CN108163891A - A kind of three-dimensional self assembly NaV2O5Nano-powder and preparation method and application - Google Patents
A kind of three-dimensional self assembly NaV2O5Nano-powder and preparation method and application Download PDFInfo
- Publication number
- CN108163891A CN108163891A CN201810117972.7A CN201810117972A CN108163891A CN 108163891 A CN108163891 A CN 108163891A CN 201810117972 A CN201810117972 A CN 201810117972A CN 108163891 A CN108163891 A CN 108163891A
- Authority
- CN
- China
- Prior art keywords
- powder
- nav
- self assembly
- nano
- dimensional self
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- 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
-
- 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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- 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 three-dimensional self assembly NaV2O5Nano-powder and preparation method and application, by sodium metavanadate and Na2S·9H2O, which is added in deionized water, obtains solution A；It is sealed after solution A is poured into reaction liner, liner is placed on hydro-thermal reaction in homogeneous reaction instrument loaded on fixation in outer kettle；Product is collected after hydro-thermal reaction and is alternately cleaned through water and alcohol；The product of collection is placed in the cold well of freeze drier to be freezed and vacuumized and is dried to obtain three-dimensional self assembly NaV2O5Nano-powder.Three-dimensional self assembly NaV2O5Nano-powder is by a diameter of 5~10 μm of micron Shu Zucheng, and micron beam is formed by the sub-micrometer rod self assembly of a diameter of 200nm, and wherein mesomorphic structure is presented in sub-micrometer rod.When being applied to negative electrode of lithium ion battery after after big multiplying power test, back to 100mAg‑1Current density under when, capacity still reaches 291mAhg‑1, in 100mAg‑1Current density under, 360 circle of cycle, capacity reaches 580mAhg‑1, in multiplying power and cycle performance test process, NaV2O5Nano-powder all shows stable coulombic efficiency.
Description
Technical field
The present invention relates to a kind of NaV2O5A kind of powder and preparation method thereof, and in particular to three-dimensional self assembly NaV2O5Nanometer
Powder and preparation method and application.
Background technology
NaV2O5Since it is with unique vanadium oxygen skeleton, the structure of stabilization, larger interlamellar spacing, excellent physical chemistry
The presence of property and a large amount of Lacking oxygens, it is considered to be a kind of very promising energy storage material, and in sodium
Applied [Liu P, Zhou D, Zhu K, Wu Q, Wang Y, Tai G, et al.Bundle- in ion battery anode field
like alpha'-NaV2O5mesocrystals:from synthesis,growth mechanism to analysis of
Na-ion intercalation/deintercalation abilities.Nanoscale.2016；8:1975-85.], so
And not yet about its report as lithium ion battery negative material application.In addition, before about NaV2O5Synthetic method
There are mainly two types of reports.One kind is solid phase method, and with higher synthesis temperature, reaction is complicated, energy consumption is big and of high cost.It is another
Kind is two one-step hydrothermals, although synthesis temperature is low, synthesis flow is tediously long and complex.
Invention content
The purpose of the present invention is to provide a kind of three-dimensional self assembly NaV2O5Nano-powder and preparation method and application.
In order to achieve the above objectives, the present invention is as follows using preparation method：
Step 1：Take 0.8~1.2g sodium metavanadates and 0.05~0.1gNa2S·9H2O is added to 55~65ml deionized waters
In, magnetic agitation or ultrasonic disperse obtain half clear solution A；
Step 2：It is sealed after solution A is poured into reaction liner by 55~65% packing ratio, by liner loaded on solid in outer kettle
Surely be placed in homogeneous reaction instrument, under the speed conditions of 5~15r/min by room temperature be heated to 195~205 DEG C carry out hydro-thermals it is anti-
It should；
Step 3：Reaction kettle is naturally cooled into room temperature after hydro-thermal reaction, collect product and is replaced through water and alcohol clear
It washes 3~6 times；
Step 4：The product of collection is placed in the cold well of freeze drier and freezed, then by the product after freezing
It is placed in pallet, covers seal closure, be evacuated down to 10~20Pa, collecting product after dry 12~18h obtains three-dimensional self assembly
NaV2O5Nano-powder.
