CN110380048A - Nanostructure LiNbO3/ Graphene electrodes material and preparation method thereof - Google Patents
Nanostructure LiNbO3/ Graphene electrodes material and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 60
- 229910003327 LiNbO3 Inorganic materials 0.000 title claims abstract description 52
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 32
- 239000000463 material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 claims abstract description 28
- 238000001354 calcination Methods 0.000 claims abstract description 20
- 239000007772 electrode material Substances 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims abstract description 9
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 9
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000012467 final product Substances 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 229910019804 NbCl5 Inorganic materials 0.000 claims abstract description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- 239000000047 product Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 230000005611 electricity Effects 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 239000002001 electrolyte material Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 9
- 239000000126 substance Substances 0.000 description 6
- 229910001416 lithium ion Inorganic materials 0.000 description 5
- 238000001069 Raman spectroscopy Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen(.) Chemical compound [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910002986 Li4Ti5O12 Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 229920000128 polypyrrole Polymers 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- -1 graphite Alkene Chemical class 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- GQYHUHYESMUTHG-UHFFFAOYSA-N lithium niobate Chemical compound [Li+].[O-][Nb](=O)=O GQYHUHYESMUTHG-UHFFFAOYSA-N 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000007773 negative electrode material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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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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- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
-
- 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
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- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
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- Manufacturing & Machinery (AREA)
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Abstract
The present invention relates to a kind of nanostructure LiNbO3/ Graphene electrodes material and preparation method thereof, the steps include: first to use NbCl5It as raw material, is mixed with oleyl amine, carries out hydro-thermal reaction after mixing evenly, then Nb is obtained by high-temperature heat treatment2O5Nano particle；Then by Nb2O5Nano particle and Li2CO3Mixed grinding, calcining obtains LiNbO under air3Nano particle；Finally by LiNbO3Nano particle is distributed in water, silane coupling agent is added, then mix with graphene oxide aqueous dispersions, is obtained LiNbO after being sufficiently stirred3/ graphene oxide, calcining obtains final product nanostructure LiNbO under air3/ Graphene electrodes material.High conductivity graphene and equally distributed nanostructure LiNbO3, ion and electron diffusion path can be shortened, so that electrolyte and electrode material come into full contact with, so that electrode material be made to show high-rate characteristics and cyclical stability outstanding.
Description
Technical field
The invention belongs to nanometer energy storage material preparation fields, and in particular to a kind of nanostructure LiNbO3/ Graphene electrodes
The preparation method of material.
Background technique
Lithium niobate (LiNbO3), it is a kind of very widely used photoelectric material in early days, some present research workers open
Begin to attempt LiNbO3As the electrode material of energy storage device, mainly due to LiNbO3With Li4Ti5O12With similar characteristics,
Middle Nb5+/Nb3+Redox couple has high operating voltage (1.7 V vs. Li+/ Li), it can effectively prevent SEI layers and lithium
The formation of dendrite makes energy storage device have higher safety；LiNbO3Volume change is small during charge discharge, promotees
Into the invertibity of lithium ion insertion abjection process；And LiNbO3With than Li4Ti5O12Higher theoretical capacity (363 mA h
g-1).The porous LiNbO of 3D is prepared using a kind of microwave-assisted natural law in Fan seminar3Nano material, as lithium-ion electric
The negative electrode material in pond shows high reversible capacity (Fan Q, Lei L X, Sun Y M. Facile synthesis of
a 3D-porous LiNbO3 nanocomposite as a novel electrode material for lithium
ion batteries. Nanoscale, 2014, 6(13): 7188-7192.).However, LiNbO3The electronic conductance of itself
Rate is lower, and electrochemical reaction dynamics is slower, cause its high rate performance and cyclical stability poor, a kind of to solve this problem
Effective ways are to prepare LiNbO3With the combination electrode material of conductive carbon material.A kind of CNT- is prepared in Fan seminar again
LiNbO3- PPy flexible compound electrode, the highly conductive network and porous structure being interweaved effectively increase material electronics and from
The electrochemical stability of sub- efficiency of transmission and electrode, test result shows that this combination electrode shows high capacity, excellent
Multiplying power property and cyclical stability (Fan Q, Lei L X, Yin G, et al. Self-weaving CNT-LiNbO3
nanoplate-polypyrrole hybrid as a flexible anode for Li-ion batteries.
