CN105731539B - Method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with high-temperature and high-pressure mixed solvent thermal system - Google Patents
Method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with high-temperature and high-pressure mixed solvent thermal system Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 47
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 43
- 239000012046 mixed solvent Substances 0.000 title claims abstract description 43
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 39
- 229910011312 Li3VO4 Inorganic materials 0.000 title claims abstract description 23
- 230000002194 synthesizing effect Effects 0.000 title abstract description 4
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 239000007787 solid Substances 0.000 claims abstract description 25
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 239000000463 material Substances 0.000 claims description 17
- 238000005406 washing Methods 0.000 claims description 14
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 11
- 239000012498 ultrapure water Substances 0.000 claims description 11
- 238000005119 centrifugation Methods 0.000 claims description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010304 firing Methods 0.000 claims description 6
- 238000003828 vacuum filtration Methods 0.000 claims description 6
- 239000006194 liquid suspension Substances 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- PNEFIWYZWIQKEK-UHFFFAOYSA-N carbonic acid;lithium Chemical compound [Li].OC(O)=O PNEFIWYZWIQKEK-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- WQEVDHBJGNOKKO-UHFFFAOYSA-K vanadic acid Chemical compound O[V](O)(O)=O WQEVDHBJGNOKKO-UHFFFAOYSA-K 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 7
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000012429 reaction media Substances 0.000 abstract description 2
- 238000004134 energy conservation Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 11
- 238000007789 sealing Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 7
- 238000010189 synthetic method Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 description 4
- 239000002244 precipitate Substances 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 239000010406 cathode material Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052809 inorganic oxide Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- -1 oxygen-containing inorganic metal compound Chemical class 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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
-
- 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
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- 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
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for synthesizing lithium vanadate Li3VO4 monocrystal micrometer powder with a high-temperature and high-pressure mixed solvent thermal system.The method comprises the steps that solid lithium carbonate powder and solid vanadium pentoxide serve as raw materials, a high-temperature and high-pressure mixed solvent serves as a reaction medium, and the lithium vanadate Li3VO4 monocrystal micrometer powder is synthesized with the condition ranges of 2-9 MPa, 200-350 DEG C and 1-4 h.The method has a unique advantage, the lithium vanadate Li3VO4 monocrystal micrometer powder can be quickly, easily and conveniently obtained, the physical phase is pure, the particle size ranges from 1 micrometer to 20 micrometers, and the dispersibility is good.The synthesizing method is easy, convenient and safe to implement, equipment is convenient to use and simple, the reaction process is easy to control, energy conservation and environment protection are achieved, and the method is especially suitable for industrialized mass production.
Description
Technical field
The present invention relates to it is a kind of can as the preparation method of the compound monocrystal micrometer structure of lithium ion battery negative material,
More particularly to it is a kind of using High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li3VO4The method of monocrystalline micron powder.
Background technology
Lithium vanadate Li3VO4It is a kind of widely used material.Its crystal structure is tied for the non-centrosymmetry of Pmn21 types
Structure, has more extensive research to performances such as its nonlinear opticses before.Li3VO4Theoretical capacity be 394mAh/g, have
Cyclicity is good, the more low feature of potential of charging and discharging.Research discovery, lithium vanadate Li3VO4It is likely to be a kind of performance excellent
Good lithium ion battery negative material.
According to the literature, lithium vanadate Li3VO4The synthetic method of dusty material typically has following several：Conventional solid synthesizes
Method, sol-gal process, common hydro-thermal method etc..These methods there are problems that at present.The powder product that solid phase synthesis are obtained
Granule-morphology is uneven, specific surface area is little, reunion is serious etc., and sol-gal process and common hydro-thermal method batching step are complicated, process
Time is longer, technique is relatively complicated etc..The pattern of material, microcrystal grain distribution of sizes, dispersibility of granule etc. are to material property
May produce greatly affects." green chemistry chemical technology " process for advocating energy-conserving and environment-protective also complies with the neck such as materialogy, chemical engineering
The development trend in domain.Therefore thing is mutually pure, granule-morphology is uniformly regular to obtain to study quick, safe and simple synthetic method
Lithium vanadate Li3VO4Dusty material has important scientific research meaning.However, Jing retrievals there is presently no and utilize High Temperature High Pressure
Mixed solvent hot system synthesizes lithium vanadate Li3VO4The pertinent literature report of monocrystalline micron powder.
