiNi
xCo
1-xO
2, LiNi
1/3Co
1/3Mn
1/3O
2And various derivatives.LiCoO
2Be the positive electrode of large-scale commercial, the research comparative maturity, high comprehensive performance, but cost an arm and a leg, capacity is lower, and toxicity is bigger, has certain safety issue, and expectation will be replaced by the new material of high-performance and low-cost.LiNiO
2Cost is lower, and capacity is higher, but the preparation difficulty, there are comparatively serious safety problem in the consistency of material property and poor reproducibility.Spinelle LiMn
2O
4Cost is low, and fail safe is good, but cycle performance especially high temperature cyclic performance is poor, certain dissolubility is arranged in electrolyte, storge quality is poor.The research and development novel anode material becomes current focus.Third generation positive electrode is with LiFePO4 (LiFePO
4) for the polyanion type compound-material of representative.Polyanion type compound is a series of tetrahedron or octahedra anion structure unit (XO of containing
m)
N-The general name of the compound of (X=P, Si, B, S, As, Mo, W etc.).Compare with lithium-compound transition metal oxide material, it is stable that polyanion type compound positive electrode generally has crystal structure, Heat stability is good, outstanding advantages such as security performance excellence.People have carried out comparatively deep research to series of phosphate material wherein, find LiFePO4 (LiFePO wherein
4) and phosphoric acid vanadium lithium (Li
3V
2(PO
4)
3) have a more excellent combination property.LiFePO particularly
4, accepted by a lot of battery enterprises, be widely used in power type and accumulation energy type lithium ion battery.
Recently, the silicate series material causes people's attention gradually.Because the abundance of silicon in the earth's crust much larger than phosphorus, therefore estimates that the cost of silicate material will be lower than phosphate.In addition, silicate is prevalent in the earth's crust, and structure is very stable, estimates that silicate material will have more excellent stability than phosphate material.People are to manganese silicate of lithium (Li
2MnSiO
4), ferric metasilicate lithium (Li
2FeSiO
4), cobaltous silicate lithium (Li
2CoSiO
4), silicic acid nickel lithium (Li
2NiSiO
4) carried out preliminary research.
V is the abundant transition metal of valence state, and chemical property is vivaciously various.Compare with other transition metal, the polyanion type compound battery material of vanadium has very big research space.The polyanion type compound battery material of the vanadium of bibliographical information mainly is a phosphate at present, as Li
3V
2(PO
4)
3, LiVPO
4F, VOPO
4, LiVOPO
4Deng, can be used as anode material for lithium-ion batteries.Up to now, the vanadium lithium silicate positive electrode is not seen bibliographical information as yet.
We are imagination SiO
4 4-Ion replaces Li
3V
2(PO
4)
3In PO
4 3-, and consider anionic variation of valence and charge balancing ion, designed Li
6V
2(SiO
4)
3New material.The molecular weight of this material and Li
3V
2(PO
4)
3About the same, but each molecule can be deviate from 6 lithiums in theory, therefore is expected to obtain to compare Li
3V
2(PO
4)
3Higher specific capacity.Studies show that the crystal structure of this new material and Li
3V
2(PO
4)
3Quite similar, shown in the X ray diffracting spectrum of accompanying drawing 1.
The present invention proposes to prepare new type lithium ion battery positive electrode material vanadium lithium silicate (Li
6V
2(SiO
4)
3) method.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of technology lithium ionic cell positive electrode material vanadium lithium silicate simple, with low cost, it is characterized in that, lithium source, vanadium source, silicon source and carbon source are made presoma by the class solgel reaction, dry back obtained vanadium lithium silicate in high-temperature heat treatment 8-48 hour through 600-900 ℃ under inertia and protection of reducing atmosphere; Gained vanadium lithium silicate powder is made up of nano-scale particle, good conductivity, specific capacity height.
Described vanadium source is one or more in vanadic oxide, the ammonium metavanadate, and the concentration that is mixed with vanadium is 0.2-3 mol solution or slurry.
Described lithium source is one or more of lithium carbonate or lithium hydroxide, and the concentration that is mixed with lithium is 0.2-3 mol solution or slurry.
Described silicon source is one or more in nano silicon or the tetraethoxysilane, and the concentration that is mixed with silicon is 0.2-3 mol solution or slurry.
The consumption in above-mentioned vanadium source, lithium source and silicon source is lithium in molar ratio: vanadium: silicon=6: 2: 3.