The step 1 magnetic agitation or ultrasonic time are 55~65min, and magnetic agitation rotating speed is 800~1000r/min.
The step 2 the hydro-thermal reaction time is 23~25h.
The collection of the step 3 is carried out using suction filtration or centrifugation.
The cleaning of the step 3 is carried out using suction filtration or centrifugation.
The freezing conditions of the step 4 are：It -60~-40 DEG C, freezes 2~5 hours.
The step 4 product is sealed it, and before being put into pallet and being dried, with preservative film to preservative film
It carries out pricking hole processing, to ensure to its abundant drying under lower pressure.
The three-dimensional self assembly NaV as made of the preparation method of the present invention2O5Nano-powder is by a diameter of 5~10 μm of micron
Shu Zucheng, micron beam are formed by the sub-micrometer rod self assembly of a diameter of 200nm, and wherein mesomorphic structure is presented in sub-micrometer rod.
By the three-dimensional self assembly NaV of the present invention2O5Application of nanopowder when negative electrode of lithium ion battery, 100,200,
500th, 1000 and 2000mAg-1Current density under, capacity can respectively reach 259,232,192,151 and 115mAhg-1,
After big multiplying power test, back to 100mAg-1Current density under when, capacity still reaches 291mAhg-1,
100mAg-1Current density under, 360 circle of cycle, capacity reaches 580mAhg-1, in multiplying power and cycle performance test process,
NaV2O5Nano-powder all shows stable coulombic efficiency.
The present invention has synthesized the three-dimensional self assembly NaV of high-purity using extremely simple efficient step hydrothermal reaction at low temperature2O5It receives
Rice flour body, this method reaction process is simple and easy to control, temperature is low, synthetic product yield is high and does not need to large scale equipment and harshness
Reaction condition.When applying above-mentioned product for lithium ion battery negative material, excellent multiplying power and cycle performance are shown.
It is embodied in：
1) present invention using a step hydro-thermal reaction due to directly synthesizing final product, thus has low synthesis temperature
Degree does not need to large scale equipment and harsh reaction condition；
2) present invention makes full use of micro Na2S·9H2O is dissolved in the S provided after water2-The reproducibility of ion, by raw material NaVO3
It has been directly reduced to NaV2O5, thus with simple synthesis path, reaction is easily-controllable, yield is high, without post-processing, to environment
Close friend can be suitble to mass produce；
3) the raw materials used in the present invention is sodium metavanadate and Na2S·9H2O, solvent use deionized water, they are common objects
Matter, it is cheap and easy to get, at low cost；
4) present invention needs stringent control Na2S·9H2The addition of O, very few addition can not be by NaVO3Fully also
Originally it was NaV2O5, excessive addition then will generation nanometer chip architecture.Therefore, Na2S·9H2The addition of O is for three-dimensional from group
Fill NaV2O5The synthesis of nano-powder plays very crucial effect；
5) present invention also needs to stringent controlling reaction temperature, and too low reaction temperature is unfavorable for three-dimensional self assembly NaV2O5It receives
The generation of rice flour body；
6) present invention does not introduce any template or surfactant during the three-dimensional self-assembled structures of synthesis,
Entire self assembling process is the topology conversion control by reaction raw materials, thus entirely reacts simple, easily-controllable, efficient and inexpensive；
7) NaV prepared by the present invention2O5There are a large amount of Lacking oxygen, storage and quick transmission for lithium ion provide on surface
A large amount of active site；
8) the three-dimensional self assembly NaV prepared by the present invention2O5There is nano-powder unique sub-micrometer rod to be self-assembled into micron
The three-dimensional structure of stick.On the one hand the self-assembled structures that this sub-micrometer rod contacts with each other can play good physics confinement and make
