CN105932278B - A kind of nanometer sheet self assembly prism-frustum-shaped (NH4)2V3O8Preparation method - Google Patents
A kind of nanometer sheet self assembly prism-frustum-shaped (NH4)2V3O8Preparation method Download PDFInfo
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- CN105932278B CN105932278B CN201610285837.4A CN201610285837A CN105932278B CN 105932278 B CN105932278 B CN 105932278B CN 201610285837 A CN201610285837 A CN 201610285837A CN 105932278 B CN105932278 B CN 105932278B
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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 present invention provides a kind of nanometer sheet self assembly prism-frustum-shaped (NH4)2V3O8Preparation method, vanadic anhydride is dissolved in deionized water is configured to suspension A first, ammonium hydroxide and ethylene glycol are then added thereto, magnetic agitation obtains solution B until suspension becomes clarification.Then, solution B is fitted into hydrothermal reaction kettle to be placed in homogeneous reaction instrument, natural cooling after hydro-thermal reaction.Finally, collecting after product washing, alcohol are washed, being dry, the prism-frustum-shaped (NH of nanometer sheet self assembly can be obtained4)2V3O8.This method simple process is easily-controllable, (the NH of preparation4)2V3O8Crystallite chemical composition is uniform, and purity is higher, shows good chemical property when being used as anode material for lithium-ion batteries.In addition, this method does not need large scale equipment and harsh reaction condition, raw material is cheap and easy to get, and preparation cost is low, and yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to be mass produced.
Description
[technical field]
The present invention relates to a kind of preparation methods of ion secondary battery positive electrode, and in particular to a kind of nanometer sheet self assembly
Prism-frustum-shaped (NH4)2V3O8Preparation method.
[background technique]
Lithium ion secondary battery is high with voltage, specific energy is big, have extended cycle life, discharge performance is stable, safety is good, nothing
The advantages that pollution and operating temperature range are wide, becomes research hotspot [Tarascon J M, Armand M.Issues in recent years
and challenges facing rechargeable lithium batteries[J].Nature,2001,414
(6861):359-367].Positive electrode accounts for the 35~40% of entire lithium ion battery cost, is the key that development.It is commercialized
Positive electrode (such as LiCoO2、LiMn2O4、 LiFePO4) capacity is generally less than 150mAhg-1, far from meeting high energy in the future
The requirement of high power battery.LiV3O8By high capacity (theoretical value 300mAhg-1), it is considered to be in vanadic acid salt system most
There is one of the positive electrode of commercial promise.But its structure less stable in charge and discharge process, though initial charge/discharge capacity is high,
Capacity attenuation is serious, and cyclical stability is poor, constrains its development and applies [A.WADSLEY, Crystal chemistry of
non-stoichiometric pentavalent vandadium oxides:crystal structure of Li1+xV3O8
[J],Acta Crystallographica.Section A,1957,4(10):261-267].NH with relatively large radius4+It can
Effectively to increase the interlamellar spacing between vanadium oxygen layer, promote Li+Quick transmission, can also interlayer formed intramolecular hydrogen bond, surely
Its fixed crystal structure, thus ammonium vanadate has structural stability more superior than lithium vanadate.Research is it has also been found that its actual discharge holds
Amount is not less than LiV3O8, and cost is lower, is a kind of more promising anode material for lithium-ion batteries.
NH is concentrated mainly on about the report of ammonium vanadate at present4V3O8Research, related scholar by control liquid phase method synthesis
Nanometer rods, micro belt, nanobelt and the isostructural NH of nano wire4V3O8, and F-doped or and carbon nanotube has been carried out to it
Compound etc. [preparation of Wang Haiyan novel high-performance vanadate electrode material and lithium ion deintercalation mechanism study [D] Central South University,
2012].In addition, by its chemical property the study found that NH4V3O8Material shows excellent cyclical stability.
(NH4)2V3O8Belong to tetragonal crystal system, possesses typical two-dimensional layered structure [Liu G, Greedan J E.Magnetic
properties of fresnoite-type vanadium oxides:A2V3O8(A=K, Rb, NH4)[J].Journal of
Solid State Chemistry, 1995,114 (2): 499-505], but about its liquid phase especially hydrothermal synthesis
Seldom, the report about its chemical property is less for report.