Chemical Communications, 2014, 50(18): 2370-2373.).Graphene is current most popular conduction
Carbon material, has many advantages, such as large specific surface area, and mechanical property is strong and high conductivity, by LiNbO3With graphene is compound can be abundant
The advantage both played, obtains the electrode material of excellent electrochemical performance, but as far as we know, report currently not yet about
LiNbO3Preparation with the combination electrode material of graphene and its application in energy storage device.
Summary of the invention
It is high that the purpose of the present invention is to provide a kind of capacity, high rate performance and the excellent LiNbO of cyclical stability3/ graphite
Alkene electrode material and preparation method thereof.
In order to solve the above technical problems, the present invention provides a kind of nanostructure LiNbO3/ Graphene electrodes material, it is described
Nanostructure LiNbO3Be uniformly coated in graphene sheet layer, wherein graphene account for electrode material gross mass 5.3 ~
32.8%。
Above-mentioned nanostructure LiNbO3The preparation method of/Graphene electrodes material, comprising the following steps:
The first step, by NbCl5Ethanol solution mixed with the ethanol solution of oleyl amine, be sufficiently stirred；
First step mixed liquor is carried out hydro-thermal reaction by second step；
The separation of second step product, washing, drying are obtained Nb after being heat-treated under a nitrogen by third step2O5Nano particle；
4th step, by Nb2O5Nano particle and Li2CO3Mixed grinding, calcining obtains LiNbO under air3Nano particle；
5th step, by LiNbO3Nano particle is distributed in water, and silane coupling agent is added, is sufficiently stirred；
Mixed liquor obtained by 5th step is added in graphene oxide aqueous dispersions by the 6th step, after being sufficiently stirred, separate, wash,
It is dry, obtain LiNbO3/ graphene oxide；
7th step, by LiNbO3/ graphene oxide is calcined under air, obtains final product nanostructure LiNbO3/ graphene
Electrode material.
Preferably, in step 1, the NbCl5Mole and oleyl amine volume ratio be 5:1 ~ 2:1 (mg:mL),
Mixing time is 20 ~ 120 min.
Preferably, in step 2, the hydrothermal temperature is 120 ~ 200 °C, and the reaction time is 10 ~ 24 h.
Preferably, in step 3, the heat treatment temperature is 600 °C, and the time is 1 ~ 3 h.
Preferably, in step 4, the Nb2O5With Li2CO3Mass ratio be 1:1 ~ 1:5, calcination temperature be 500 ~ 900
°C, calcination time is 1 ~ 5 h.
Preferably, in step 5, the LiNbO3The quality of nano particle and the volume ratio of silane coupling agent be 1:5 ~
1:2 (mg:uL), mixing time are 12 ~ 30 h.
Preferably, in step 6, the concentration of the graphene oxide aqueous dispersions is 0.2 ~ 3 mg/mL, mixing time
For 1 ~ 5 h.
Preferably, LiNbO3The mass ratio of nano particle and graphene oxide is 5:1 ~ 10:1.
Preferably, in step 7, calcination temperature is 200 °C, and calcination time is 1 ~ 3 h.
Compared with prior art, the present invention the advantage is that: the graphene of (1) high conductivity is the quick transmission of electronics
Channel is provided；(2) LiNbO of nanostructure3It is evenly distributed in graphene sheet layer, shortens ion diffusion path, so that electrolysis
Liquid and electrode material come into full contact with；(3) graphene and LiNbO3Between synergistic effect effectively improve the electrochemistry of composite material
Performance；(4) nanostructure LiNbO prepared by the present invention3/ Graphene electrodes material and single LiNbO3It compares, shows more
More capacity are (in 0.05 A g-1, discharge capacity is 165 mA h g-1), higher multiplying power property is (in 5 A g-1, discharge capacity
For 68 mA h g-1) and superior cyclical stability.
Present invention is further described in detail with reference to the accompanying drawing.
Detailed description of the invention
Fig. 1 is nanostructure LiNbO of the present invention3The preparation flow schematic diagram of/Graphene electrodes material.
Fig. 2 is nanostructure LiNbO prepared by present example one3The TEM of/Graphene electrodes material schemes.
Fig. 3 is nanostructure LiNbO prepared by present example one3The XRD diagram (a) and Raman of/Graphene electrodes material
Scheme (b).
Fig. 4 is nanostructure LiNbO prepared by present example one3The chemical property figure of/Graphene electrodes material,
Wherein LiNbO3@rGO is LiNbO3/ Graphene electrodes material, LiNbO3It is single LiNbO3Electrode material.
Fig. 5 is present example two (a), the nanostructure LiNbO of example three (b) and example four (c) preparation3/ graphene
The chemical property figure of electrode material.
