CN103490065A - Preparation method for card-shaped NH4V308 micro crystal - Google Patents

Preparation method for card-shaped NH4V308 micro crystal Download PDF

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CN103490065A
CN103490065A CN201310422044.9A CN201310422044A CN103490065A CN 103490065 A CN103490065 A CN 103490065A CN 201310422044 A CN201310422044 A CN 201310422044A CN 103490065 A CN103490065 A CN 103490065A
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solution
card
crystallite
deionized water
described step
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CN103490065B (en
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黄剑锋
曹杉杉
曹丽云
费杰
欧阳海波
李翠艳
吴建鹏
卢静
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Yancheng julonghu Business Cluster Development Co.,Ltd.
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G31/00—Compounds of vanadium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • 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

Disclosed is a preparation method for a card-shaped NH4V308 micro crystal. Ammonium metavanadate is dissolved in deionized water to prepare an NH4VO3 solution with the concentration of NH4+ being 0.03-0.15mol/L, and then the pH of the solution is regulated to be 3.5-4.5 to obtain a solution B; microwaves and an ultraviolet lamp simultaneously act on the solution B in a microwave and ultraviolet combined mode, the temperature rises to be at 50-90 DEG C and then is kept, and suspension liquid is obtained; centrifugal separation is carried out on the suspension liquid to obtain powdery products, and then the products are dried. The NH4V308 micro crystal prepared in the method is uniform in chemical composition, is high in purity and is shaped like a card, the thickness of the NH4V308 micro crystal is about 200-500nm, and the NH4V308 micro crystal has good electric chemical performance when serving as anode materials for a lithium ion battery. The preparation method for the card-shaped NH4V308 micro crystal is simple, low in reaction temperature, short in reaction period, without subsequent processing, friendly to the environment, and suitable for large-scale production.