[summary of the invention]
The purpose of the present invention is to provide a kind of nanometer sheet self assembly prism-frustum-shaped (NH4)2V3O8Preparation method, operation
Simply, reaction temperature is low, reaction time is short, (NH obtained4)2V3O8Chemical constituent is uniform, purity is high.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of nanometer sheet self assembly prism-frustum-shaped (NH4)2V3O8Preparation method, after being completely dissolved vanadium source, the concentration control of vanadium
System is put it into hydrothermal reaction kettle in 0.108~1mol/L, reacts 6~24 hours under conditions of 120~200 DEG C, instead
It is cooling after answering, drying;Vanadium source dissolution method are as follows: vanadium source is dissolved in deionized water first be configured to it is suspended
Then ammonium hydroxide, Organic Alcohol is successively added in liquid into the suspension, stirring is until vanadium source is completely dissolved.
Further, the vanadium source is vanadic anhydride, sodium metavanadate or ammonium metavanadate.
Further, the Organic Alcohol is ethylene glycol, ethyl alcohol or isopropanol.
Further, the stirring is magnetic agitation or ultrasonic activation.
Further, the speed of the magnetic agitation is 400~900r/min.
Further, the ultrasonic activation time is 10~60min.
Further, the product type of cooling after the hydro-thermal reaction uses natural cooling.
Further, the product after the hydro-thermal reaction successively carries out cooling down, washs, collects, drying, detailed process
Are as follows: after product natural cooling, washing 2~5 times, alcohol wash 2~5 times, then the collection of products after washing is placed in baking oven,
And dry 6 under the conditions of 60~120 DEG C~for 24 hours.
Further, the washing is filtering and washing or centrifuge washing, and collection mode is collected by suction or is collected by centrifugation.
Compared with the existing technology, the present invention at least has the advantages that
The present invention is using at a lower temperature using the method preparation nanometer sheet self assembly prism-frustum-shaped (NH of hydrothermal synthesis4)2V3O8Nano material, the preparation method is simple, does not need large scale equipment and harsh reaction condition, and raw material is cheap and easy to get, preparation
At low cost, simple process, yield is high, is not necessarily to post-processing, environmentally friendly, can be suitble to be mass produced.Meanwhile passing through control
(NH may be implemented in reactant ratio, reaction temperature and reaction time processed etc.4)2V3O8The control of structure obtains a variety of prism-frustum-shaped knots
Structure, and the control of terrace with edge size may be implemented.In addition, (the NH synthesized by this method4)2V3O8Material has chemical composition equal
One, purity is higher, and good chemical property is shown when as anode material for lithium-ion batteries.
[Detailed description of the invention]
Fig. 1 is nanometer sheet self assembly prism-frustum-shaped (NH prepared by the embodiment of the present invention 14)2V3O8X-ray diffraction (XRD)
Map;
Fig. 2 is self assembly prism-frustum-shaped (NH prepared by the embodiment of the present invention 14)2V3O8Scanning electron microscope (SEM) photo.
[specific embodiment]
Invention is further described in detail with reference to the accompanying drawings and embodiments.
A kind of nanometer sheet self assembly prism-frustum-shaped (NH4)2V3O8Preparation method, comprising the following steps:
(1) vanadium source is dissolved in deionized water and is configured to suspension A, the concentration of vanadium is 0.108~1mol/L at this time, so
Afterwards successively into suspension A be added ammonium hydroxide, Organic Alcohol, stirring until vanadium source be completely dissolved, obtain solution B.Vanadium source is five oxidations
Two vanadium, sodium metavanadate or ammonium metavanadate;Organic Alcohol is ethylene glycol, ethyl alcohol or isopropanol.
Further, the mode of the stirring is magnetic agitation or ultrasonic activation.The speed of the magnetic agitation is 400
~900r/min;The ultrasonic activation time is 10~60min.
(2) solution B is fitted into hydrothermal reaction kettle, and placed it in homogeneous reaction instrument, in 120~200 DEG C of temperature
Under the conditions of, reaction 6~for 24 hours.
(3) to fully reacting after natural cooling, then use filtering and washing or centrifuge washing, by product wash 2~5
Secondary, alcohol washes 2~5 times, then the product collected by suction after washing or be collected by centrifugation is placed in baking oven, and at 60~120 DEG C
Under the conditions of dry 6~for 24 hours, the prism-frustum-shaped (NH of nanometer sheet self assembly can be obtained4)2V3O8。
It is described in detail below by specific embodiment.
