CN103490066A - Preparation method for prismatic NH4V3O8 nanometer crystal - Google Patents

Preparation method for prismatic NH4V3O8 nanometer crystal Download PDF

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CN103490066A
CN103490066A CN201310422104.7A CN201310422104A CN103490066A CN 103490066 A CN103490066 A CN 103490066A CN 201310422104 A CN201310422104 A CN 201310422104A CN 103490066 A CN103490066 A CN 103490066A
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CN103490066B (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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Abstract

Disclosed is a preparation method for a prismatic NH4V3O8 nanometer crystal. Ammonium metavanadate is dissolved in deionized water to obtain an NH4VO3 solution; after the pH value is regulated, the solution is poured into a vessel, the vessel is placed into a microwave-ultraviolet-ultrasonic combined extraction reaction instrument, the temperature rises to be 40-80 DEG C in a microwave-ultraviolet-ultrasonic combined mode and then kept, and suspension liquid is obtained; centrifugal separation is carried out on the suspension liquid to obtain the NH4V3O8 nanometer crystal. According to the preparation method for the prismatic NH4V3O8 nanometer crystal, microwave, ultraviolet and ultrasonic can all provide energy for chemical reaction and promote uniform, rapid and complete conduction of the chemical reaction. The NH4V3O8 nanometer crystal prepared through the method is uniform in shape and granule diameter, and prismatic, the granule diameter is 100-150nm, and the NH4V3O8 nanometer crystal can be used as cathode materials for a lithium ion secondary battery. The preparation method is simple, low in reaction temperature, short in reaction period, simple in process equipment, free of subsequent processing, friendly to the environment and suitable for large-scale production.