The content of the invention
For the not enough and drawback of existing synthetic technology, the invention provides a kind of simple and feasible utilization High Temperature High Pressure is mixed
Bonding solvent hot system synthesizes lithium vanadate Li3VO4The method of monocrystalline micron powder.
Utilization High Temperature High Pressure mixed solvent hot system of the present invention synthesizes lithium vanadate Li3VO4The side of monocrystalline micron powder
Method, step is：
(1) dispensing：Will be used as synthesis target lithium vanadate Li3VO4In raw material components Li, V according to atomic ratio Li V=3 1
Ratio, in the form of solid carbonic acid lithium powder and solid vanadium pentoxide powder mix；
(2) prepare mixed solvent：Acetone is mixed according to the arbitrary proportion between volume ratio 19 to 91 with ultra-pure water, is made
Obtain mixed solvent；
(3) dispersed material：Step (1) mixed pressed powder is scattered in the mixed solvent prepared by step (2),
Solid-liquid suspension body is formed, the amount of wherein mixed solvent is 50～120 times of powder material volume；
(4) implement isothermal reaction using High Temperature High Pressure mixed solvent hot system；
(5) cool down：After isothermal reaction, reaction vessel is cooled down, container inner pressure is down to normal pressure；
(6) wash：The solid in reaction vessel is separated with liquid using centrifugation or with Vacuum filtration device, with super
Solid precipitation obtained by pure water, ethanol or washing with acetone at least 3 times, or the liquid pH=7 after washing to washing stops；
(7) dry：Solid precipitation after step (6) is washed drying equipment is dried, and the product of acquisition is pure phase
Lithium vanadate Li3VO4Monocrystalline micron powder；
It is characterized in that：
Step (4) the utilization High Temperature High Pressure mixed solvent hot system implements the method for isothermal reaction：Step (3) is obtained
To solid-liquid suspension body be put in high-temperature high-voltage reaction container, it is closed after reaction vessel is put be heated in firing equipment 200～
350 DEG C, container inner pressure be 2～9MPa, isothermal reaction 1～4 hour, now the technical characteristic of reaction system be High Temperature High Pressure mix
Bonding solvent thermal response system；Wherein, the high-temperature high-voltage reaction container is the high-temperature high-voltage reaction with thermometric, pressure tester
Kettle；The firing equipment refers to one of the Muffle furnace of precise control of temperature device, resistance furnace, tube furnace, baking oven；
Step (5) reaction vessel is cooled to 20～25 DEG C, and the mode of cooling is that heater is cold according to setting speed
But to room temperature, or directly cooling in power-off stove, or reaction vessel is directly taken out from heater natural cooling, or will
Reaction vessel is cooled down in being put into frozen water after taking out from heater；
The condition that step (6) centrifugation is implemented is：1000～2000 revs/min of centrifugal rotational speed, centrifugation time 10～
20 minutes；The Vacuum filtration device adopts aperture for 0.2～0.5 micron of filtering membrane of filter；
Step (7) drying equipment is baking oven, drying baker or infrared lamp, and drying temperature is 50～60 DEG C.
Above-mentioned utilization High Temperature High Pressure mixed solvent hot system synthesizes lithium vanadate Li3VO4In the method for monocrystalline micron powder：Step
Suddenly (2) described acetone and ultra-pure water are preferably according to volume ratio 1:2 to 2:Arbitrary proportion mixing between 1.