Embodiment 1
Step 1: by 1gV2O5It is dissolved in deionized water and is configured to suspension A, the concentration of vanadium is 0.3mol/L at this time, so
9mL ammonium hydroxide ultrasonic activation 10min is added in backward suspension A, adds 10mL ethylene glycol ultrasonic activation 30min, until
V2O5It is completely dissolved, obtains solution B.Vanadic anhydride can be substituted with sodium metavanadate or ammonium metavanadate;Ethylene glycol can use ethyl alcohol or different
Propyl alcohol substitution.
Step 2: solution B is fitted into hydrothermal reaction kettle, and is placed it in homogeneous reaction instrument, in 160 DEG C of temperature strip
Under part, 12h is reacted.
Step 3: then natural cooling after to fully reacting washes product washing 3 times, alcohol 3 times, then will washing
Collection of products afterwards is placed in baking oven, and dry 12h under the conditions of 60 DEG C, and the prism-frustum-shaped of nanometer sheet self assembly can be obtained
(NH4)2V3O8。
From figure 1 it appears that (the NH prepared by this method4)2V3O8With very high crystallinity, and purity
Also higher.
It can be clearly seen that the terrace with edge of self assembly has smooth surface from Fig. 2, and having a size of micron order.
Embodiment 2
Step 1:
By 0.5g V2O5It is dissolved in deionized water and is configured to suspension A, the concentration of vanadium is 0.108mol/L at this time, then
3mL ammonium hydroxide magnetic agitation 5min is added into suspension A, adds 5mL ethylene glycol magnetic agitation 10min, until V2O5It is completely molten
Solution, obtains solution B.The revolving speed of magnetic agitation is 400r/min~600r/min.Vanadic anhydride can use sodium metavanadate or inclined vanadium
Sour ammonium substitution;Ethylene glycol can be substituted with ethyl alcohol or isopropanol.
Step 2: solution B is fitted into hydrothermal reaction kettle, and is placed it in homogeneous reaction instrument, in 120 DEG C of temperature strip
Under part, 6h is reacted.
Step 3: then natural cooling after to fully reacting washes product washing 2 times, alcohol 2 times, then will washing
Collection of products afterwards is placed in baking oven, and dry 6h under the conditions of 80 DEG C, and the prism-frustum-shaped of nanometer sheet self assembly can be obtained
(NH4)2V3O8。
Embodiment 3
Step 1: by 1.5gV2O5It being dissolved in deionized water and is configured to suspension A, the concentration of vanadium is 0.8mol/L at this time,
Then 6mL ammonium hydroxide magnetic agitation 10min is added into suspension A, adds 15mL ethylene glycol magnetic agitation 60min, until
V2O5It is completely dissolved, obtains solution B, the revolving speed of the magnetic agitation is 500r/min~900r/min.Vanadic anhydride is available inclined
Sodium vanadate or ammonium metavanadate substitution;Ethylene glycol can be substituted with ethyl alcohol or isopropanol.
Step 2: solution B is fitted into hydrothermal reaction kettle, and is placed it in homogeneous reaction instrument, in 140 DEG C of temperature strip
Under part, 18h is reacted.
Step 3: then natural cooling after to fully reacting washes product washing 4 times, alcohol 4 times, then will washing
Collection of products afterwards is placed in baking oven, and dry 18h under the conditions of 100 DEG C, and the prism-frustum-shaped of nanometer sheet self assembly can be obtained
(NH4)2V3O8。
Embodiment 4
Step 1: by 2gV2O5It is dissolved in deionized water and is configured to suspension A, the concentration of vanadium is 1mol/L at this time, then
15mL ammonium hydroxide ultrasonic activation 20min is added into suspension A, adds 20mL ethylene glycol ultrasonic activation 60min, until
V2O5It is completely dissolved, obtains solution B, vanadic anhydride can be substituted with sodium metavanadate or ammonium metavanadate;Ethylene glycol can use ethyl alcohol or different
Propyl alcohol substitution.
Step 2: solution B is fitted into hydrothermal reaction kettle, and is placed it in homogeneous reaction instrument, in 200 DEG C of temperature strip
Under part, reaction is for 24 hours.