Description

A kind of card-like NH 4v 3o 8the preparation method of crystallite
Technical field
The present invention relates to a kind of preparation method of lithium ion secondary battery anode material, particularly a kind of card-like NH 4v 3o 8the method of crystallite.
Background technology
The advantages such as lithium rechargeable battery has that voltage is high, specific energy is large, have extended cycle life, discharge performance is stable, fail safe is good, pollution-free and operating temperature range is wide, be with a wide range of applications, and becomes study hotspot in recent years.
Vanadium is the polyvalent metal element in a kind of transition elements, and it both can form many oxide with oxygen, also can form composite oxides together with oxygen with other cations, and they generally all have embedding lithium ability, can be used as anode material for lithium-ion batteries, as V 2o 5, LiV 3o 8deng.NH 4v 3o 8at LiV 3o 8research foundation on a kind of novel intercalation materials of li ions found, it and LiV 3o 8be all layer structure, belong to monoclinic P21/m space group.At NH 4v 3o 8in structure, V 3o 8 -layer closely couples together along c-axis, NH 4 +, in its interlayer, can stablize its structure, and there is certain embedding lithium ability, can be used as a kind of anode material for lithium-ion batteries.In addition, NH 4v 3o 8also because of its unique structure and electronic transport characteristic, be expected to for sensor material [Xu Lin, etc. constructing and electronic transport performance [J] of barium oxide monodimension nanometer material for Gao Qian, Mai Liqiang. the Chinese science and technology paper is online, 2010,5(4): 323-331].
Prepare at present NH 4v 3o 8method mainly contain: the precipitation method and hydro thermal method.The employing precipitation method such as Heai-KuPark have prepared the NH of wide about 60nm 4v 3o 8nanometer rods, in the voltage range of the current density of 10mA/g and 1.8-4.0V, its initial discharge capacity can reach 210mAh/g[Heai-KuPark, Guntae Kin.Ammonium hexavanadate nanorods prepared by homogeneous precipitation using urea as cathodes for lithium batteries[J] .Solid State Ionics, 2010,181:311-314.].Haiyan Wang etc. are with NH 4vO 3for raw material, using dodecyl sodium sulfate as surfactant, adopt hydro thermal method to make thickness be about the sheet NH of 150nm 4v 3o 80.2H 2o, in the voltage range of the current density of 15mA/g and 1.8-4.0V, its initial discharge capacity is 225.9mAh/g, after 30 circulations, Capacitance reserve is at 209.4mAh/g[Haiyan Wang, Kelong Huang, Suqin Liu, et al.Electrochemical property of NH 4v 3o 80.2H 2o flakes prepared by surfactant assisted hydrothermal method[J] .Journal of Power Source, 2011,196:788-792.].G.S.Zakharova etc. are with NH 4vO 3with acetic acid be raw material, adopt hydro thermal method to prepare the NH of various patterns 4v 3o 8(as the shuttle shape, flower-shaped and banded etc.) [G.S.Zakharova, Ch.Taschner, T.Kolb, et al.Morphology controlled NH 4v 3o 8microcrystals by hydrothermal synthesis[J] .Dalton Transactions, 2013,42:4897-4902.].
Due to the synthetic NH of the precipitation method 4v 3o 8exist reaction to be not easy to control, to have the shortcomings such as side reaction generation, product purity be low, hydro thermal method is synthesized NH 4v 3o 8there are the shortcomings such as reaction temperature is relatively high, the reaction time is long.So find a kind of low temperature, easily control, synthesize fast NH 4v 3o 8method, the research and development of high performance lithium ion battery anode material and sensor material is significant.
Summary of the invention
The object of the present invention is to provide a kind of card-like NH 4v 3o 8the preparation method of crystallite, it is simple to operate, preparation temperature is low, reaction time is short, makes NH 4v 3o 8the chemical composition homogeneous of crystallite, purity is high.
In order to achieve the above object, the technical solution used in the present invention is:
The present invention includes following steps:
1) ammonium metavanadate is dissolved in deionized water, is mixed with NH 4 +the concentration NH that is 0.03～0.15mol/L 4vO 3solution, be designated as A solution;
2) the pH value of adjusting A solution is 3.5～4.5, obtains B solution;
3) adopt microwave-ultraviolet synthesis model, microwave, uviol lamp are acted on to B solution simultaneously, make B solution be warmed up to 50～90 ℃ with the heating rate of 8 ℃/min by room temperature, be incubated 30～120min, then cool to room temperature, obtain suspension;
4) the suspension centrifugation is obtained to the powder product, then the powder product is used respectively to deionized water and soaked in absolute ethyl alcohol cyclic washing, then dry, obtain the NH of card-like 4v 3o 8crystallite.
In described step 1), the temperature of deionized water is 50～60 ℃.
Described step 2) in, the pH value is to adopt 3～5molL -1hydrochloric acid solution regulated.
The ultraviolet wavelength of described step 3) medium ultraviolet lamp is 365nm, and uviol lamp power is 300W, and microwave power is 200-400W.
50～90 ℃ in described step 3) adopt platinum resistance to be measured.
Be 10min with the time of deionized water and soaked in absolute ethyl alcohol respectively in described step 4).
In described step 4), washing is specially first and washs with deionized water, then uses absolute ethanol washing.
In described step 4), dry detailed process, for the powder product is placed in the electric vacunm drying case, heats 6～10 hours under 50～60 ℃.
With respect to prior art, the beneficial effect that the present invention has: the present invention adopts microwave-ultraviolet technique to prepare NH 4v 3o 8crystallite, microwave heating evenly and efficiency higher, can promote chemical reaction evenly, carry out rapidly.The NH that the inventive method makes 4v 3o 8crystallite chemical composition homogeneous, purity is higher, is card-like pattern, NH 4v 3o 8the thickness of microwafer is about 200-500nm, has good chemical property during as anode material for lithium-ion batteries; Preparation method of the present invention is simple, and reaction temperature is low, and reaction time is short, without subsequent treatment, environmentally friendly, can be applicable to large-scale production.
The accompanying drawing explanation
The anode material for lithium-ion batteries NH that Fig. 1 is the embodiment of the present invention 1 preparation 4v 3o 8the X-ray diffraction of crystallite (XRD) collection of illustrative plates.
The anode material for lithium-ion batteries NH that Fig. 2 is the embodiment of the present invention 1 preparation 4v 3o 8the ESEM of crystallite (SEM) photo.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Embodiment 1
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 50 ℃ of deionized waters, magnetic agitation 0.5h is uniformly dissolved ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.05mol/L 4vO 3solution, be designated as A solution;
2) adopt 3molL -1the dilute hydrochloric acid solution pH value of regulating A solution be 4.5, obtain B solution;
3) B solution is poured in four neck round-bottomed flasks, then four neck round bottom flask are entered in the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave Trinity, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring); Adopt microwave-ultraviolet synthesis model, make microwave and uviol lamp act on solution simultaneously, wherein the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and microwave power is controlled at 400W.Select temperature-time service pattern, after being warmed up to 60 ℃ with the heating rate of 8 ℃/min by room temperature, insulation 60min, reaction naturally cools to room temperature after finishing, and obtains suspension;
4) the suspension centrifugation is obtained to the powder product, again the powder product is respectively soaked to 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to use again with the deionized water washing operation 3 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 50 ℃ dry 10 hours, fully grind after being cooled to room temperature, obtain the NH of card-like 4v 3o 8crystallite.
The anode material for lithium-ion batteries NH that Fig. 1 is the embodiment of the present invention 1 preparation 4v 3o 8the X-ray diffraction of crystallite (XRD) collection of illustrative plates.As can be seen from Figure 1, prepared card-like NH 4v 3o 8microcrystallization is good, and purity is higher.
The anode material for lithium-ion batteries NH that Fig. 2 is the embodiment of the present invention 1 preparation 4v 3o 8the ESEM of crystallite (SEM) photo.As shown in Figure 2, the NH that prepared by this method 4v 3o 8crystallite is grown better, is special card-like pattern, and the thickness of sheet is about 200-500nm.
Embodiment 2
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 60 ℃ of deionized waters, magnetic agitation 0.5h is uniformly dissolved ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.10mol/L 4vO 3solution, be designated as A solution;
2) adopt 4molL -1the dilute hydrochloric acid solution pH value of regulating A solution be 4.0, obtain B solution;
3) B solution is poured in four neck round-bottomed flasks, then four neck round bottom flask are entered in the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave Trinity, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring); Adopt microwave-ultraviolet synthesis model, make microwave and uviol lamp act on solution simultaneously, wherein the ultraviolet ray of uviol lamp is 365nm, and the power of uviol lamp is 300W, and microwave power is controlled at 300W.Select temperature-time service pattern, with the heating rate of 8 ℃/min, by room temperature, be warmed up to 90 ℃, insulation 30min, reaction naturally cools to room temperature after finishing, and obtains suspension;
4) the suspension centrifugation is obtained to the powder product, again the powder product is respectively soaked to 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to use again with the deionized water washing operation 3 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 60 ℃ dry 8 hours, fully grind after being cooled to room temperature, obtain the NH of card-like 4v 3o 8crystallite.
Embodiment 3
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 55 ℃ of deionized waters, magnetic agitation 0.5h is uniformly dissolved ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.15mol/L 4vO 3solution, be designated as A solution;
2) adopt 5molL -1the dilute hydrochloric acid solution pH value of regulating A solution be 4.5, obtain B solution;
3) B solution is poured in four neck round-bottomed flasks, then four neck round bottom flask are entered in the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave Trinity, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring); Adopt microwave-ultraviolet synthesis model, make microwave and uviol lamp act on solution simultaneously, wherein the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and microwave power is controlled at 200W.Select temperature-time service pattern, after being warmed up to 80 ℃ with the heating rate of 8 ℃/min by room temperature, insulation 90min, reaction naturally cools to room temperature after finishing, and obtains suspension;
4) the suspension centrifugation is obtained to the powder product, again the powder product is respectively soaked to 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to use again with the deionized water washing operation 3 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 60 ℃ dry 6 hours, fully grind after being cooled to room temperature, obtain the NH of card-like 4v 3o 8crystallite.