Specific embodiment
The invention will be further described for following embodiment, but the contents of the present invention are not limited by this embodiment.
Nanostructure LiNbO in following examples3The preparation process of/Graphene electrodes material is as shown in Fig. 1.
Embodiment one:
The first step, the NbCl of 0.4 mmol5It is dissolved in ethyl alcohol, then mixes, is sufficiently stirred with the oleyl amine ethanol solution of 5 uL/mL
30 min；
Second step moves to first step mixed liquor in water heating kettle, in 180 °C of 14 h of reaction；
Third step, by the separation of second step product, washing, drying, 600 °C of 2 h of heat treatment obtain Nb under a nitrogen2O5Nanometer
Grain；
4th step, by third step product Nb2O5Nano particle and Li2CO3Mixed grinding, the two mass ratio are 1:5, under air
500 °C of 3 h of calcining obtain LiNbO3Nano particle；
5th step, by the 4th step product LiNbO325 mg of nano particle is distributed in water, and 100 uL silane coupling agents are added, fill
Divide stirring 24 h；
Above-mentioned mixed liquor is added in the graphene oxide aqueous dispersions of 0.5 mg/mL by the 6th step, after 2 h are sufficiently stirred, point
From, washing, dry, LiNbO is obtained3/ graphene oxide；
7th step, by above-mentioned product, 200 °C of 2 h of calcining obtain final product nanostructure LiNbO under air3/ graphene electricity
Pole material.
Fig. 2 is the TEM figure of the electrode material, it can be seen that the LiNbO of nanostructure3It is evenly distributed in graphene sheet layer
In.Moreover, the XRD diagram (a) of Fig. 3 and Raman map (b) obviously show LiNbO3XRD and Raman characteristic peak, Yi Jishi
The Raman characteristic peak of black alkene, it was demonstrated that LiNbO is successfully prepared in we3/ graphene combination electrode material.Fig. 4 is the electrode
The electrochemical property test of material is as a result, with single LiNbO3It compares, nanostructure LiNbO3The conduct of/graphene composite material
Electrode material shows higher capacity, preferable high rate performance and cyclical stability.
Embodiment two:
The first step, the NbCl of 0.1 mmol5It is dissolved in ethyl alcohol, then mixes, is sufficiently stirred with the oleyl amine ethanol solution of 1 uL/mL
20 min；
Second step moves to first step mixed liquor in water heating kettle, in 150 °C of 20 h of reaction；
Third step, by the separation of second step product, washing, drying, 600 °C of 1 h of heat treatment obtain Nb under a nitrogen2O5Nanometer
Grain；
4th step, by third step product Nb2O5Nano particle and Li2CO3Mixed grinding, the two mass ratio are 1:4, under air
600 °C of 5 h of calcining obtain LiNbO3Nano particle；
5th step, by the 4th step product LiNbO320 mg of nano particle is distributed in water, 50 uL silane coupling agents is added, sufficiently
Stir 12 h；
Above-mentioned mixed liquor is added in the graphene oxide aqueous dispersions of 0.2 mg/mL by the 6th step, after 1 h is sufficiently stirred, point
From, washing, dry, LiNbO is obtained3/ graphene oxide；
7th step, by above-mentioned product, 200 °C of 2.5 h of calcining obtain final product nanostructure LiNbO under air3/ graphene
Electrode material.
The nanostructure LiNbO that embodiment two obtains3The chemical property of/Graphene electrodes material such as Fig. 5 a.
Embodiment three:
The first step, the NbCl of 0.6 mmol5It is dissolved in ethyl alcohol, then mixes, is sufficiently stirred with the oleyl amine ethanol solution of 10 uL/mL
90 min；
Second step moves to first step mixed liquor in water heating kettle, in 120 °C of 24 h of reaction；
Third step, by the separation of second step product, washing, drying, 600 °C of 3 h of heat treatment obtain Nb under a nitrogen2O5Nanometer
Grain；
4th step, by third step product Nb2O5Nano particle and Li2CO3Mixed grinding, the two mass ratio are 1:2, under air
800 °C of 2 h of calcining obtain LiNbO3Nano particle；
5th step, by the 4th step product LiNbO3100 mg of nano particle is distributed in water, and 200 uL silane coupling agents are added, fill
Divide stirring 28 h；
Above-mentioned mixed liquor is added in the graphene oxide aqueous dispersions of 3 mg/mL by the 6th step, after 5 h are sufficiently stirred, point
From, washing, dry, LiNbO is obtained3/ graphene oxide；
7th step, by above-mentioned product, 200 °C of 1 h of calcining obtain final product nanostructure LiNbO under air3/ graphene electricity
Pole material.