Step 3: then natural cooling after to fully reacting washes product washing 5 times, alcohol 5 times, then will washing
Collection of products afterwards is placed in baking oven, and for 24 hours, the prism-frustum-shaped of nanometer sheet self assembly can be obtained in drying under the conditions of 120 DEG C
(NH4)2V3O8。
Embodiment 5
Step 1: by 2gV2O5It is dissolved in deionized water and is configured to suspension A, the concentration of vanadium is 0.5mol/L at this time, so
10mL ammonium hydroxide magnetic agitation 60min is added in backward suspension A, 20mL ethylene glycol magnetic agitation 60min is added, until V2O5
It is completely dissolved, obtains solution B, the revolving speed of the magnetic agitation is 600r/min.Vanadic anhydride can use sodium metavanadate or inclined vanadium
Sour ammonium substitution;Ethylene glycol can be substituted with ethyl alcohol or isopropanol.
Step 2: solution B is fitted into hydrothermal reaction kettle, and is placed it in homogeneous reaction instrument, in 180 DEG C of temperature strip
Under part, reaction is for 24 hours.
Step 3: then natural cooling after to fully reacting washes product washing 3 times, alcohol 3 times, then will washing
Collection of products afterwards is placed in baking oven, and dry 14h under the conditions of 70 DEG C, and the prism-frustum-shaped of nanometer sheet self assembly can be obtained
(NH4)2V3O8。
Claims (7)
1. a kind of nanometer sheet self assembly prism-frustum-shaped (NH4)2V3O8Preparation method, which is characterized in that after being completely dissolved vanadium source, vanadium
Concentration be 0.108~1mol/L, put it into hydrothermal reaction kettle, reacted 6~24 hours under conditions of 120~200 DEG C,
After reaction, cooling, drying;The method of vanadium source dissolution are as follows: vanadium source is dissolved in is configured to hang in deionized water first
Then ammonium hydroxide, Organic Alcohol is successively added in turbid into the suspension, stirring is until vanadium source is completely dissolved;The vanadium source is five oxygen
Change two vanadium, sodium metavanadate or ammonium metavanadate;The stirring is magnetic agitation or ultrasonic activation.
2. a kind of nanometer sheet self assembly prism-frustum-shaped (NH according to claim 14)2V3O8Preparation method, which is characterized in that
The Organic Alcohol is ethylene glycol, ethyl alcohol or isopropanol.
3. a kind of nanometer sheet self assembly prism-frustum-shaped (NH according to claim 14)2V3O8Preparation method, which is characterized in that
The speed of the magnetic agitation is 400~900r/min.
4. a kind of nanometer sheet self assembly prism-frustum-shaped (NH according to claim 14)2V3O8Preparation method, which is characterized in that
The ultrasonic activation time is 10~60min.
5. a kind of nanometer sheet self assembly prism-frustum-shaped (NH according to claim 14)2V3O8Preparation method, which is characterized in that
The product type of cooling after hydro-thermal reaction uses natural cooling.
6. a kind of nanometer sheet self assembly prism-frustum-shaped (NH according to claim 14)2V3O8Preparation method, which is characterized in that
Product after hydro-thermal reaction successively carries out cooling down, washs, collects, drying, detailed process are as follows: after product natural cooling, water
Wash 2~5 times, alcohol wash 2~5 times, then the collection of products after washing is placed in baking oven, and under the conditions of 60~120 DEG C do
Dry 6~for 24 hours.
7. a kind of nanometer sheet self assembly prism-frustum-shaped (NH according to claim 64)2V3O8Preparation method, which is characterized in that
The washing is filtering and washing or centrifuge washing, and collection mode is collected by suction or is collected by centrifugation.
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CN107162054B (en) * | 2017-05-16 | 2019-04-02 | 陕西科技大学 | A kind of preparation method of three-dimensional netted ammonium vanadate nanocrystal |
CN107170984B (en) * | 2017-05-24 | 2020-01-24 | 江苏大学 | Preparation method of ammonium vanadate anode material of lithium ion battery |
CN107720822B (en) * | 2017-09-15 | 2019-08-09 | 陕西科技大学 | A kind of preparation method of sea urchin shape anode material for lithium-ion batteries |
CN110065968B (en) * | 2019-04-28 | 2021-06-25 | 陕西科技大学 | Tetragonal phase (NH) with photo-thermal characteristic4)2V3O8Preparation method and application of nanosheet |
CN110255616B (en) * | 2019-07-03 | 2021-06-15 | 陕西科技大学 | Method for preparing ultrathin nano flaky NH4V3O8 nano material under ultrahigh pressure |
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