With another aspect also provides cushion space to the expansion of sub-micrometer rod and contraction, so as to greatly alleviate sub-micrometer rod
Volume change, finally significantly improve its cyclical stability；
9) the three-dimensional self assembly NaV prepared by the present invention2O5The smaller scale of construct sub-micrometer rod in nano-powder, no
Larger specific surface area can be only generated, but also more surface-active sites can be provided, and then electrochemistry can be promoted
Performance.In addition, this extra small scale can not only shorten charge transfer path, but also can be provided for the storage of lithium ion
More active sites, so as to promote the specific capacity of material and high rate performance；
10) the three-dimensional self assembly NaV prepared by the present invention2O5Construct sub-micrometer rod NaV in nano-powder2O5With edge
(001) Jie of high preferred orientation growth sees crystal property, and larger interplanar distance can be the quick abundant hair of electrochemical reaction
It is raw that preferably space is provided.Meanwhile NaV2O5The single crystal characteristics for seeing crystal that are situated between and high crystallinity, can make it in charge and discharge
Excellent structural stability is shown in journey；
11) the product chemistry composition of the invention prepared is uniform, purity is high, pattern is uniform, is used as negative electrode of lithium ion battery
Excellent chemical property can be shown during material.In 0.01~3.0 voltage range, in 100,200,500,1000 and
2000mAg-1Current density under, show up to 259,232,192,151 and 115mAhg-1Specific capacity, when back to
100mAg-1Current density under, capacity can reach 291mAhg-1.In 100mAg-1Current density under, cycle 360 circle, hold
Amount can reach 580mAhg-1.In addition, in the test process of entire multiplying power and cycle performance, stable coulomb effect is all shown
Rate.
Description of the drawings
Fig. 1 is the X-ray diffractogram that the embodiment of the present invention 1 prepares product.
Fig. 2 is the scanning electron microscope (SEM) photograph of the raw materials used in the present invention sodium metavanadate.
Fig. 3 is the low power scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 prepares product.
Fig. 4 is the high power SEM figures that the embodiment of the present invention 1 prepares product.
Fig. 5 is the super-high power SEM figures that the embodiment of the present invention 1 prepares product.
Fig. 6 is the transmission electron microscope picture that the embodiment of the present invention 1 prepares product.
Fig. 7 is the diffraction pattern figure that the embodiment of the present invention 1 prepares product.
Fig. 8 is the high rate performance when embodiment of the present invention 1 prepares product as negative electrode of lithium ion battery.
Fig. 9 is the cycle performance when embodiment of the present invention 1 prepares product as lithium ion battery negative material.
Figure 10 is to work as Na in the embodiment of the present invention 12S·9H2When the additive amount of O is increased to 0.5g, the structure of synthetic product is
Nanometer chip architecture.
Specific embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings.
Embodiment 1：
Step 1：Take 1.0g sodium metavanadates and 0.08gNa2S·9H2O is added in 60ml deionized waters, with 800r/min
Lower magnetic agitation 65min obtains half clear solution A；
Step 2：It seals, liner is loaded in outer kettle after fixing after solution A is poured into reaction liner by 60% packing ratio
It is placed in homogeneous reaction instrument, being heated to 200 DEG C by room temperature under the speed conditions of 10r/min carries out hydro-thermal reaction for 24 hours；
Step 3：Reaction kettle is naturally cooled into room temperature after hydro-thermal reaction, using collected by suction product and through water and
Alcohol is cleaned 3 times using alternating is filtered；
Step 4：The product of collection is placed in the cold well of freeze drier in -60 DEG C, freezed 2 hours, it then will freezing
Product afterwards is placed in pallet, covers seal closure, is evacuated down to 15Pa, and collecting product after dry 12h obtains three-dimensional self assembly
NaV2O5Nano-powder.