Described carbon source is selected from one or more in citric acid, ethylene glycol, sucrose, the glucose.
Described inertia and reducing atmosphere mist are the mist of 90% nitrogen+10% hydrogen.
The invention has the beneficial effects as follows that this preparation method prepares nano level vanadium lithium silicate positive electrode.During the 1C multiplying power, 3-4.8V discharges and recharges the interior reversible specific capacity of scope greater than 160mAh/g, and 1.5-4.8V discharges and recharges the interior reversible specific capacity of scope greater than 285mAh/g, and cycle performance is good, has application prospect.And the phosphoric acid vanadium lithium positive electrode that the same terms prepares down, during the 1C multiplying power, it is 147mAh/g that 3-4.8V discharges and recharges the interior reversible specific capacity of scope, it is 243mAh/g that 1.5-4.8V discharges and recharges the interior reversible specific capacity of scope.
Description of drawings
Fig. 1 is phosphoric acid vanadium lithium (Li
3V
2(PO
4)
3) and vanadium lithium silicate (Li
6V
2(SiO
4)
3) X-ray diffractogram.
Embodiment
The invention provides the preparation method of a kind of technology lithium ionic cell positive electrode material vanadium lithium silicate simple, with low cost.Its specific implementation method comprises following each step successively:
1. compound concentration is the lithium source solution or the slurry of 0.2-3 mol.
2. compound concentration is the vanadium source solution or the slurry of 0.2-3 mol.
3. compound concentration is the silicon source solution or the slurry of 0.2-3 mol.
4. press lithium: vanadium: silicon=6: 2: 3 (mol ratio) mixes above-mentioned three kinds of solution or slurry, stirring reaction, and control reaction temperature is 35-90 ℃, and solvent is evaporated gradually, generates gelatinous mixture.
With step (4) gained material in drier in 80-100 ℃ of dry 2-4 hour, the vanadium lithium silicate presoma.
6. step (5) products therefrom is placed stove, under inertia, reducing atmosphere or inertia and protection of reducing atmosphere, be warming up to 600-900 ℃, constant temperature 8-48 hour, natural cooling in stove obtained vanadium lithium silicate.
In above-mentioned preparation method, the described lithium of step (1) source is one or more of lithium carbonate or lithium hydroxide.
In above-mentioned preparation method, the described vanadium of step (2) source is one or more in vanadic oxide, the ammonium metavanadate.
In above-mentioned preparation method, the described silicon of step (3) source is one or more in nano silicon or the tetraethoxysilane.
In above-mentioned preparation method, during step (4) preparation vanadium lithium silicate presoma, the carbon source of mixing simultaneously is selected from one or more in citric acid, ethylene glycol, sucrose, the glucose, and its consumption is the 0.5-30wt% of vanadium lithium silicate.
In above-mentioned preparation method, described inertia of step (6) and reducing atmosphere source of the gas are the mist of nitrogen and hydrogen, preferably the mist of 90% nitrogen+10% hydrogen.
Introduce embodiments of the invention below:
Embodiment 1
The 2.5176g lithium hydroxide is dissolved in the 25ml deionized water, the 2.3396g ammonium metavanadate is dissolved in the 25ml deionized water, with 1.8g nano silicon 25ml ethanol decentralized system form slurry, aforementioned three is mixed, magnetic agitation adds 8.4056g citric acid and 9.9312g ethylene glycol after 1 hour, continuing to stir and control mixeding liquid temperature is 80 ℃, and solvent is evaporated gradually, becomes the gel of stable homogeneous until mixed liquor.With product in drying box in 100 ℃ dry 2 hours down, obtain vanadium lithium silicate material presoma.Dried presoma is put into alumina crucible, be warming up to 800 ℃ in the tube furnace, constant temperature 20 hours cools off with stove; In this process, continue to feed the mist of 90% nitrogen+10% hydrogen in the tube furnace, obtain vanadium lithium silicate (Li
6V
2(SiO
4)
3) product.With the lithium sheet is negative pole, tests under room temperature and 1C multiplying power, and this vanadium lithium silicate positive electrode reversible specific capacity in 3-4.8V discharges and recharges scope is 166mAh/g, and it is 291mAh/g that 1.5-4.8V discharges and recharges the interior reversible specific capacity of scope.