Description

A kind of prism-shaped NH 4v 3o 8nanocrystalline preparation method
Technical field
The present invention relates to a kind of preparation method of lithium ion secondary battery anode material, particularly a kind of prism-shaped NH 4v 3o 8nanocrystalline preparation method.
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 invention is to provide a kind of prism-shaped NH 4v 3o 8nanocrystalline preparation method, its preparation temperature is low, and reaction time is short, the NH that the present invention makes 4v 3o 8nanocrystalline chemistry forms homogeneous, and purity is high, and pattern homogeneous and particle diameter are even.
In order to achieve the above object, the present invention adopts following technical scheme:
1) ammonium metavanadate is dissolved in deionized water, is mixed with NH 4 +the concentration NH that is 0.10～0.25mol/L 4vO 3solution, be designated as A solution;
2) the pH value of adjusting A solution is 3.0～5.0, obtains B solution;
3) B solution is poured in container, again container is put into to the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave Trinity, adopt microwave-ultraviolet-ultrasonic synthesis model, microwave, uviol lamp and ultrasonic wave are acted on to B solution simultaneously, make B solution be warmed up to 40～80 ℃ with the heating rate of 10 ℃/min by room temperature, insulation 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, and cyclic washing, then dry, obtain NH 4v 3o 8nanocrystalline.
In described step 1), the temperature of deionized water is 60～70 ℃.
Described step 2) in, the pH value is to adopt 2～5molL -1hydrochloric acid solution regulated.
The ultraviolet wavelength of described step 3) medium ultraviolet lamp is 365nm, and the power of uviol lamp is 300W, and hyperacoustic power output is 400-800W, and microwave power is 200-400W.
In described step 3), 40～80 ℃ 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 ℃.
The present invention adopts microwave-ultraviolet-ultrasonic technique to prepare NH 4v 3o 8nanocrystalline, microwave, ultraviolet, ultrasonic all can be for chemical reaction provides energy, promote chemical reaction evenly, fast, carry out fully.The NH that the present invention makes 4v 3o 8nanocrystalline chemistry forms homogeneous, and purity is higher, and pattern homogeneous and particle diameter are even, are prism-shaped; The NH that the present invention makes 4v 3o 8nanocrystallinely can be used as lithium ion secondary battery anode material, NH 4v 3o 8nanocrystalline particle diameter is 100-150nm, due to its specific area with less particle diameter and Geng Gao, can improve the chemical property of material.Preparation method of the present invention is simple, and reaction temperature is low, and reaction time is short, and process equipment is simple, without subsequent treatment, environmentally friendly, is 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 8nanocrystalline X-ray diffraction (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 8nanocrystalline ESEM (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 60 ℃ of deionized waters, magnetic agitation 0.5h dissolves ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.10mol/L 4vO 3solution, be designated as A solution;
2) adopt 5molL -1hydrochloric acid solution regulate A solution pthe H value is 3.0, obtains 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-ultrasonic synthesis model, solution is imposed to microwave, uviol lamp and ultrasonic wave simultaneously, the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and hyperacoustic output power is at 600W, and microwave power is controlled at 300W.Select temperature-time service pattern, open microwave, uviol lamp and ultrasonic wave simultaneously, after being warmed up to 60 ℃ with the heating rate of 10 ℃/min by room temperature, insulation 60min, then naturally cool to room temperature, 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, and repeat first to use again with the deionized water washing operation 5 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 50 ℃ dry 10 hours, obtains NH 4v 3o 8nanocrystalline.
The anode material for lithium-ion batteries NH that Fig. 1 is the embodiment of the present invention 1 preparation 4v 3o 8nanocrystalline X-ray diffraction (XRD) collection of illustrative plates.As can be seen from Figure 1, prepared NH 4v 3o 8nanocrystalline good crystallinity, 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 8nanocrystalline ESEM (SEM) photo.As shown in Figure 2, the NH that prepared by this method 4v 3o 8nanocrystalline growth is better, and the pattern homogeneous, be prism-shaped, and particle diameter is less and be evenly distributed, and is 100-150nm.
Embodiment 2
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 63 ℃ of deionized waters, magnetic agitation 0.5h dissolves ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.20mol/L 4vO 3solution, be designated as A solution;
2) adopt 4molL -1the 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-ultrasonic synthesis model, B solution is imposed to microwave, uviol lamp and ultrasonic wave simultaneously, the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and hyperacoustic output power is at 400W, and microwave power is controlled at 300W.Select temperature-time service pattern, open microwave, uviol lamp and ultrasonic wave simultaneously, after being warmed up to 80 ℃ with the heating rate of 10 ℃/min by room temperature, insulation 30min, then naturally cool to room temperature, 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, and repeat first with deionized water, to wash, use again the operation 5 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 60 ℃ dry 8 hours, obtains NH 4v 3o 8nanocrystalline.
Embodiment 3
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 66 ℃ of deionized waters, magnetic agitation 0.5h dissolves ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.25mol/L 4vO 3solution, be designated as A solution;
2) adopt 4molL -1the 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-ultrasonic synthesis model, B solution is imposed to microwave, uviol lamp and ultrasonic wave simultaneously, the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and hyperacoustic output power is at 500W, and microwave power is controlled at 300W.Select temperature-time service pattern, open microwave, uviol lamp and ultrasonic wave simultaneously, after being warmed up to 70 ℃ with the heating rate of 10 ℃/min by room temperature, insulation 60min, then naturally cool to room temperature, 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, and repeat first with deionized water, to wash, use again the operation 5 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 60 ℃ dry 6 hours, obtains NH 4v 3o 8nanocrystalline.
Embodiment 4
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 70 ℃ of deionized waters, magnetic agitation 0.5h dissolves ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.15mol/L 4vO 3solution, be designated as A solution;
2) adopt 3molL -1the hydrochloric acid solution pH value of regulating A solution be 5.0, 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-ultrasonic synthesis model, B solution is imposed to microwave, uviol lamp and ultrasonic wave simultaneously, the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and hyperacoustic output power is at 800W, and microwave power is controlled at 200W.Select temperature-time service pattern, open microwave, uviol lamp and ultrasonic wave simultaneously, after being warmed up to 50 ℃ with the heating rate of 10 ℃/min by room temperature, insulation 90min, then naturally cool to room temperature, 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, and repeat first with deionized water, to wash, use again the operation 5 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 60 ℃ dry 8 hours, obtains NH 4v 3o 8nanocrystalline.
Embodiment 5
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 60 ℃ of deionized waters, magnetic agitation 0.5h dissolves 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 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-ultrasonic synthesis model, B solution is imposed to microwave, uviol lamp and ultrasonic wave simultaneously, the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and hyperacoustic output power is at 700W, and microwave power is controlled at 400W.Select temperature-time service pattern, open microwave, uviol lamp and ultrasonic wave simultaneously, after being warmed up to 40 ℃ with the heating rate of 10 ℃/min by room temperature, insulation 120min, then naturally cool to room temperature, 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, and repeat first with deionized water, to wash, use again the operation 5 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 50 ℃ dry 10 hours, obtains NH 4v 3o 8nanocrystalline.
Embodiment 6
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 70 ℃ of deionized waters, magnetic agitation 0.5h dissolves ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.1mol/L 4vO 3solution, be designated as A solution;
2) adopt 3.5molL -1the hydrochloric acid solution pH value of regulating A solution be 3, 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-ultrasonic synthesis model, B solution is imposed to microwave, uviol lamp and ultrasonic wave simultaneously, the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and hyperacoustic output power is at 550W, and microwave power is controlled at 250W.Select temperature-time service pattern, open microwave, uviol lamp and ultrasonic wave simultaneously, after being warmed up to 45 ℃ with the heating rate of 10 ℃/min by room temperature, insulation 100min, then naturally cool to room temperature, 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, and repeat first with deionized water, to wash, use again the operation 5 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 55 ℃ dry 9 hours, obtains NH 4v 3o 8nanocrystalline.
Embodiment 7
1) by analytically pure ammonium metavanadate (NH 4vO 3) be dissolved in 65 ℃ of deionized waters, magnetic agitation 0.5h dissolves ammonium metavanadate, is mixed with NH 4 +the concentration NH that is 0.2mol/L 4vO 3solution, be designated as A solution;
2) adopt 4.5molL -1the hydrochloric acid solution pH value of regulating A solution be 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-ultrasonic synthesis model, B solution is imposed to microwave, uviol lamp and ultrasonic wave simultaneously, the ultraviolet wavelength of uviol lamp is 365nm, and the power of uviol lamp is 300W, and hyperacoustic output power is at 650W, and microwave power is controlled at 350W.Select temperature-time service pattern, open microwave, uviol lamp and ultrasonic wave simultaneously, after being warmed up to 65 ℃ with the heating rate of 10 ℃/min by room temperature, insulation 75min, then naturally cool to room temperature, 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, and repeat first to use again with the deionized water washing operation 5 times of absolute ethanol washing, then the powder product is placed in the electric vacunm drying case under 60 ℃ dry 7 hours, obtains NH 4v 3o 8nanocrystalline.

Claims (8)

1. a prism-shaped NH 4v 3o 8nanocrystalline preparation method, 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 0.10～0.25mol/L 4vO 3solution, be designated as A solution;
2) the pH value of adjusting A solution is 3.0～5.0, obtains B solution;
3) B solution is poured in container, again container is put into to the synthetic extractive reaction instrument of the microwave ultraviolet excess sound wave Trinity, adopt microwave-ultraviolet-ultrasonic synthesis model, microwave, uviol lamp and ultrasonic wave are acted on to B solution simultaneously, make B solution be warmed up to 40～80 ℃ with the heating rate of 10 ℃/min by room temperature, insulation 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 prism-shaped NH 4v 3o 8nanocrystalline.
2. a kind of prism-shaped NH according to claim 1 4v 3o 8nanocrystalline preparation method, is characterized in that, in described step 1), the temperature of deionized water is 60～70 ℃.
3. a kind of prism-shaped NH according to claim 1 4v 3o 8nanocrystalline preparation method, is characterized in that, described step 2) in pH value be the employing 2～5molL -1hydrochloric acid solution regulated.
4. a kind of prism-shaped NH according to claim 1 4v 3o 8nanocrystalline preparation method, is characterized in that, the ultraviolet wavelength of described step 3) medium ultraviolet lamp is 365nm, and the power of uviol lamp is 300W, and hyperacoustic power output is 400-800W, and microwave power is 200-400W.
5. a kind of prism-shaped NH according to claim 1 4v 3o 8nanocrystalline preparation method, is characterized in that, in described step 3), 40～80 ℃ adopt platinum resistance to be measured.
6. a kind of prism-shaped NH according to claim 1 4v 3o 8nanocrystalline preparation method, 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 prism-shaped NH according to claim 1 4v 3o 8nanocrystalline preparation method, 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 prism-shaped NH according to claim 1 4v 3o 8nanocrystalline preparation method, 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 (6)

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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
CN105932278A (en) * 2016-04-29 2016-09-07 陕西科技大学 Preparation method of nanosheet self-assembled frustum-shaped (NH4)2V3O8
CN107854861A (en) * 2017-12-04 2018-03-30 太原理工大学 A kind of method of the extract and separate of organic matter in coal carbonaceous residues
CN109761276A (en) * 2018-12-20 2019-05-17 广东工业大学 A kind of stratiform ammonium vanadate electrode material and its preparation method and application
CN111137923A (en) * 2020-01-06 2020-05-12 山东理工大学 Preparation method of prismatic tantalum oxide nano material

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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

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CN102936028A (en) * 2012-11-14 2013-02-20 陕西科技大学 Method for preparing platy lanthanum hydroxide nanocrystalline through microwave-ultrasonic method
CN102942223A (en) * 2012-11-14 2013-02-27 陕西科技大学 Preparation method of hexagonal flaky NH4V3O8 microcrystals

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN105932278A (en) * 2016-04-29 2016-09-07 陕西科技大学 Preparation method of nanosheet self-assembled frustum-shaped (NH4)2V3O8
CN105932278B (en) * 2016-04-29 2019-03-22 陕西科技大学 A kind of nanometer sheet self assembly prism-frustum-shaped (NH4)2V3O8Preparation method
CN107854861A (en) * 2017-12-04 2018-03-30 太原理工大学 A kind of method of the extract and separate of organic matter in coal carbonaceous residues
CN109761276A (en) * 2018-12-20 2019-05-17 广东工业大学 A kind of stratiform ammonium vanadate electrode material and its preparation method and application
CN109761276B (en) * 2018-12-20 2021-08-24 广东工业大学 Layered ammonium vanadate electrode material and preparation method and application thereof
CN111137923A (en) * 2020-01-06 2020-05-12 山东理工大学 Preparation method of prismatic tantalum oxide nano material
CN111137923B (en) * 2020-01-06 2022-08-16 山东理工大学 Preparation method of prismatic tantalum oxide nano material

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