It can be clearly seen that the diffraction maximum of synthesized product and orthorhombic phase NaV from Fig. 12O5Standard card PDF#89-
8040 fit like a glove, and the product for illustrating synthesis is pure phase orthorhombic phase NaV2O5.In addition, smooth elongated diffraction maximum illustrates the product
With good crystallinity, and the corresponding diffraction peak intensity of (001) crystal face is most strong, and it is significant along (001) to show that the product has
The characteristic of high preferred orientation growth.
From figure 2 it can be seen that sodium metavanadate raw material is by the micron Shu Zucheng of sub-micro stick self assembly.
From figure 3, it can be seen that products therefrom has shown the microstructure similar to sodium metavanadate raw material, i.e., by uniform
Sub-micro stick be self-assembled into 5~10 μm of micron beams.
It can be clearly seen that sub-micro stick, which closely fits together, forms a micron beam from Fig. 4.
It will be apparent from fig. 5 that the diameter of sub-micro stick is about 200nm, and with larger draw ratio.
Can be with it is further seen that the micro- solid construction of sub-micro stick from Fig. 6, and diameter is about 200nm.
As can be seen from Figure 7 sub-micrometer rod presents clearly mono-crystalline structures.
As can be seen from Figure 8, in 100,200,500,1000 and 2000mAg-1Current density under, capacity can be distinguished
Reach 259,232,192,151 and 115mAhg-1, after big multiplying power test is undergone, back to 100mAg-1Current density
When lower, capacity remains able to reach 291mAhg-1.Meanwhile under the conditions of different multiplying powers, product has all shown excellent library
Human relations efficiency,
It can be seen in figure 9 that in 100mAg-1Current density under 360 circle of cycle, capacity can reach 580mAhg-1。
Meanwhile entire cyclic process all shows stable coulombic efficiency.
Figure 10 is to work as Na in the embodiment of the present invention 12S·9H2When the additive amount of O is increased to 0.5g, the structure of synthetic product is
Nanometer chip architecture.It is noted that when being added without Na2S·9H2It is clear solution after hydro-thermal reaction, and deposit-free produces during O
It is raw.When by reaction temperature is reduced to 180 DEG C in the embodiment of the present invention 1 when, be clear solution after hydro-thermal reaction, also deposit-free produces
It is raw.Therefore, very few Na2S·9H2O is added in and too low reaction temperature is all unfavorable for NaV2O5Synthesis.
Embodiment 2：
Step 1：Take 0.8g sodium metavanadates and 0.05gNa2S·9H2O is added in 55ml deionized waters, with 900r/min
Lower magnetic agitation 60min obtains half clear solution A；
Step 2：It seals, liner is loaded in outer kettle after fixing after solution A is poured into reaction liner by 58% packing ratio
It is placed in homogeneous reaction instrument, being heated to 195 DEG C by room temperature under the speed conditions of 8r/min carries out hydro-thermal reaction 25h；
Step 3：Reaction kettle is naturally cooled into room temperature after hydro-thermal reaction, using product is collected by centrifugation and through water and
Alcohol is using centrifugation alternately cleaning 5 times；
Step 4：The product of collection is placed in the cold well of freeze drier in -55 DEG C, freezed 3 hours, it then will freezing
Product afterwards is placed in pallet, it is sealed with preservative film, and preservative film is carried out to prick hole processing, is covered seal closure, is taken out
Vacuum is to 12Pa, and collection product obtains three-dimensional self assembly NaV after drying 15h2O5Nano-powder.
