CN102354746A - Preparation method for silver vanadate cathode material - Google Patents
Preparation method for silver vanadate cathode material Download PDFInfo
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- CN102354746A CN102354746A CN2011103555357A CN201110355535A CN102354746A CN 102354746 A CN102354746 A CN 102354746A CN 2011103555357 A CN2011103555357 A CN 2011103555357A CN 201110355535 A CN201110355535 A CN 201110355535A CN 102354746 A CN102354746 A CN 102354746A
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- preparation
- compound
- vanadium source
- vanadic acid
- acid silver
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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 relates to a preparation method for a silver vanadate cathode material. The method comprises the following steps: stirring vanadium source and oxalic acid at certain stoichiometric ratio in solution until the solution becomes blue; then, adding Ag-contained compound; fully stirring; and after drying, heating in the air at the temperature of 300-550DEG C to obtain silver vanadate compound. The preparation technology is simple and is suitable for large-scale production, and a product serves as lithium battery cathode material and has better electrochemistry performance.
Description
Technical field
The present invention relates to a kind of anode material of lithium battery, vanadic acid silver positive electrode preparation methods.
Background technology
Implantable cardiac changes multiple defibrillator, and (Impantable Cardiac Defibrillator is to use electric shock to rescue the patient with medical arrhythmia cordis ICD), and is very effective for the prevention cardiac sudden death.Defibrillator needs battery-operated, because implant, battery performance is required relatively strictness, for example non-stop run, and stable, nothing is leaked, energy is high, the life-span is long, nontoxic etc.
Vanadic acid silver/lithium primary battery is the main battery that present heart changes multiple defibrillator, and its energy density is high, and self discharge is little, and is safe and reliable, long service life.Because vanadic acid silver/lithium battery is a primary cell, during depleted of energy, need to change, this causes economical and spiritual loss to patient.Therefore improve the energy density of battery, reduce cost, increasing the service life has great importance.
AgVO
3, Ag
2V
4O
11Be many vanadic acid silver positive electrode materials of two kinds of researchs.At present, the main synthesis method of vanadic acid silver electrode material is a high temperature solid-state method, sol-gel process etc., and the reaction time is longer, and chemical property is restricted.Therefore seek a kind of method of easy synthetic vanadic acid silver positive electrode material, and have better electrochemical performance and have important and practical meanings.
Summary of the invention
The present invention relates to a kind of preparation method of vanadic acid silver electrode material.This method technology is simple, and cost is low, and the vanadic acid silver anode material of lithium battery that obtains has better electrochemical performance.
The objective of the invention is to realize in the following manner:
A kind of vanadic acid silver positive electrode preparation methods comprises the steps:
Vanadium source and oxalic acid mix stirring (mol ratio of oxalic acid and v element >=3: 2) in solution, become blueness up to solution; Afterwards, add again and contain the Ag compound, fully stir, after dry (50-200 ℃ of baking temperature scope), in oxidizing atmosphere,, obtain vanadic acid silver compound in 300～550 ℃ of heating 1-8 hour.
Described vanadium source comprises V
2O
5, NH
4VO
3And HVO
3In one or more mixing.
The described Ag of containing compound is AgNO
3, the mixing of one or more in AgO, the silver acetate.
Described vanadic acid silver compound is AgVO
3Or Ag
2V
4O
11, for AgVO
3, the vanadium source of adding with contain the Ag compound according to mol ratio V: Ag=1: 1 ratio adds; For Ag
2V
4O
11, the vanadium source of adding with contain the Ag compound according to mol ratio V: Ag=2: 1 ratio adds.
Described oxidizing atmosphere is air or oxygen.
The present invention is to V
2O
5, NH
4VO
3Reduce processing in vanadium source etc., oxalic acid is reducing agent, obtains VOC
2O
4Blue precursor solution, after this precursor solution and the Ag compound, the vanadic acid silver particle size that after lower temperature roasting, prepares is little, is evenly distributed, and the tool chemical property is better.
Description of drawings
Fig. 1 is the XRD figure spectrum of the vanadic acid silver of preparation among the embodiment 1;
Fig. 2 is 400 ℃ of synthetic AgVO among the embodiment 1
325,50 with 100mA g
-1Current density under discharge curve;
Fig. 3 is 500 ℃ of synthetic AgVO among the embodiment 1
325,50 with 100mA g
-1Current density under discharge curve;
The Ag of Fig. 4 for preparing among the embodiment 3
2V
4O
11XRD figure spectrum.
Embodiment
Be intended to further specify the present invention below in conjunction with embodiment, and unrestricted the present invention.
V
2O
5Powder and oxalic acid join in the aqueous solution and fully stir, up to the solution becomes au bleu according to 1: 3 mol ratio.Afterwards according to V: Ag=1; 1 element mol ratio adds AgNO
3, stirring after 1 hour, 80 ℃ of heating, evaporates to dryness obtain solid mixture.This solid mixture heated 4 hours in air at 400 ℃ and 500 ℃ respectively, obtained AgVO
3Anode material of lithium battery.Fig. 1 is 400 ℃ and 500 ℃ of synthetic AgVO among the embodiment 1
3The XRD figure spectrum of electrode material.The result shows that this method can successfully make AgVO
3, and purity is high.Fig. 2 and Fig. 3 be respectively 400 ℃ with 500 ℃ of synthetic vanadic acid silver discharge curves under different current densities.As shown in Figure 2,400 ℃ of synthetic AgVO
3At 25mA g
-1Current density under, can discharge 255mAh g
-1The ratio discharge capacity.500 ℃ of synthetic AgVO that Fig. 3 shows
3Electrode is at 25mA g
-1Current density under can discharge 220mAh g
-1The ratio discharge capacity.
Embodiment 2
V among the embodiment 1
2O
5Can use NH
4VO
3The mol ratio of replacement and oxalic acid is 1: 6.Join in the aqueous solution and stir, redox reaction takes place, solution becomes blueness.Afterwards according to V: Ag=1; 1 element mol ratio adds AgNO
3, stirring after 1 hour, 80 ℃ of heating, evaporates to dryness obtain solid mixture.This solid mixture heated 4 hours in air at 400 ℃ and 500 ℃ respectively, obtained AgVO
3Anode material of lithium battery.
Embodiment 3
Ag among the adjustment embodiment 1 and the mol ratio of V are 1: 2, can prepare Ag
2V
4O
11Concrete steps are following: V
2O
5Powder and oxalic acid join in the aqueous solution and fully stir, up to the solution becomes au bleu according to 1: 3 mol ratio.Afterwards according to V: Ag=2: 1 element mol ratio adds AgNO
3, stirring after 1 hour, 80 ℃ of heating, evaporates to dryness obtain solid mixture.This solid mixture heated 4 hours in air at 400 ℃ and 500 ℃ respectively, obtained Ag
2V
4O
11Anode material of lithium battery.Fig. 4 shows Ag synthetic among the embodiment 3
2V
4O
11XRD figure spectrum.This XRD figure spectrum and Ag
2V
4O
11Corresponding relatively good of XRD figure spectrum, illustrate that this method can successfully make Ag
2V
4O
11Cell positive material.
Claims (5)
1. a vanadic acid silver positive electrode preparation methods is characterized in that, comprises the steps: that vanadium source and oxalic acid mix stirring in solution, become blueness up to solution; Afterwards, add again and contain the Ag compound, fully stir, after the drying, in oxidizing atmosphere,, obtain vanadic acid silver compound in 300～550 ℃ of heating 1-8 hour.
2. preparation method according to claim 1 is characterized in that, described vanadium source comprises V
2O
5, NH
4VO
3And HVO
3In one or more mixing.
3. preparation method according to claim 1 is characterized in that, the described Ag of containing compound is AgNO
3, the mixing of one or more in AgO, the silver acetate.
4. preparation method according to claim 1 is characterized in that, described vanadic acid silver compound is AgVO
3Or Ag
2V
4O
11, for AgVO
3, the vanadium source of adding with contain the Ag compound according to mol ratio V: Ag=1: 1 ratio adds; For Ag
2V
4O
11, the vanadium source of adding with contain the Ag compound according to mol ratio V: Ag=2: 1 ratio adds.
5. preparation method according to claim 1 is characterized in that, described oxidizing atmosphere is air or oxygen.
Priority Applications (1)
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|---|---|---|---|
| CN2011103555357A CN102354746A (en) | 2011-11-11 | 2011-11-11 | Preparation method for silver vanadate cathode material |
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|---|---|---|---|
| CN2011103555357A CN102354746A (en) | 2011-11-11 | 2011-11-11 | Preparation method for silver vanadate cathode material |
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| CN102354746A true CN102354746A (en) | 2012-02-15 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102765756A (en) * | 2012-07-24 | 2012-11-07 | 武汉理工大学 | Radial beta-AgVO3 nanowire cluster and preparation method of radial beta-AgVO3 nanowire cluster |
| CN104577124A (en) * | 2013-10-14 | 2015-04-29 | 中国电子科技集团公司第十八研究所 | Preparation method of mixed anode material for lithium battery |
| CN106219606A (en) * | 2016-07-12 | 2016-12-14 | 陕西科技大学 | A kind of spherical Ag of nano flower3vO4preparation method |
| CN107293735A (en) * | 2017-06-02 | 2017-10-24 | 河南工业大学 | Fluorin doped vanadic acid silver electrode material and preparation method and application |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5695892A (en) * | 1996-08-20 | 1997-12-09 | Wilson Greatbatch Ltd. | Preparation of silver vanadium oxide using nitric acid with oxide starting materials |
| CN1397497A (en) * | 2002-08-15 | 2003-02-19 | 武汉大学 | Process for synthesizing silver vanadium oxide |
-
2011
- 2011-11-11 CN CN2011103555357A patent/CN102354746A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5695892A (en) * | 1996-08-20 | 1997-12-09 | Wilson Greatbatch Ltd. | Preparation of silver vanadium oxide using nitric acid with oxide starting materials |
| CN1397497A (en) * | 2002-08-15 | 2003-02-19 | 武汉大学 | Process for synthesizing silver vanadium oxide |
Non-Patent Citations (1)
| Title |
|---|
| ANQIANG PAN等: "Template free synthesis of LiV3O8 nanorods as a cathode material for high-rate secondary lithium batteries", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102765756A (en) * | 2012-07-24 | 2012-11-07 | 武汉理工大学 | Radial beta-AgVO3 nanowire cluster and preparation method of radial beta-AgVO3 nanowire cluster |
| CN104577124A (en) * | 2013-10-14 | 2015-04-29 | 中国电子科技集团公司第十八研究所 | Preparation method of mixed anode material for lithium battery |
| CN106219606A (en) * | 2016-07-12 | 2016-12-14 | 陕西科技大学 | A kind of spherical Ag of nano flower3vO4preparation method |
| CN106219606B (en) * | 2016-07-12 | 2018-07-10 | 陕西科技大学 | A kind of nanometer of flower ball-shaped Ag3VO4Preparation method |
| CN107293735A (en) * | 2017-06-02 | 2017-10-24 | 河南工业大学 | Fluorin doped vanadic acid silver electrode material and preparation method and application |
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Application publication date: 20120215 |