Embodiment 4
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 58 ℃ of deionized waters, magnetic agitation 0.5h is uniformly dissolved ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.12mol/L 4vO 3solution, be designated as A solution;
2) adopt 3molL -1the dilute hydrochloric acid solution pH value of regulating A solution be 3.5, obtain B solution;
3) B solution is poured in four neck round-bottomed flasks, then four neck round bottom flask are entered in the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave Trinity, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring); Adopt microwave-ultraviolet synthesis model, make microwave and uviol lamp act on solution simultaneously, wherein the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and microwave power is controlled at 300W.Select temperature-time service pattern, after being warmed up to 70 ℃ with the heating rate of 8 ℃/min by room temperature, insulation 60min, reaction naturally cools to room temperature after finishing, and obtains suspension;
4) the suspension centrifugation is obtained to the powder product, again the powder product is respectively soaked to 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to use again with the deionized water washing operation 3 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 60 ℃ dry 8 hours, fully grind after being cooled to room temperature, obtain the NH of card-like 4v 3o 8crystallite.
Embodiment 5
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 52 ℃ of deionized waters, magnetic agitation 0.5h is uniformly dissolved ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.03mol/L 4vO 3solution, be designated as A solution;
2) adopt 4molL -1the dilute hydrochloric acid solution pH value of regulating A solution be 4.0, obtain B solution;
3) B solution is poured in four neck round-bottomed flasks, then four neck round bottom flask are entered in the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave Trinity, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring); Adopt microwave-ultraviolet synthesis model, make microwave and uviol lamp act on solution simultaneously, wherein the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and microwave power is controlled at 400W.Select temperature-time service pattern, after being warmed up to 50 ℃ with the heating rate of 8 ℃/min by room temperature, insulation 120min, reaction naturally cools to room temperature after finishing, and obtains suspension;
4) the suspension centrifugation is obtained to the powder product, again the powder product is respectively soaked to 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to use again with the deionized water washing operation 3 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 50 ℃ dry 10 hours, fully grind after being cooled to room temperature, obtain the NH of card-like 4v 3o 8crystallite.
Embodiment 6
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 50 ℃ of deionized waters, magnetic agitation 0.5h is uniformly dissolved ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.07mol/L 4vO 3solution, be designated as A solution;
2) adopt 3.5molL -1the dilute hydrochloric acid solution pH value of regulating A solution be 4.0, obtain B solution;
3) B solution is poured in four neck round-bottomed flasks, then four neck round bottom flask are entered in the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave Trinity, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring); Adopt microwave-ultraviolet synthesis model, make microwave and uviol lamp act on solution simultaneously, wherein the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and microwave power is controlled at 250W.Select temperature-time service pattern, after being warmed up to 55 ℃ with the heating rate of 8 ℃/min by room temperature, insulation 105min, reaction naturally cools to room temperature after finishing, and obtains suspension;
4) the suspension centrifugation is obtained to the powder product, again the powder product is respectively soaked to 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to use again with the deionized water washing operation 3 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 53 ℃ dry 9 hours, fully grind after being cooled to room temperature, obtain the NH of card-like 4v 3o 8crystallite.
Embodiment 7
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 60 ℃ of deionized waters, magnetic agitation 0.5h is uniformly dissolved ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.03mol/L 4vO 3solution, be designated as A solution;
2) adopt 4.5molL -1the dilute hydrochloric acid solution pH value of regulating A solution be 4.5, obtain B solution;
3) B solution is poured in four neck round-bottomed flasks, then four neck round bottom flask are entered in the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave Trinity, and fix, adopt direct temperature measurement mode thermometric (platinum resistor temperature measuring); Adopt microwave-ultraviolet synthesis model, make microwave and uviol lamp act on solution simultaneously, wherein the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and microwave power is controlled at 350W.Select temperature-time service pattern, after being warmed up to 65 ℃ with the heating rate of 8 ℃/min by room temperature, insulation 45min, reaction naturally cools to room temperature after finishing, and obtains suspension;
4) the suspension centrifugation is obtained to the powder product, again the powder product is respectively soaked to 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to use again with the deionized water washing operation 3 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 57 ℃ dry 7 hours, fully grind after being cooled to room temperature, obtain the NH of card-like 4v 3o 8crystallite.

Claims (8)

1. a card-like NH 4v 3o 8the method of crystallite, is characterized in that, comprises the following steps:
1) ammonium metavanadate is dissolved in deionized water, is mixed with NH 4 +the concentration NH that is 0.03～0.15mol/L 4vO 3solution, be designated as A solution;
2) the pH value of adjusting A solution is 3.5～4.5, obtains B solution;
3) adopt microwave-ultraviolet synthesis model, microwave, uviol lamp are acted on to B solution simultaneously, make B solution be warmed up to 50～90 ℃ with the heating rate of 8 ℃/min by room temperature, be incubated 30～120min, then cool to room temperature, obtain suspension;
4) the suspension centrifugation is obtained to the powder product, then the powder product is used respectively to deionized water and soaked in absolute ethyl alcohol cyclic washing, then dry, obtain the NH of card-like 4v 3o 8crystallite.
2. a kind of card-like NH according to claim 1 4v 3o 8the method of crystallite, is characterized in that, in described step 1), the temperature of deionized water is 50～60 ℃.
3. a kind of card-like NH according to claim 1 4v 3o 8the method of crystallite, is characterized in that, described step 2) in pH value be the employing 3～5molL -1hydrochloric acid solution regulated.
4. a kind of card-like NH according to claim 1 4v 3o 8the method of crystallite, is characterized in that, the ultraviolet wavelength of described step 3) medium ultraviolet lamp is 365nm, and uviol lamp power is 300W, and microwave power is 200-400W.
5. a kind of card-like NH according to claim 1 4v 3o 8the method of crystallite, is characterized in that, 50～90 ℃ in described step 3) adopt platinum resistance to be measured.
6. a kind of card-like NH according to claim 1 4v 3o 8the method of crystallite, is characterized in that, in described step 4), is 10min with the time of deionized water and soaked in absolute ethyl alcohol respectively.
7. a kind of card-like NH according to claim 1 4v 3o 8the method of crystallite, is characterized in that, in described step 4), washing is specially first and washs with deionized water, then uses absolute ethanol washing.
8. a kind of card-like NH according to claim 1 4v 3o 8the method of crystallite, is characterized in that, in described step 4), dry detailed process, for the powder product is placed in the electric vacunm drying case, heats 6～10 hours under 50～60 ℃.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103922402A (en) * 2014-03-24 2014-07-16 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing NH4V3O8 nanoribbon
CN104485442A (en) * 2014-12-05 2015-04-01 陕西科技大学 Preparation method of self-assembled ball-flower type cathode material for lithium ion battery
CN104916833A (en) * 2015-05-18 2015-09-16 陕西科技大学 Preparation method of LiV3O8 lithium ion battery cathode material in self-assembly structure
CN106129349A (en) * 2016-06-27 2016-11-16 陕西科技大学 A kind of anode material for lithium-ion batteries ammonium vanadate/Graphene and preparation method thereof
CN115594221A (en) * 2022-11-15 2023-01-13 攀钢集团攀枝花钢铁研究院有限公司（Cn） Method for preparing flaky high-density ammonium polyvanadate from vanadium liquid with low ammonium content

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CN102942223A (en) * 2012-11-14 2013-02-27 陕西科技大学 Preparation method of hexagonal flaky NH4V3O8 microcrystals
CN102951681A (en) * 2012-11-14 2013-03-06 陕西科技大学 Method for synthesizing flower-like bismuth vanadate microcrystals

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102942223A (en) * 2012-11-14 2013-02-27 陕西科技大学 Preparation method of hexagonal flaky NH4V3O8 microcrystals
CN102951681A (en) * 2012-11-14 2013-03-06 陕西科技大学 Method for synthesizing flower-like bismuth vanadate microcrystals

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103922402A (en) * 2014-03-24 2014-07-16 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing NH4V3O8 nanoribbon
CN103922402B (en) * 2014-03-24 2015-04-29 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing NH4V3O8 nanoribbon
CN104485442A (en) * 2014-12-05 2015-04-01 陕西科技大学 Preparation method of self-assembled ball-flower type cathode material for lithium ion battery
CN104916833A (en) * 2015-05-18 2015-09-16 陕西科技大学 Preparation method of LiV3O8 lithium ion battery cathode material in self-assembly structure
CN106129349A (en) * 2016-06-27 2016-11-16 陕西科技大学 A kind of anode material for lithium-ion batteries ammonium vanadate/Graphene and preparation method thereof
CN115594221A (en) * 2022-11-15 2023-01-13 攀钢集团攀枝花钢铁研究院有限公司（Cn） Method for preparing flaky high-density ammonium polyvanadate from vanadium liquid with low ammonium content
CN115594221B (en) * 2022-11-15 2024-03-19 攀钢集团攀枝花钢铁研究院有限公司 Method for preparing flaky high-density ammonium polyvanadate from low ammonium content in vanadium liquid

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