Embodiment 3：
Step 1：Take 1.2g sodium metavanadates and 0.06gNa2S·9H2O is added in 65ml deionized waters, with 1000r/min
Lower magnetic agitation 55min obtains half clear solution A；
Step 2：It seals, liner is loaded in outer kettle after fixing after solution A is poured into reaction liner by 65% packing ratio
It is placed in homogeneous reaction instrument, being heated to 205 DEG C by room temperature under the speed conditions of 12r/min carries out hydro-thermal reaction 23h；
Step 3：Reaction kettle is naturally cooled into room temperature after hydro-thermal reaction, using collected by suction product and through water and
Alcohol is using centrifugation alternately cleaning 4 times；
Step 4：The product of collection is placed in the cold well of freeze drier in -45 DEG C, freezed 4 hours, it then will freezing
Product afterwards is placed in pallet, it is sealed with preservative film, and preservative film is carried out to prick hole processing, is covered seal closure, is taken out
Vacuum is to 18Pa, and collection product obtains three-dimensional self assembly NaV after drying 18h2O5Nano-powder.
Embodiment 4：
Step 1：Take 0.9g sodium metavanadates and 0.07gNa2S·9H2O is added in 58ml deionized waters, ultrasonic disperse
58min obtains half clear solution A；
Step 2：It seals, liner is loaded in outer kettle after fixing after solution A is poured into reaction liner by 55% packing ratio
It is placed in homogeneous reaction instrument, being heated to 198 DEG C by room temperature under the speed conditions of 5r/min carries out hydro-thermal reaction 25h；
Step 3：Reaction kettle is naturally cooled into room temperature after hydro-thermal reaction, using product is collected by centrifugation and through water and
Alcohol is cleaned 6 times using alternating is filtered；
Step 4：The product of collection is placed in the cold well of freeze drier in -40 DEG C, freezed 5 hours, it then will freezing
Product afterwards is placed in pallet, it is sealed with preservative film, and preservative film is carried out to prick hole processing, is covered seal closure, is taken out
Vacuum is to 10Pa, and collection product obtains three-dimensional self assembly NaV after drying 16h2O5Nano-powder.
Embodiment 5：
Step 1：Take 1.1g sodium metavanadates and 0.1gNa2S·9H2O is added in 62ml deionized waters, ultrasonic disperse
63min obtains half clear solution A；
Step 2：It seals, liner is loaded in outer kettle after fixing after solution A is poured into reaction liner by 62% packing ratio
It is placed in homogeneous reaction instrument, being heated to 202 DEG C by room temperature under the speed conditions of 15r/min carries out hydro-thermal reaction for 24 hours；
Step 3：Reaction kettle is naturally cooled into room temperature after hydro-thermal reaction, using product is collected by centrifugation and through water and
Alcohol is using centrifugation alternately cleaning 5 times；
Step 4：The product of collection is placed in the cold well of freeze drier in -50 DEG C, freezed 4 hours, it then will freezing
Product afterwards is placed in pallet, it is sealed with preservative film, and preservative film is carried out to prick hole processing, is covered seal closure, is taken out
Vacuum is to 20Pa, and collection product obtains three-dimensional self assembly NaV after drying 13h2O5Nano-powder.
Claims (9)
1. a kind of three-dimensional self assembly NaV2O5The preparation method of nano-powder, it is characterised in that：
Step 1：Take 0.8~1.2g sodium metavanadates and 0.05~0.1gNa2S·9H2O is added in 55~65ml deionized waters,
Magnetic agitation or ultrasonic disperse obtain half clear solution A；
Step 2：It seals, liner is loaded in outer kettle after fixing after solution A is poured into reaction liner by 55~65% packing ratio
It is placed in homogeneous reaction instrument, 195~205 DEG C of progress hydro-thermal reactions is heated to by room temperature under the speed conditions of 5~15r/min；
Step 3：Reaction kettle is naturally cooled into room temperature after hydro-thermal reaction, collect product and through water and alcohol alternately cleaning 3~
6 times；
Step 4：The product of collection is placed in the cold well of freeze drier and freezed, be then placed in the product after freezing
In pallet, seal closure is covered, is evacuated down to 10~20Pa, collecting product after dry 12~18h obtains three-dimensional self assembly NaV2O5
Nano-powder.
2. three-dimensional self assembly NaV according to claim 12O5The preparation method of nano-powder, it is characterised in that：The step
A rapid magnetic agitation or ultrasonic time are 55~65min, and magnetic agitation rotating speed is 800~1000r/min.