Above-mentioned utilization High Temperature High Pressure mixed solvent hot system synthesizes lithium vanadate Li3VO4In the method for monocrystalline micron powder：Step
Suddenly the amount of (3) described mixed solvent is preferably 60～90 times of powder material volume.
Above-mentioned utilization High Temperature High Pressure mixed solvent hot system synthesizes lithium vanadate Li3VO4In the method for monocrystalline micron powder：Step
Suddenly preferably 250～300 DEG C of (4) described heating-up temperature, container inner pressure are preferably 6～9MPa, and isothermal reaction time preferably 1～
2 hours；The firing equipment refers to the Muffle furnace of precise control of temperature device.
Above-mentioned utilization High Temperature High Pressure mixed solvent hot system synthesizes lithium vanadate Li3VO4In the method for monocrystalline micron powder：Step
Suddenly the condition of (6) described centrifugation is preferably：1500 revs/min of centrifugal rotational speed, centrifugation time 20 minutes.
Above-mentioned utilization High Temperature High Pressure mixed solvent hot system synthesizes lithium vanadate Li3VO4In the method for monocrystalline micron powder：Step
Suddenly (6) described Vacuum filtration device preferably adopts aperture for 0.22～0.45 micron of filtering membrane of filter.
The utilization High Temperature High Pressure mixed solvent hot system synthesis lithium vanadate Li that the present invention is provided3VO4The side of monocrystalline micron powder
Method has unique advantage, can obtain lithium vanadate Li with quick, safe and simple method3VO4Monocrystalline micro-powder material, solution
Some problems determined in the presence of current synthetic process, promote novel cathode material for lithium ion battery synthesis and should
With the development for waiting sciemtifec and technical sphere.
In the inventive method, it is raw material by conventional solid phase inorganic salt and oxide first, is made with acetone and aqueous mixtures
For reaction media, lithium vanadate is synthesized in 2～9MPa, 200～350 DEG C of temperature range, 1～4 little the reaction time
Li3VO4Monocrystalline micron dusty material.The lithium vanadate Li synthesized with the method3VO4Monocrystalline micron dusty material, thing are mutually pure,
Particle shape looks are more regular, and particle size range is 1～20 micron, and granule is difficult to reunite, and dispersibility is relatively good.
The inventive method has used the reactant feed of solid phase, with High Temperature High Pressure mixed solvent hot system as reactant
System, simplifies synthesis step, and course of reaction is quick, while reducing the unsafe factor in building-up process, easily realizes synthesis
The control of process and the control of product grain pattern.Because preparation of raw material, consersion unit are fairly simple, course of reaction is easily adjusted
Control, the inventive method are particularly suitable for industrialized mass production.
The lithium vanadate Li that the present invention is provided3VO4The High Temperature High Pressure mixed solvent hot system synthesis side of monocrystalline micron dusty material
Method applies also for the synthesis of some multivariant oxide monocrystalline micro materials, is a kind of the general of synthesizing oxygen-containing inorganic metal compound
Suitable method.
Description of the drawings
Fig. 1：The lithium vanadate Li prepared using High Temperature High Pressure mixed solvent hot system synthetic method3VO4Microcrystalline powder.
Wherein：Fig. 1 a are X-ray diffracting spectrums；Fig. 1 b are stereoscan photograph.
Fig. 2：The lithium vanadate Li prepared using High Temperature High Pressure mixed solvent hot system synthetic method3VO4Microcrystalline powder.
Wherein：Fig. 2 a are X-ray diffracting spectrums；Fig. 2 b are stereoscan photograph.
Fig. 3：The lithium vanadate Li prepared using High Temperature High Pressure mixed solvent hot system synthetic method3VO4Microcrystalline powder.
Wherein：Fig. 3 a are X-ray diffracting spectrums；Fig. 3 b are stereoscan photograph.
Fig. 4：The lithium vanadate Li prepared using High Temperature High Pressure mixed solvent hot system synthetic method3VO4Microcrystalline powder.
Wherein：Fig. 4 a are X-ray diffracting spectrums；Fig. 4 b are stereoscan photograph.