Embodiment 2
The 2.5176g lithium hydroxide is dissolved in the 25ml deionized water, with 3.6376g vanadic oxide 25ml deionized water decentralized system form slurry, the 6.24g tetraethoxysilane is dissolved in the 25ml deionized water, aforementioned three is mixed, magnetic agitation adds 8.4056g citric acid and 9.9312g ethylene glycol after 1 hour, continuing to stir and control mixeding liquid temperature is 60 ℃, and solvent is evaporated gradually, becomes the gel of stable homogeneous until mixed liquor.With product in drying box in 80 ℃ dry 3 hours down, obtain vanadium lithium silicate material presoma.Dried presoma is put into alumina crucible, be warming up to 700 ℃ in the tube furnace, constant temperature 36 hours cools off with stove; In this process, continue to feed the mist of 90% nitrogen+10% hydrogen in the tube furnace, obtain vanadium lithium silicate (Li
6V
2(SiO
4)
3) product.With the lithium sheet is negative pole, tests under room temperature and 1C multiplying power, and this vanadium lithium silicate positive electrode reversible specific capacity in 3-4.8V discharges and recharges scope is 161mAh/g, and it is 288mAh/g that 1.5-4.8V discharges and recharges the interior reversible specific capacity of scope.
Embodiment 3
With 5.76g lithium carbonate 25ml deionized water decentralized system form slurry, with 3.6376g vanadic oxide 25ml deionized water decentralized system form slurry, with 1.8g nano silicon 25ml ethanol decentralized system form slurry, aforementioned three is mixed, magnetic agitation adds 6.5g glucose after 1 hour, continuing to stir and control mixeding liquid temperature is 70 ℃, and solvent is evaporated gradually, becomes the gel of stable homogeneous until mixed liquor.With product in drying box in 80 ℃ dry 3 hours down, obtain vanadium lithium silicate material presoma.Dried presoma is put into alumina crucible, be warming up to 900 ℃ in the tube furnace, constant temperature 8 hours cools off with stove; In this process, continue to feed the mist of 90% nitrogen+10% hydrogen in the tube furnace, obtain vanadium lithium silicate (Li
6V
2(SiO
4)
3) product.With the lithium sheet is negative pole, tests under room temperature and 1C multiplying power, and this vanadium lithium silicate positive electrode reversible specific capacity in 3-4.8V discharges and recharges scope is 162mAh/g, and it is 289mAh/g that 1.5-4.8V discharges and recharges the interior reversible specific capacity of scope.
Embodiment 4
With 5.76g lithium carbonate 25ml deionized water decentralized system form slurry, with 3.6376g vanadic oxide 25ml deionized water decentralized system form slurry, the 6.24g tetraethoxysilane is dissolved in the 25ml deionized water, aforementioned three is mixed, magnetic agitation adds 10.5g sucrose after 1 hour, continuing to stir and control mixeding liquid temperature is 90 ℃, and solvent is evaporated gradually, becomes the gel of stable homogeneous until mixed liquor.With product in drying box in 80 ℃ dry 3 hours down, obtain vanadium lithium silicate material presoma.Dried presoma is put into alumina crucible, be warming up to 600 ℃ in the tube furnace, constant temperature 48 hours cools off with stove; In this process, continue to feed the mist of 90% nitrogen+10% hydrogen in the tube furnace, obtain vanadium lithium silicate (Li
6V
2(SiO
4)
3) product.With the lithium sheet is negative pole, tests under room temperature and 1C multiplying power, and this vanadium lithium silicate positive electrode reversible specific capacity in 3-4.8V discharges and recharges scope is 162mAh/g, and it is 289mAh/g that 1.5-4.8V discharges and recharges the interior reversible specific capacity of scope.
Comparing embodiment--preparation phosphoric acid vanadium lithium (Li
3V
2(PO
4)
3)
The 1.2588g lithium hydroxide is dissolved in the 25ml deionized water, the 2.3396g ammonium metavanadate is dissolved in the 25ml deionized water, the 3.45g ammonium dihydrogen phosphate is dissolved in the 25ml deionized water, aforementioned three is mixed, magnetic agitation adds 8.4056g citric acid and 9.9312g ethylene glycol after 1 hour, continuing to stir and control mixeding liquid temperature is 80 ℃, and solvent is evaporated gradually, becomes the gel of stable homogeneous until mixed liquor.With product in drying box in 100 ℃ dry 2 hours down, obtain phosphoric acid vanadium lithium material presoma.Dried presoma is put into alumina crucible, be warming up to 800 ℃ in the tube furnace, constant temperature 20 hours cools off with stove; In this process, continue to feed the mist of 90% nitrogen+10% hydrogen in the tube furnace, obtain phosphoric acid vanadium lithium (Li
3V
2(PO
4)
3) product.With the lithium sheet is negative pole, tests under room temperature and 1C multiplying power, and this phosphoric acid vanadium lithium positive electrode reversible specific capacity in 3-4.8V discharges and recharges scope is 147mAh/g, and it is 243mAh/g that 1.5-4.8V discharges and recharges the interior reversible specific capacity of scope.
Gained phosphoric acid vanadium lithium (Li
3V
2(PO
4)
3) and vanadium lithium silicate (Li
6V
2(SiO
4)
3) X-ray diffractogram as shown in Figure 1.
Claims (7)
1. the preparation method of a lithium ionic cell positive electrode material vanadium lithium silicate, it is characterized in that: lithium is pressed in lithium source, silicon source and vanadium source: vanadium: silicon=6: 2: 3 (mol ratio) mixes, and and carbon source mix, make presoma by solgel reaction, dry back obtained the vanadium lithium silicate powder in high-temperature heat treatment 8-48 hour through 600-900 ℃ under inertia and protection of reducing atmosphere; Gained vanadium lithium silicate powder is made up of nano-scale particle, good conductivity, specific capacity height.
2. according to the preparation method of the described lithium ionic cell positive electrode material vanadium lithium silicate of claim 1, it is characterized in that this method comprises following each step:
1) lithium source, silicon source and vanadium source are mixed with solution or the slurry that concentration is the 0.2-3 mol respectively;
2) in lithium: vanadium: silicon=6: 2: 3 (mol ratio) ratio, above-mentioned three kinds of solution or slurry are mixed, mix carbon source simultaneously, consumption is the 0.5-30wt% of vanadium lithium silicate.Continue stirring reaction, control reaction temperature is 35-90 ℃, and solvent is evaporated gradually, generates gelatinous mixture;
3) with step 2) the gained gelatinous mixture in drier in 80-100 ℃ of dry 2-4 hour, the vanadium lithium silicate presoma;
4) step 3) gained vanadium lithium silicate presoma is placed stove, under inertia, reducing atmosphere or inertia and protection of reducing atmosphere, be warming up to 600-900 ℃, constant temperature 8-48 hour, natural cooling in stove obtained the vanadium lithium silicate powder.
3. according to the preparation method of claim 1 or 2 described lithium ionic cell positive electrode material vanadium lithium silicates, it is characterized in that: described lithium source is one or more in lithium carbonate or the lithium hydroxide.
4. according to the preparation method of claim 1 or 2 described lithium ionic cell positive electrode material vanadium lithium silicates, it is characterized in that: described vanadium source is one or more in vanadic oxide, the ammonium metavanadate.
5. according to the preparation method of claim 1 or 2 described lithium ionic cell positive electrode material vanadium lithium silicates, it is characterized in that: described silicon source is one or more in silicon dioxide or the tetraethoxysilane.
6. according to the preparation method of claim 1 or 2 described lithium ionic cell positive electrode material vanadium lithium silicates, it is characterized in that: described carbon source is selected from one or more in citric acid, ethylene glycol, sucrose, the glucose.
7. according to the preparation method of claim 1 or 2 described lithium ionic cell positive electrode material vanadium lithium silicates, it is characterized in that: described inertia and reducing atmosphere are the mist of 90% nitrogen+10% hydrogen.
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| CN101540392B (en) * | 2009-04-09 | 2011-04-06 | 西安建筑科技大学 | Method for preparing lithium-manganese silicate of cathode material of lithium-ion battery |
| CN102290575A (en) * | 2011-07-21 | 2011-12-21 | 中国电子科技集团公司第十八研究所 | Lithium ion cell anode material and preparation method thereof |
| CN102903919A (en) * | 2012-10-23 | 2013-01-30 | 中国科学院过程工程研究所 | Anode material lithium vanadium silicate for lithium ion battery, preparation method and application of anode material |
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| US6085015A (en) * | 1997-03-25 | 2000-07-04 | Hydro-Quebec | Lithium insertion electrode materials based on orthosilicate derivatives |
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| US20030190527A1 (en) * | 2002-04-03 | 2003-10-09 | James Pugh | Batteries comprising alkali-transition metal phosphates and preferred electrolytes |
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