3. three-dimensional self assembly NaV according to claim 12O5The preparation method of nano-powder, it is characterised in that：The step
Rapid two the hydro-thermal reaction time is 23~25h.
4. three-dimensional self assembly NaV according to claim 12O5The preparation method of nano-powder, it is characterised in that：The step
Rapid three collection is carried out using suction filtration or centrifugation.
5. three-dimensional self assembly NaV according to claim 12O5The preparation method of nano-powder, it is characterised in that：The step
Rapid three cleaning is carried out using suction filtration or centrifugation.
6. three-dimensional self assembly NaV according to claim 12O5The preparation method of nano-powder, it is characterised in that：The step
Rapid four freezing conditions are：It -60~-40 DEG C, freezes 2~5 hours.
7. three-dimensional self assembly NaV according to claim 12O5The preparation method of nano-powder, it is characterised in that：The step
Rapid four product is sealed it before being put into pallet and being dried, with preservative film, and preservative film is carried out to prick hole processing, with
Ensure to its abundant drying under lower pressure.
8. a kind of three-dimensional self assembly NaV made of preparation method as described in claim 12O5Nano-powder, it is characterised in that：
Three-dimensional self assembly NaV2O5For nano-powder by a diameter of 5~10 μm of micron Shu Zucheng, micron beam is by the Asia of a diameter of 200nm
Micron bar self assembly forms, and wherein mesomorphic structure is presented in sub-micrometer rod.
9. a kind of three-dimensional self assembly NaV made of preparation method as described in claim 12O5Application of nanopowder is in lithium ion
During battery cathode, in 100,200,500,1000 and 2000mAg-1Current density under, capacity can respectively reach 259,232,
192nd, 151 and 115mAhg-1, after after big multiplying power test, back to 100mAg-1Current density under when, capacity is still
So reach 291mAhg-1, in 100mAg-1Current density under, 360 circle of cycle, capacity reaches 580mAhg-1, in multiplying power and cycle
During performance test, NaV2O5Nano-powder all shows stable coulombic efficiency.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810117972.7A CN108163891B (en) | 2018-02-06 | 2018-02-06 | Three-dimensional self-assembly NaV2O5Micron powder and preparation method and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810117972.7A CN108163891B (en) | 2018-02-06 | 2018-02-06 | Three-dimensional self-assembly NaV2O5Micron powder and preparation method and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108163891A true CN108163891A (en) | 2018-06-15 |
| CN108163891B CN108163891B (en) | 2020-09-22 |
Family
ID=62513292
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810117972.7A Active CN108163891B (en) | 2018-02-06 | 2018-02-06 | Three-dimensional self-assembly NaV2O5Micron powder and preparation method and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108163891B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110467221A (en) * | 2019-09-17 | 2019-11-19 | 安徽建筑大学 | A kind of NaV6O15The preparation method of film and NaV obtained6O15Film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102417206A (en) * | 2011-08-30 | 2012-04-18 | 河北工业大学 | Preparation method of NaV2O5 crystal material with right angle morphology |
| CN102557131A (en) * | 2010-12-07 | 2012-07-11 | 吉林师范大学 | Preparation method for NaV2O5 |
| CN106335924A (en) * | 2016-08-12 | 2017-01-18 | 武汉理工大学 | Preparation method of NaV2O5 |
-
2018
- 2018-02-06 CN CN201810117972.7A patent/CN108163891B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102557131A (en) * | 2010-12-07 | 2012-07-11 | 吉林师范大学 | Preparation method for NaV2O5 |
| CN102417206A (en) * | 2011-08-30 | 2012-04-18 | 河北工业大学 | Preparation method of NaV2O5 crystal material with right angle morphology |
| CN106335924A (en) * | 2016-08-12 | 2017-01-18 | 武汉理工大学 | Preparation method of NaV2O5 |
Non-Patent Citations (4)
| Title |
|---|