Specific embodiment
Embodiment 1
1. dispensing：
By 60ml acetone and 40ml ultra-pure water mix homogeneously, 0.6651 gram of lithium carbonate, 0.5457 gram of vanadic anhydride are mixed
It is distributed to after conjunction in above-mentioned mixed solvent.(volume is to be then added to the high-temperature high-pressure reaction kettle with thermometric, pressure tester
250 milliliters) in, sealing.
2. isothermal reaction is implemented using High Temperature High Pressure mixed solvent hot system：
The reactor of sealing is put in Muffle furnace, is heated to 280 DEG C (container inner pressure reaches 9MPa), it is permanent at this temperature
It is fixed 2 hours.
3. cool down：
Make reactor naturally cool to room temperature (20 DEG C～25 DEG C), reactor is taken out from Muffle furnace.
4. wash：
Product is taken out from reactor, and product is filtered by vacuum filter (aperture is 0.45 micron), solid is obtained
Precipitate；Stopped with the liquid pH=7 after solid precipitation obtained by ultra-pure water, washing with alcohol to washing.
5. dry：
The solid obtained after filtration is dried in the baking oven at a temperature of 50 DEG C～60 DEG C, lithium vanadate Li is obtained3VO4Powder.
X-ray diffraction result shows that the powder that experiment is obtained is the lithium vanadate Li of phase3VO4(Fig. 1 a).Scanning electron shows
Micro mirror observation shows that powder is the Polyhedral Particles (Fig. 1 b) of 1～3 micron of average-size.
Embodiment 2
1. dispensing：
By 60ml acetone and 40ml ultra-pure water mix homogeneously, 0.6651 gram of lithium carbonate, 0.5457 gram of vanadic anhydride are mixed
It is distributed to after conjunction in above-mentioned mixed solvent.(volume is to be then added to the high-temperature high-pressure reaction kettle with thermometric, pressure tester
250 milliliters) in, sealing.
2. isothermal reaction is implemented using High Temperature High Pressure mixed solvent hot system：
The reactor of sealing is put in Muffle furnace, 250 DEG C (container inner pressure reaches 6.2MPa) is heated to, at this temperature
Constant 1 hour.
3. cool down：
Make reactor naturally cool to room temperature (20 DEG C～25 DEG C), reactor is taken out from Muffle furnace.
4. wash：
Product is taken out from reactor, and product is filtered by vacuum filter (aperture is 0.45 micron), solid is obtained
Precipitate；Stopped with the liquid pH=7 after solid precipitation obtained by ultra-pure water, washing with acetone to washing.
5. dry：
The solid obtained after filtration is dried in the baking oven at a temperature of 50 DEG C～60 DEG C, lithium vanadate Li is obtained3VO4Crystallite
Powder.
X-ray diffraction result shows that it is lithium vanadate Li to test the powder for obtaining3VO4(Fig. 2 a).Scanning electron microscope is seen
Examine and show, powder is long 3～5 microns rod-shpaed particle (Fig. 2 b) of 1 micron of average-size diameter.
Embodiment 3
1. dispensing：
By 50ml acetone and 50ml ultra-pure water mix homogeneously, 0.6651 gram of lithium carbonate, 0.5457 gram of vanadic anhydride are mixed
It is distributed to after conjunction in above-mentioned mixed solvent.(volume is to be then added to the high-temperature high-pressure reaction kettle with thermometric, pressure tester
250 milliliters) in, sealing.
2. isothermal reaction is implemented using High Temperature High Pressure mixed solvent hot system：
The reactor of sealing is put in Muffle furnace, is heated to 250 DEG C (container inner pressure reaches 6MPa), it is permanent at this temperature
It is fixed 1 hour.
3. cool down：
Make reactor naturally cool to room temperature (20 DEG C～25 DEG C), reactor is taken out from Muffle furnace.
4. wash：
Product is taken out from reactor, and product is filtered by vacuum filter (aperture is 0.22 micron), solid is obtained
Precipitate；Stopped with the liquid pH=7 after solid precipitation obtained by ultra-pure water, washing with alcohol to washing.
5. dry：
The solid obtained after filtration is dried in the baking oven at a temperature of 50 DEG C～60 DEG C, lithium vanadate Li is obtained3VO4Crystallite
Powder.
X-ray diffraction result shows that it is lithium vanadate Li to test the powder for obtaining3VO4(Fig. 3 a).Scanning electron microscope is seen
Examine and show, irregularly shaped particles (Fig. 3 b) of the powder for 1～2 micron of average-size.
Embodiment 4
1. dispensing：
By 60ml acetone and 40ml ultra-pure water mix homogeneously, 0.6651 gram of lithium carbonate, 0.5457 gram of vanadic anhydride are mixed
It is distributed to after conjunction in above-mentioned mixed solvent.(volume is to be then added to the high-temperature high-pressure reaction kettle with thermometric, pressure tester
250 milliliters) in, sealing.
2. isothermal reaction is implemented using High Temperature High Pressure mixed solvent hot system：
The reactor of sealing is put in Muffle furnace, is heated to 270 DEG C (container inner pressure reaches 8MPa), it is permanent at this temperature
It is fixed 1 hour.
3. cool down：
Make reactor naturally cool to room temperature (20 DEG C～25 DEG C), reactor is taken out from Muffle furnace.
4. wash：
Product is taken out from reactor, and product is filtered by vacuum filter (aperture is 0.45 micron), solid is obtained
Precipitate；Stopped with the liquid pH=7 after solid precipitation obtained by ultra-pure water, washing with acetone to washing.
5. dry：
The solid obtained after filtration is dried in the baking oven at a temperature of 50 DEG C～60 DEG C, lithium vanadate Li is obtained3VO4Crystallite
Powder.
X-ray diffraction result shows that it is lithium vanadate Li to test the powder for obtaining3VO4(Fig. 4 a).Scanning electron microscope is seen
Examine and show, most of powder is the long 20 microns rod-shpaed particle (Fig. 4 b) of 5～10 microns of diameter.
Claims (4)
1. it is a kind of to synthesize lithium vanadate Li using High Temperature High Pressure mixed solvent hot system3VO4The method of monocrystalline micron powder, step is：
(1) dispensing：Will be used as synthesis target lithium vanadate Li3VO4In raw material components Li, V according to atomic ratio Li V=3 1 ratio
Example, is mixed in the form of solid carbonic acid lithium powder and solid vanadium pentoxide powder；
(2) prepare mixed solvent：Acetone is mixed according to the arbitrary proportion between volume ratio 19 to 91 with ultra-pure water, is obtained mixed
Bonding solvent；
(3) dispersed material：Step (1) mixed pressed powder is scattered in the mixed solvent prepared by step (2), is formed
The amount of solid-liquid suspension body, wherein mixed solvent is 50～120 times of powder material volume；
(4) implement isothermal reaction using High Temperature High Pressure mixed solvent hot system；
(5) cool down：After isothermal reaction, reaction vessel is cooled down, container inner pressure is down to normal pressure；
(6) wash：The solid in reaction vessel is separated with liquid using centrifugation or with Vacuum filtration device, with ultrapure
Solid precipitation obtained by water, ethanol or washing with acetone at least 3 times, or the liquid pH=7 after washing to washing stops；
(7) dry：Solid precipitation after step (6) is washed drying equipment is dried, and the product of acquisition is the vanadic acid of pure phase
Lithium Li3VO4Monocrystalline micron powder；
It is characterized in that：
Step (4) the utilization High Temperature High Pressure mixed solvent hot system implements the method for isothermal reaction：Step (3) is obtained
Solid-liquid suspension body is put in high-temperature high-voltage reaction container, it is closed after reaction vessel is put be heated in firing equipment 200～350
DEG C, container inner pressure be 2～9MPa, isothermal reaction 1～4 hour, now the technical characteristic of reaction system be High Temperature High Pressure mixing
Solvent thermal reaction system；Wherein, the high-temperature high-voltage reaction container is the high-temperature high-pressure reaction kettle with thermometric, pressure tester；
The firing equipment refers to one of the Muffle furnace of precise control of temperature device, resistance furnace, tube furnace, baking oven；
Step (5) reaction vessel is cooled to 20～25 DEG C, and the mode of cooling is to be cooled to heater according to setting speed
Room temperature, or directly cooling in power-off stove, or reaction vessel is directly taken out from heater natural cooling, or will reaction
Container is cooled down in being put into frozen water after taking out from heater；
The condition that step (6) centrifugation is implemented is：1000～2000 revs/min of centrifugal rotational speed, 10～20 points of centrifugation time
Clock；The Vacuum filtration device adopts aperture for 0.2～0.5 micron of filtering membrane of filter；
Step (7) drying equipment is baking oven, drying baker or infrared lamp, and drying temperature is 50～60 DEG C.
2. lithium vanadate Li is synthesized using High Temperature High Pressure mixed solvent hot system as claimed in claim 13VO4Monocrystalline micron powder
Method, is characterized in that：Step (4) heating-up temperature is 250～300 DEG C, and container inner pressure is 6～9MPa, isothermal reaction 1～
2 hours；The firing equipment refers to the Muffle furnace of precise control of temperature device.
3. lithium vanadate Li is synthesized using High Temperature High Pressure mixed solvent hot system as claimed in claim 13VO4Monocrystalline micron powder
Method, is characterized in that：The condition of step (6) centrifugation is：1500 revs/min of centrifugal rotational speed, centrifugation time 20 minutes.
4. lithium vanadate Li is synthesized using High Temperature High Pressure mixed solvent hot system as claimed in claim 13VO4Monocrystalline micron powder
Method, is characterized in that：Step (6) Vacuum filtration device adopts aperture for 0.22～0.45 micron of filtering membrane of filter.
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| CN108321373B (en) * | 2018-02-01 | 2020-07-07 | 山东大学 | Method for synthesizing lithium titanate/titanium dioxide composite nano polycrystalline powder material by utilizing high-temperature high-pressure mixed solvent thermal system |
| CN109052471B (en) * | 2018-07-12 | 2020-10-27 | 中国科学院合肥物质科学研究院 | Method for preparing lithium vanadate porous film by electrostatic spraying and application |
| CN111106335B (en) * | 2019-12-20 | 2022-05-03 | 三峡大学 | Preparation method of lithium ion battery composite negative electrode material |
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| JP3136812B2 (en) * | 1991-12-20 | 2001-02-19 | 宇部興産株式会社 | Single crystal manufacturing method |
| FR2831715B1 (en) * | 2001-10-25 | 2004-03-19 | Centre Nat Rech Scient | LITHIUM AND VANADIUM OXIDE, ITS USE AS AN ACTIVE ELECTRODE MATERIAL |
| CN102509782A (en) * | 2011-11-23 | 2012-06-20 | 陕西科技大学 | Microwave hydrothermal preparation method of positive electrode material LiV3O8 of lithium battery |
| EP2629353A1 (en) * | 2012-02-17 | 2013-08-21 | Belenos Clean Power Holding AG | Non-aqueous secondary battery having a blended cathode active material |
| CN102683665B (en) * | 2012-05-18 | 2014-05-14 | 武汉理工大学 | Lithium-vanadium oxide over-long nano wire and preparation method and application thereof |
| CN103474641A (en) * | 2013-09-25 | 2013-12-25 | 三峡大学 | Lithium ion battery anode material Li3VO4 and preparation method thereof |
| CN105133016B (en) * | 2015-10-09 | 2018-10-16 | 新疆大学 | The preparation method and purposes of lithium vanadate nonlinear optical crystal |
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