The nanostructure LiNbO that embodiment three obtains3The chemical property of/Graphene electrodes material such as Fig. 5 b.
Example IV:
The first step, the NbCl of 0.8 mmol5It is dissolved in ethyl alcohol, then mixes, is sufficiently stirred with the oleyl amine ethanol solution of 20 uL/mL
120 min；
Second step moves to first step mixed liquor in water heating kettle, in 200 °C of 10 h of reaction；
Third step, by the separation of second step product, washing, drying, 600 °C of 1.5 h of heat treatment obtain Nb under a nitrogen2O5Nanometer
Particle；
4th step, by third step product Nb2O5Nano particle and Li2CO3Mixed grinding, the two mass ratio are 1:1, under air
900 °C of 1 h of calcining obtain LiNbO3Nano particle；
5th step, by the 4th step product LiNbO360 mg of nano particle is distributed in water, and 300 uL silane coupling agents are added, fill
Divide stirring 30 h；
Above-mentioned mixed liquor is added in the graphene oxide aqueous dispersions of 1 mg/mL by the 6th step, after 4 h are sufficiently stirred, point
From, washing, dry, LiNbO is obtained3/ graphene oxide；
7th step, by above-mentioned product, 200 °C of 3 h of calcining obtain final product nanostructure LiNbO under air3/ graphene electricity
Pole material.
The nanostructure LiNbO that example IV obtains3The chemical property of/Graphene electrodes material such as Fig. 5 c.
Claims (10)
1. a kind of nanostructure LiNbO3/ Graphene electrodes material, which is characterized in that the nanostructure LiNbO3Equably
It is coated in graphene sheet layer, wherein graphene accounts for the 5.3 ~ 32.8% of electrode material gross mass.
2. nanostructure LiNbO3The preparation method of/Graphene electrodes material, which comprises the following steps:
The first step, by NbCl5Ethanol solution mixed with the ethanol solution of oleyl amine, be sufficiently stirred；
First step mixed liquor is carried out hydro-thermal reaction by second step；
The separation of second step product, washing, drying are obtained Nb after being heat-treated under a nitrogen by third step2O5Nano particle；
4th step, by Nb2O5Nano particle and Li2CO3Mixed grinding, calcining obtains LiNbO under air3Nano particle；
5th step, by LiNbO3Nano particle is distributed in water, and silane coupling agent is added, is sufficiently stirred；
Mixed liquor obtained by 5th step is added in graphene oxide aqueous dispersions by the 6th step, after being sufficiently stirred, separate, wash,
It is dry, obtain LiNbO3/ graphene oxide；
7th step, by LiNbO3/ graphene oxide is calcined under air, obtains final product nanostructure LiNbO3/ graphene electricity
Pole material.
3. method according to claim 2, which is characterized in that in step 1, the NbCl5Mole and oleyl amine body
For product than being 5:1 ~ 2:1 (mg:mL), mixing time is 20 ~ 120 min.
4. method according to claim 2, which is characterized in that in step 2, the hydrothermal temperature is 120 ~ 200
°C, the reaction time is 10 ~ 24 h.
5. method according to claim 2, which is characterized in that in step 3, the heat treatment temperature is 600 °C, when
Between be 1 ~ 3 h.
6. method according to claim 2, which is characterized in that in step 4, the Nb2O5With Li2CO3Mass ratio be
1:1 ~ 1:5, calcination temperature are 500 ~ 900 °C, and calcination time is 1 ~ 5 h.
7. method according to claim 2, which is characterized in that in step 5, the LiNbO3The quality of nano particle with
The volume ratio of silane coupling agent is 1:5 ~ 1:2 (mg:uL), and mixing time is 12 ~ 30 h.
8. method according to claim 2, which is characterized in that in step 6, the graphene oxide aqueous dispersions it is dense
Degree is 0.2 ~ 3 mg/mL, and mixing time is 1 ~ 5 h.
9. method according to claim 2, which is characterized in that LiNbO3The mass ratio of nano particle and graphene oxide is 5:1
~10:1。
10. method according to claim 2, which is characterized in that in step 7, calcination temperature is 200 °C, and calcination time is
1~3 h。
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| CN116314603A (en) * | 2023-05-25 | 2023-06-23 | 宁德新能源科技有限公司 | Negative electrode plate, electrochemical device and electronic device |
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|---|---|---|---|---|
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