CN103490065B - A kind of card-like NH 4v 3o 8the preparation method of crystallite - Google Patents

A kind of card-like NH 4v 3o 8the preparation method of crystallite Download PDF

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CN103490065B
CN103490065B CN201310422044.9A CN201310422044A CN103490065B CN 103490065 B CN103490065 B CN 103490065B CN 201310422044 A CN201310422044 A CN 201310422044A CN 103490065 B CN103490065 B CN 103490065B
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solution
crystallite
card
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deionized water
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CN103490065A (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

A kind of card-like NH 4v 3o 8the preparation method of crystallite, dissolves ammonium metavanadate in deionized water, is mixed with NH 4 +concentration be the NH of 0.03 ~ 0.15mol/L 4vO 3solution, then adjust ph is 3.5 ~ 4.5, obtains B solution; Adopt microwave-ultraviolet synthesis model, microwave, uviol lamp are acted on B solution simultaneously, is warmed up to 50 ~ 90 DEG C, insulation, obtains suspension; Suspension centrifugation is obtained powder product, then dry.The NH that the inventive method is obtained 4v 3o 8crystallite chemical composition is homogeneous, and purity is higher, is card-like pattern, NH 4v 3o 8the thickness of microwafer is about 200-500nm, as having good chemical property during 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 the need to subsequent treatment, environmentally friendly, can be applicable to 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, are with a wide range of applications, become study hotspot in recent years.
Vanadium is the multivalent metal element in a kind of transition elements, and it both can form many oxide with oxygen, also can form composite oxides with other cations together with oxygen, and they generally all have embedding lithium ability, can as anode material for lithium-ion batteries, as V 2o 5, LiV 3o 8deng.NH 4v 3o 8at LiV 3o 8research foundation on the novel intercalation materials of li ions of one that finds, 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 gets up along c-axis compact siro spinning technology, NH 4 +then be in its interlayer, its structure can be stablized, and there is certain embedding lithium ability, can as a kind of anode material for lithium-ion batteries.In addition, NH 4v 3o 8also because of structure and the Electrical transport of its uniqueness, be expected to for sensor material [Gao Qian, Mai Liqiang, Xu Lin, etc. constructing and electronic transport performance [J] of barium oxide monodimension nanometer material. Chinese science and technology paper is online, 2010,5(4): 323-331].
Current preparation NH 4v 3o 8method mainly contain: the precipitation method and hydro thermal method.Heai-KuPark etc. adopt the precipitation method to prepare the NH of wide about 60nm 4v 3o 8nanometer rods, in the current density of 10mA/g and the voltage range of 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, employing hydro thermal method has obtained the sheet NH that thickness is about 150nm 4v 3o 80.2H 2o, in the current density of 15mA/g and the voltage range of 1.8-4.0V, its initial discharge capacity is 225.9mAh/g, after 30 circulations, capacity remains on 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 3be raw material with acetic acid, adopt hydro thermal method to prepare the NH of various pattern 4v 3o 8(as 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 precipitation method synthesis NH 4v 3o 8there is reaction and be not easy shortcomings such as controlling, have side reaction generation, product purity low, water heat transfer NH 4v 3o 8there is the shortcomings such as reaction temperature is relatively high, the reaction time is longer.So find a kind of low temperature, easily control, Fast back-projection algorithm 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, obtained NH 4v 3o 8the chemical composition of crystallite is homogeneous, and 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, be mixed with NH 4 +concentration be the NH of 0.03 ~ 0.15mol/L 4vO 3solution, is designated as solution A;
2) pH value regulating solution A is 3.5 ~ 4.5, obtains B solution;
3) adopt microwave-ultraviolet synthesis model, microwave, uviol lamp are acted on B solution simultaneously, make B solution with the heating rate of 8 DEG C/min by room temperature to 50 ~ 90 DEG C, insulation 30 ~ 120min, then cool to room temperature, obtain suspension;
4) suspension centrifugation is obtained powder product, then powder product is used respectively deionized water and soaked in absolute ethyl alcohol and 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 DEG C.
Described step 2) in pH value be employing 3 ~ 5molL -1hydrochloric acid solution carry out regulating.
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 DEG C in described step 3) adopt platinum resistance to measure.
10min is with the time of deionized water and soaked in absolute ethyl alcohol respectively in described step 4).
In described step 4), washing is specially and first spends deionized water, then uses absolute ethanol washing.
In described step 4), dry detailed process is for be placed in electric vacunm drying case by powder product, heats 6 ~ 10 hours at 50 ~ 60 DEG C.
Relative 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 is even and efficiency is higher, can promote that chemical reaction evenly, rapidly carries out.The NH that the inventive method is obtained 4v 3o 8crystallite chemical composition is homogeneous, and purity is higher, is card-like pattern, NH 4v 3o 8the thickness of microwafer is about 200-500nm, as having good chemical property during 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 the need to subsequent treatment, environmentally friendly, can be applicable to large-scale production.
Accompanying drawing explanation
Fig. 1 is anode material for lithium-ion batteries NH prepared by the embodiment of the present invention 1 4v 3o 8x-ray diffraction (XRD) collection of illustrative plates of crystallite.
Fig. 2 is anode material for lithium-ion batteries NH prepared by the embodiment of the present invention 1 4v 3o 8eSEM (SEM) photo of crystallite.
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 DEG C of deionized waters, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.05mol/L 4vO 3solution, is designated as solution A;
2) 3molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to 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 microwave ultraviolet excess sound wave Trinity synthesis extractive reaction instrument, 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, wherein the ultraviolet wavelength of uviol lamp is 365nm simultaneously, and the power of uviol lamp is 300W, and microwave power controls at 400W.Selective temperature-time service pattern, with the heating rate of 8 DEG C/min by room temperature to after 60 DEG C, insulation 60min, naturally cools to room temperature after reaction terminates, obtains suspension;
4) suspension centrifugation is obtained powder product, again powder product is respectively soaked 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to spend the operation 3 times that deionized water uses absolute ethanol washing again, then powder product to be placed in electric vacunm drying case at 50 DEG C dry 10 hours, fully grind after being cooled to room temperature, obtain the NH of card-like 4v 3o 8crystallite.
Fig. 1 is anode material for lithium-ion batteries NH prepared by the embodiment of the present invention 1 4v 3o 8x-ray diffraction (XRD) collection of illustrative plates of crystallite.As can be seen from Figure 1, prepared card-like NH 4v 3o 8microcrystallization is good, and purity is higher.
Fig. 2 is anode material for lithium-ion batteries NH prepared by the embodiment of the present invention 1 4v 3o 8eSEM (SEM) photo of crystallite.As shown in Figure 2, the NH for preparing of this method 4v 3o 8crystallite is grown better, and be special card-like pattern, the thickness of sheet is about 200-500nm.
Embodiment 2
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 60 DEG C of deionized waters, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.10mol/L 4vO 3solution, is designated as solution A;
2) 4molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to 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 microwave ultraviolet excess sound wave Trinity synthesis extractive reaction instrument, 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, wherein the ultraviolet of uviol lamp is 365nm simultaneously, and the power of uviol lamp is 300W, and microwave power controls at 300W.Selective temperature-time service pattern, with the heating rate of 8 DEG C/min by room temperature to 90 DEG C, insulation 30min, reaction terminate after naturally cool to room temperature, obtain suspension;
4) suspension centrifugation is obtained powder product, again powder product is respectively soaked 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to spend the operation 3 times that deionized water uses absolute ethanol washing again, then powder product to be placed in electric vacunm drying case at 60 DEG C 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 DEG C of deionized waters, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.15mol/L 4vO 3solution, is designated as solution A;
2) 5molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to 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 microwave ultraviolet excess sound wave Trinity synthesis extractive reaction instrument, 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, wherein the ultraviolet wavelength of uviol lamp is 365nm simultaneously, and the power of uviol lamp is 300W, and microwave power controls at 200W.Selective temperature-time service pattern, with the heating rate of 8 DEG C/min by room temperature to after 80 DEG C, insulation 90min, naturally cools to room temperature after reaction terminates, obtains suspension;
4) suspension centrifugation is obtained powder product, again powder product is respectively soaked 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to spend the operation 3 times that deionized water uses absolute ethanol washing again, then powder product to be placed in electric vacunm drying case at 60 DEG C 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 DEG C of deionized waters, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.12mol/L 4vO 3solution, is designated as solution A;
2) 3molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to 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 microwave ultraviolet excess sound wave Trinity synthesis extractive reaction instrument, 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, wherein the ultraviolet wavelength of uviol lamp is 365nm simultaneously, and the power of uviol lamp is 300W, and microwave power controls at 300W.Selective temperature-time service pattern, with the heating rate of 8 DEG C/min by room temperature to after 70 DEG C, insulation 60min, naturally cools to room temperature after reaction terminates, obtains suspension;
4) suspension centrifugation is obtained powder product, again powder product is respectively soaked 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to spend the operation 3 times that deionized water uses absolute ethanol washing again, then powder product to be placed in electric vacunm drying case at 60 DEG C 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 DEG C of deionized waters, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.03mol/L 4vO 3solution, is designated as solution A;
2) 4molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to 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 microwave ultraviolet excess sound wave Trinity synthesis extractive reaction instrument, 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, wherein the ultraviolet wavelength of uviol lamp is 365nm simultaneously, and the power of uviol lamp is 300W, and microwave power controls at 400W.Selective temperature-time service pattern, with the heating rate of 8 DEG C/min by room temperature to after 50 DEG C, insulation 120min, naturally cools to room temperature after reaction terminates, obtains suspension;
4) suspension centrifugation is obtained powder product, again powder product is respectively soaked 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to spend the operation 3 times that deionized water uses absolute ethanol washing again, then powder product to be placed in electric vacunm drying case at 50 DEG C 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 DEG C of deionized waters, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.07mol/L 4vO 3solution, is designated as solution A;
2) 3.5molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to 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 microwave ultraviolet excess sound wave Trinity synthesis extractive reaction instrument, 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, wherein the ultraviolet wavelength of uviol lamp is 365nm simultaneously, and the power of uviol lamp is 300W, and microwave power controls at 250W.Selective temperature-time service pattern, with the heating rate of 8 DEG C/min by room temperature to after 55 DEG C, insulation 105min, naturally cools to room temperature after reaction terminates, obtains suspension;
4) suspension centrifugation is obtained powder product, again powder product is respectively soaked 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to spend the operation 3 times that deionized water uses absolute ethanol washing again, then powder product to be placed in electric vacunm drying case at 53 DEG C 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 DEG C of deionized waters, magnetic agitation 0.5h makes ammonium metavanadate be uniformly dissolved, and is mixed with NH 4 +concentration be the NH of 0.03mol/L 4vO 3solution, is designated as solution A;
2) 4.5molL is adopted -1dilute hydrochloric acid solution regulate the pH value of solution A to 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 microwave ultraviolet excess sound wave Trinity synthesis extractive reaction instrument, 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, wherein the ultraviolet wavelength of uviol lamp is 365nm simultaneously, and the power of uviol lamp is 300W, and microwave power controls at 350W.Selective temperature-time service pattern, with the heating rate of 8 DEG C/min by room temperature to after 65 DEG C, insulation 45min, naturally cools to room temperature after reaction terminates, obtains suspension;
4) suspension centrifugation is obtained powder product, again powder product is respectively soaked 10min with deionized water and absolute ethyl alcohol respectively, then repeat first to spend the operation 3 times that deionized water uses absolute ethanol washing again, then powder product to be placed in electric vacunm drying case at 57 DEG C dry 7 hours, fully grind after being cooled to room temperature, obtain the NH of card-like 4v 3o 8crystallite.

Claims (7)

1. a card-like NH 4v 3o 8the preparation method of crystallite, is characterized in that, comprises the following steps:
1) ammonium metavanadate is dissolved in deionized water, be mixed with NH 4 +concentration be the NH of 0.03 ~ 0.15mol/L 4vO 3solution, is designated as solution A;
2) pH value regulating solution A is 3.5 ~ 4.5, obtains B solution;
3) adopt microwave-ultraviolet synthesis model, microwave, uviol lamp are acted on B solution simultaneously, make B solution with the heating rate of 8 DEG C/min by room temperature to 50 ~ 90 DEG C, insulation 30 ~ 120min, then cool to room temperature, obtain suspension;
4) suspension centrifugation is obtained powder product, then powder product is used respectively deionized water and soaked in absolute ethyl alcohol and cyclic washing, then dry, obtain the NH of card-like 4v 3o 8crystallite;
Described step 3) ultraviolet wavelength of medium ultraviolet lamp is 365nm, uviol lamp power is 300W, and microwave power is 200-400W.
2. a kind of card-like NH according to claim 1 4v 3o 8the preparation method of crystallite, is characterized in that, described step 1) in the temperature of deionized water be 50 ~ 60 DEG C.
3. a kind of card-like NH according to claim 1 4v 3o 8the preparation method of crystallite, is characterized in that, described step 2) in pH value be employing 3 ~ 5molL -1hydrochloric acid solution carry out regulating.
4. a kind of card-like NH according to claim 1 4v 3o 8the preparation method of crystallite, is characterized in that, described step 3) in 50 ~ 90 DEG C adopt platinum resistance measure.
5. a kind of card-like NH according to claim 1 4v 3o 8the preparation method of crystallite, is characterized in that, described step 4) in be 10min with the time of deionized water and soaked in absolute ethyl alcohol respectively.
6. a kind of card-like NH according to claim 1 4v 3o 8the preparation method of crystallite, is characterized in that, described step 4) in washing be specially and first spend deionized water, then use absolute ethanol washing.
7. a kind of card-like NH according to claim 1 4v 3o 8the preparation method of crystallite, is characterized in that, described step 4) in dry detailed process for powder product is placed in electric vacunm drying case, at 50 ~ 60 DEG C heat 6 ~ 10 hours.
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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
CN104485442B (en) * 2014-12-05 2017-01-11 陕西科技大学 Preparation method of self-assembled ball-flower type cathode material for lithium ion battery
CN104916833B (en) * 2015-05-18 2017-10-13 陕西科技大学 A kind of preparation method of self-assembled structures LiV3O8 anode material for lithium-ion batteries
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
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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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

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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

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