| G UI ZHOU等: "Hydrothermal synthesis and magnetic property of NaV2O5 nanorods", 《TRANS.NONFERROUS MET.SOC .CHINA》 * |
| HU FANG等: "Physical and Electrochemical Characterization of", 《CHEM. RES. CHINESE UNIVERSITIES》 * |
| 刘鹏程等: "新型钠离子电池正极材料a－ＮaＶ2O5 纳米带的水热合成及表", 《中国硅酸盐学会陶瓷分会2016学术年会会刊》 * |
| 胡方等: "钒酸盐化合物NaV2O5的水热合成及电化学性质", 《电化学》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110467221A (en) * | 2019-09-17 | 2019-11-19 | 安徽建筑大学 | A kind of NaV6O15The preparation method of film and NaV obtained6O15Film |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108163891B (en) | 2020-09-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107840368B (en) | A kind of nanometer sheet self assembly sub-micrometer flower-shape M-phase vanadium dioxide powder and preparation method thereof | |
| CN106532015B (en) | Molybdenum disulfide hybrid titanium carbide lithium ion battery negative material and preparation method thereof | |
| CN110534741A (en) | A kind of fast preparation method and application of few layer MXenes | |
| CN107902697B (en) | A kind of nanometer sheet self assembled three-dimensional VS of (001) orientation2Micron bar and preparation method thereof | |
| CN108585042A (en) | A kind of extra small flower-shaped VS of nanometer sheet self assembly2Powder and preparation method thereof | |
| CN107221646B (en) | A kind of vanadium disulfide nanometer sheet and its preparation method and application of hydroxide vanadyl cladding | |
| CN107381636A (en) | A kind of vanadic sulfide powder of nano-particles self assemble three dimensional micron cauliflower-shaped four and its preparation method and application | |
| CN105845915B (en) | A kind of preparation method of three-dimensional porous carbon skeleton/CoO negative pole of lithium ion battery with compound structure material | |
| CN108899504A (en) | A kind of antimony-carbon nanotube-carbon composite, preparation method and application | |
| CN110336021A (en) | Graphene and/or compound Na2Fe (SO4) 2/C electrode material, preparation method and the battery of preparation of acetylene black | |
| CN109449402A (en) | A kind of nano carbon microsphere supports preparation and its application method of MXene composite material | |
| CN108126712A (en) | A kind of VOOH/VS4Micron composite granule and preparation method and application | |
| CN109888223A (en) | A kind of preparation method and application of four vanadic sulfides@redox graphene composite granule | |
| CN106129407A (en) | MoS2the synthetic method of@graphene composite nano material | |
| CN108423711A (en) | A kind of tetragonal phase NaV2O5·H2O nano-sheet powders and its preparation method and application | |
| CN109748319A (en) | A kind of preparation method and application of four vanadic sulfides@carbon nano-tube composite powder | |
| CN108539175A (en) | A kind of molybdenum disulfide/stannic disulfide/graphene composite material and preparation method thereof | |
| CN108365185A (en) | The preparation method of porous manganese sulfide and graphene composite material | |
| CN104466110B (en) | Preparation method of high-performance lithium ion battery negative electrode material | |
| CN108110246A (en) | A kind of extra small VS4/ Super P composite nano-powders and preparation method and application | |
| Yang et al. | Synthesis of flower-like nickel oxide/nickel silicate nanocomposites and their enhanced electrochemical performance as anode materials for lithium batteries | |
| CN108767203B (en) | Titanium dioxide nanotube-graphene-sulfur composite material and preparation method and application thereof | |
| CN108172805A (en) | A kind of carbon coating nickel cobalt molybdenum oxide combination electrode material and preparation method thereof | |
| CN107792878A (en) | A kind of graded structure titanium dioxide（B）Preparation method and its application in lithium ion battery | |
| CN102544457A (en) | Method for preparing graphene oxide-iron sesquioxide nanotube composite material by using in-situ method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |