CN106684376A - Method for preparing zinc ferrite nanosheet assembled hollow microsphere by utilizing hydrothermal and calcination methods, and application - Google Patents
Method for preparing zinc ferrite nanosheet assembled hollow microsphere by utilizing hydrothermal and calcination methods, and application Download PDFInfo
- Publication number
- CN106684376A CN106684376A CN201611237945.0A CN201611237945A CN106684376A CN 106684376 A CN106684376 A CN 106684376A CN 201611237945 A CN201611237945 A CN 201611237945A CN 106684376 A CN106684376 A CN 106684376A
- Authority
- CN
- China
- Prior art keywords
- nanometer sheet
- zinc ferrite
- micron ball
- zinc
- isopropanol
- 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.)
- Pending
Links
Classifications
-
- 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
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Compounds Of Iron (AREA)
Abstract
The invention relates to a method for preparing a zinc ferrite nanosheet assembled hollow microsphere by utilizing hydrothermal and calcination methods, and application, and relates to a preparation method and application of a hollow microsphere. The invention aims to solve the problems that the specific capacity of an electrode material is severely attenuated and the cyclic stability is decreased due to the fact that the electrode material is powdered when the existing zinc ferrite electrode material generates enormous volume expansion and shrinkage in a Li<+> embedding and releasing process. The preparation method comprises the following steps of: (1), preparing a propyl alcohol iron and propyl alcohol zinc nanosheet assembled solid microsphere precursor by using a hydrothermal method; and (2), preparing the zinc ferrite nanosheet assembled hollow microsphere by using a calcination method. The first discharge capacity of a lithium ion battery prepared by taking the zinc ferrite nanosheet assembled hollow microsphere prepared by the invention as the anode material of the lithium ion battery can be up to 2295.6 mAh/g; and the first charge capacity of the lithium ion battery can be up to 1179.7 mAh/g. The method disclosed by the invention is suitable for preparing the zinc ferrite nanosheet assembled hollow microsphere.
Description
Technical field
The present invention relates to a kind of preparation method and application of hollow micron ball.
Background technology
At present, zinc ferrite electrode material, is a kind of lithium ion battery negative material of great application prospect, because of itself and tradition
Negative material compare, possess more excellent chemical property, and its preparation process is simple, possess specific surface area higher, can
To provide more embedding lithium positions.However, in Li+During embedded and abjection, they can produce huge volumetric expansion and receipts
Contracting, causes electrode material powdered, so as to the special capacity fade of material can be caused acutely, stable circulation performance declines.Made
It is standby into hollow-core construction be a kind of more effective and simple method.Because hollow-core construction can provide larger specific surface area and interior
Chamber free space, is conducive to infiltration, the Li of electrolyte+Diffusion and Volume Changes alleviation, and and then improve material circulation
Energy.The present invention mainly uses simple and effective hydro-thermal and zinc ferrite nanometer sheet obtained in calcination method to assemble hollow micron ball, due to
Its preparation method is simple, green, with low cost, possesses specific surface area higher than traditional material, it is adaptable to industrialized production, makees
For lithium ion battery negative material when, possess high power charging-discharging characteristic and cyclical stability.
The content of the invention
The invention aims to solve existing zinc ferrite electrode material in Li+During embedded and abjection, produce huge
Volumetric expansion and contraction, cause electrode material powdered, so as to the special capacity fade of electrode material can be caused acutely, circulation is steady
Determine the problem of hydraulic performance decline, and provide a kind of utilization hydro-thermal and calcination method prepares the side that zinc ferrite nanometer sheet assembles hollow micron ball
Method and application.
A kind of utilization hydro-thermal and calcination method prepare the method that zinc ferrite nanometer sheet assembles hollow micron ball, specifically by following
What step was completed：
First, zinc acetate, nine water ferric nitrates, isopropanol and glycerine are well mixed, in transferring to hydrothermal reaction kettle, then
Hydro-thermal reaction 10h~14h at being 170 DEG C~190 DEG C in temperature, obtains the solid micron of propyl alcohol iron and the assembling of propanol zinc nanometer sheet
Ball presoma；
The quality of the zinc acetate described in step one is (0.1g~0.3g) with the volume ratio of isopropanol:30mL；
The quality of nine water ferric nitrates described in step one is (0.3g~0.6g) with the volume ratio of isopropanol:30mL；
Glycerine and the volume ratio of isopropanol described in step one are (5~10):30；
2nd, in air atmosphere, the solid micron ball presoma for propyl alcohol iron and propanol zinc nanometer sheet being assembled is with 1 DEG C/min
The heating rate of~4 DEG C/min is warming up to 380 DEG C~420 DEG C, then is calcined in the case where air atmosphere and temperature are for 380 DEG C~420 DEG C
1h~3h, obtains zinc ferrite nanometer sheet and assembles hollow micron ball.
Principle of the invention：
Zn2++Fe3++C3H8O3→Zn3(C3H5O3)2+FeC3H5O3+H2；
Zn3(C3H5O3)2+FeC3H5O3→ZnFe2O4+CO2+H2O。
Advantages of the present invention：
First, the present invention prepares zinc ferrite nanometer sheet and assembles hollow micron ball, the raw material vinegar for using using hydro-thermal and calcination method
Sour zinc, nine water ferric nitrates, isopropanol and glycerine abundance, and whole experiment process is simple to operate, with low cost, product is gathered around
There are high power charging-discharging characteristic and cyclical stability, can be used as commercial Li-ion battery negative material；
2nd, hollow micron ball is assembled using zinc ferrite nanometer sheet prepared by the present invention to be prepared as lithium ion battery negative material
The discharge capacity first of lithium ion battery can reach more than 2295.6mAh/g, initial charge capacity be 1179.7mAh/g with
On, discharge capacity keeps more than 640mAh/g after 100 times circulate.
The present invention assembles hollow micron ball suitable for preparing zinc ferrite nanometer sheet.
Brief description of the drawings
The solid micron ball presoma that Fig. 1 is assembled for the propyl alcohol iron and propanol zinc nanometer sheet that are obtained in the step one of embodiment one
SEM figure；
Fig. 2 assembles the SEM figures of hollow micron ball for the zinc ferrite nanometer sheet obtained in the step 2 of embodiment one；
Fig. 3 is XRD, and 1 is ZnFe in Fig. 32O4Standard x RD curves, 2 is the ferrous acid that obtains in the step 2 of embodiment one
Zinc nanometer sheet assembles the XRD curves of hollow micron ball；
Fig. 4 is that the zinc ferrite nanometer sheet obtained using in the step 2 of embodiment one assembles hollow micron ball as lithium ion battery
First three the circle charging and discharging curve figure of lithium ion battery prepared by negative material under the conditions of current density 100mA/g；1 is in Fig. 4
First lap charging and discharging curve, 2 is the second circle charging and discharging curve, and 3 is the 3rd circle charging and discharging curve；
Fig. 5 is that the zinc ferrite nanometer sheet obtained using in the step 2 of embodiment one assembles hollow micron ball as lithium ion battery
The lithium electricity cycle performance figure of lithium ion battery prepared by negative material under the conditions of current density 100mA/g, 1 to charge in Fig. 5,
2 is electric discharge；
Fig. 6 is that the zinc ferrite nanometer sheet obtained using in the step 2 of embodiment one assembles hollow micron ball as lithium ion battery
The lithium electricity high rate performance figure of lithium ion battery prepared by negative material under different current densities；A is current density difference in Fig. 6
It is the high rate performance curve under 100mA/g, B is respectively the high rate performance curve under 200mA/g for current density, and C is that electric current is close
Degree is respectively the high rate performance curve under 400mA/g, and D is respectively the high rate performance curve under 800mA/g for current density, and E is
Current density is respectively the high rate performance curve under 1600mA/g.
Specific embodiment
Specific embodiment one：Present embodiment is a kind of using hydro-thermal and calcination method to prepare the assembling of zinc ferrite nanometer sheet
The method of empty micron ball, is specifically realized by the following steps：
First, zinc acetate, nine water ferric nitrates, isopropanol and glycerine are well mixed, in transferring to hydrothermal reaction kettle, then
Hydro-thermal reaction 10h~14h at being 170 DEG C~190 DEG C in temperature, obtains the solid micron of propyl alcohol iron and the assembling of propanol zinc nanometer sheet
Ball presoma；
The quality of the zinc acetate described in step one is (0.1g~0.3g) with the volume ratio of isopropanol:30mL；
The quality of nine water ferric nitrates described in step one is (0.3g~0.6g) with the volume ratio of isopropanol:30mL；
Glycerine and the volume ratio of isopropanol described in step one are (5~10):30；
2nd, in air atmosphere, the solid micron ball presoma for propyl alcohol iron and propanol zinc nanometer sheet being assembled is with 1 DEG C/min
The heating rate of~4 DEG C/min is warming up to 380 DEG C~420 DEG C, then is calcined in the case where air atmosphere and temperature are for 380 DEG C~420 DEG C
1h~3h, obtains zinc ferrite nanometer sheet and assembles hollow micron ball.
The principle of present embodiment：
Zn2++Fe3++C3H8O3→Zn3(C3H5O3)2+FeC3H5O3+H2；
Zn3(C3H5O3)2+FeC3H5O3→ZnFe2O4+CO2+H2O。
The advantage of present embodiment：
First, present embodiment prepares zinc ferrite nanometer sheet and assembles hollow micron ball, the original for using using hydro-thermal and calcination method
Material zinc acetate, nine water ferric nitrates, isopropanol and glycerine abundance, and whole experiment process is simple to operate, it is with low cost, produce
Thing possesses high power charging-discharging characteristic and cyclical stability, can be used as commercial Li-ion battery negative material；
2nd, hollow micron ball as lithium ion battery negative material is assembled using zinc ferrite nanometer sheet prepared by present embodiment
The discharge capacity first of the lithium ion battery of preparation can reach more than 2295.6mAh/g, and initial charge capacity is 1179.7mAh/g
More than, discharge capacity keeps more than 640mAh/g after 100 times circulate.
Present embodiment assembles hollow micron ball suitable for preparing zinc ferrite nanometer sheet.
Specific embodiment two：Present embodiment is with the difference of specific embodiment one：By zinc acetate, nine in step one
Water ferric nitrate, isopropanol and glycerine are well mixed, and hydro-thermal is anti-in transferring to hydrothermal reaction kettle, then at being 180 DEG C in temperature
12h is answered, the solid micron ball presoma of propyl alcohol iron and the assembling of propanol zinc nanometer sheet is obtained.Other steps and specific embodiment one
It is identical.
Specific embodiment three：One of present embodiment and specific embodiment one or two difference is：Institute in step one
The quality of the zinc acetate stated is (0.1g~0.2g) with the volume ratio of isopropanol:30mL.Other steps and specific embodiment one
Or two is identical.
Specific embodiment four：One of present embodiment and specific embodiment one to three difference is：Institute in step one
The quality of the zinc acetate stated is (0.2g~0.3g) with the volume ratio of isopropanol:30mL.Other steps and specific embodiment one
It is identical to three.
Specific embodiment five：One of present embodiment and specific embodiment one to four difference is：Institute in step one
The quality of the nine water ferric nitrates stated is (0.3g~0.45g) with the volume ratio of isopropanol:30mL.Other steps and specific embodiment party
Formula one to four is identical.
Specific embodiment six：One of present embodiment and specific embodiment one to five difference is：Institute in step one
The quality of the nine water ferric nitrates stated is (0.45g~0.6g) with the volume ratio of isopropanol:30mL.Other steps and specific embodiment party
Formula one to five is identical.
Specific embodiment seven：One of present embodiment and specific embodiment one to six difference is：Institute in step one
The glycerine stated is (5~8) with the volume ratio of isopropanol:30.Other steps are identical with specific embodiment one to six.
Specific embodiment eight：One of present embodiment and specific embodiment one to seven difference is：Institute in step one
The glycerine stated is (8~10) with the volume ratio of isopropanol:30.Other steps are identical with specific embodiment one to seven.
Specific embodiment nine：One of present embodiment and specific embodiment one to eight difference is：In step 2
Under air atmosphere, the intensification of 1 DEG C/min~2 DEG C of solid micron ball presoma/min that propyl alcohol iron and propanol zinc nanometer sheet are assembled
Speed is warming up to 380 DEG C~400 DEG C, then calcines 1h~2h in the case where air atmosphere and temperature are for 380 DEG C~400 DEG C, obtains ferrous acid
Zinc nanometer sheet assembles hollow micron ball.Other steps are identical with specific embodiment one to eight.
Specific embodiment ten：Present embodiment is that the zinc ferrite nanometer sheet hollow micron ball of assembling is negative as lithium ion battery
Pole materials application.
Embodiment one：A kind of utilization hydro-thermal and calcination method prepare the method that zinc ferrite nanometer sheet assembles hollow micron ball, tool
Body is completed according to the following steps：
First, 0.109g zinc acetates, the water ferric nitrates of 0.404g nine, 30mL isopropanols and 8mL glycerine are well mixed, then are turned
In moving to 40mL hydrothermal reaction kettles, then hydro-thermal reaction 12h at being 180 DEG C in temperature, obtain propyl alcohol iron and propanol zinc nanometer sheet group
The solid micron ball presoma of dress；
2nd, in air atmosphere, zinc ferrite nanometer sheet is assembled into hollow micron ball presoma with the heating rate of 2 DEG C/min
400 DEG C are warming up to, then 2h is calcined in the case where air atmosphere and temperature are for 400 DEG C, obtained zinc ferrite nanometer sheet and assemble hollow micron ball.
The solid micron ball presoma that Fig. 1 is assembled for the propyl alcohol iron and propanol zinc nanometer sheet that are obtained in the step one of embodiment one
SEM figure；
From fig. 1, it can be seen that water-heat process resulting materials are the solid spherical assembled with nanometer sheet, size is 1 μm~1.5
μm。
Fig. 2 assembles the SEM figures of hollow micron ball for the zinc ferrite nanometer sheet obtained in the step 2 of embodiment one；
As can be seen from Figure 2, after calcining, material is still assembled by nanometer sheet and formed, but solid sphere has been converted to hollow ball,
Size is at 1 μm~1.5 μm.
Fig. 3 is XRD, and 1 is ZnFe in Fig. 32O4Standard x RD curves, 2 is the ferrous acid that obtains in the step 2 of embodiment one
Zinc nanometer sheet assembles the XRD curves of hollow micron ball；
As can be seen from Figure 3, ZnFe2O4At 2 θ=29.9 °, 35.3 °, 36.9 °, 42.8 °, 53.1 °, 56.6 ° and 62.2 °,
There is the diffraction maximum corresponding with standard card PDF#22-1012, it was demonstrated that it is the ZnFe of spinel structure2O4。
Hollow micron ball is assembled using zinc ferrite nanometer sheet prepared by embodiment one to be prepared as lithium ion battery negative material
Lithium ion battery manufacturing process it is as follows：
(1) the zinc ferrite nanometer sheet for, obtaining the step 2 of embodiment one assembles hollow micron ball, acetylene black and polytetrafluoroethyl-ne
Dilute emulsion is 80 according to mass ratio:10:10 mixing, obtain mixture I；To METHYLPYRROLIDONE is added dropwise in mixture I,
Obtain mixture II；Solid concentration is 60% in described polytetrafluoroethyl-ne dilute emulsion；The quality of described mixture I and N- first
The volume ratio of base -2-Pyrrolidone is 0.25g:1mL；
(2), mixture II is uniformly coated on the foam mirror weighed of a diameter of 14mm, pole piece is obtained；Exist again
Temperature is 80 DEG C of vacuum drying 10h, is re-weighed, and ZnFe in the pole piece is obtained using difference assay2O4Quality；
(3), dry pole piece is transferred in vacuum glove box the assembling for completing button cell, wherein, polypropylene high score
Sub- film is battery diaphragm, and lithium piece is counter electrode of battery, electrolyte be ethylene carbonate, dimethyl carbonate, methyl ethyl carbonate and
The LiPF of 1mol/L6Solution is according to 1:1:1:1 mixes；Pad is the stainless steel substrates of 16.2mm × 1mm (diameter × thickness)；
By dry pole piece, pad, electrolyte, barrier film, button cell that CR2025 is assembled into electrode and battery case in glove box
Afterwards, button cell is sealed using sealing machine, the button cell of preparation is finally stood into 12h at normal temperatures, obtain battery
To activation, the electrical property of material gives full play to, that is, the zinc ferrite nanometer sheet for obtaining being prepared with embodiment one assembles hollow micron ball
As lithium ion battery prepared by lithium ion battery negative material.
In current density 100mA/g, under conditions of charging/discharging voltage scope is 0-3V, to the ferrous acid prepared with embodiment one
Zinc nanometer sheet assembles hollow micron ball and carries out charge-discharge performance survey as lithium ion battery prepared by lithium ion battery negative material
Examination, as shown in Figure 4 and Figure 5；
Fig. 4 is that the zinc ferrite nanometer sheet obtained using in the step 2 of embodiment one assembles hollow micron ball as lithium ion battery
First three the circle charging and discharging curve figure of lithium ion battery prepared by negative material under the conditions of current density 100mA/g；1 is in Fig. 4
First lap charging and discharging curve, 2 is the second circle charging and discharging curve, and 3 is the 3rd circle charging and discharging curve；
As can be seen from Figure 4, using the zinc ferrite nanometer sheet that obtains in the step 2 of embodiment one assemble hollow micron ball as lithium from
After 100 times circulate, its capacity is up to 640mAh/g to lithium ion battery prepared by sub- cell negative electrode material.
Fig. 5 is that the zinc ferrite nanometer sheet obtained using in the step 2 of embodiment one assembles hollow micron ball as lithium ion battery
The lithium electricity cycle performance figure of lithium ion battery prepared by negative material under the conditions of current density 100mA/g, 1 to charge in Fig. 5,
2 is electric discharge；
As can be seen from Figure 5, using the zinc ferrite nanometer sheet that obtains in the step 2 of embodiment one assemble hollow micron ball as lithium from
Lithium ion battery prepared by sub- cell negative electrode material has excellent cycle performance.
Fig. 6 is that the zinc ferrite nanometer sheet obtained using in the step 2 of embodiment one assembles hollow micron ball as lithium ion battery
The lithium electricity high rate performance figure of lithium ion battery prepared by negative material under different current densities；A is current density difference in Fig. 6
It is the high rate performance curve under 100mA/g, B is respectively the high rate performance curve under 200mA/g for current density, and C is that electric current is close
Degree is respectively the high rate performance curve under 400mA/g, and D is respectively the high rate performance curve under 800mA/g for current density, and E is
Current density is respectively the high rate performance curve under 1600mA/g.
As can be seen from Figure 6, using the zinc ferrite nanometer sheet that obtains in the step 2 of embodiment one assemble hollow micron ball as lithium from
Lithium ion battery prepared by sub- cell negative electrode material has excellent high rate performance.
Claims (10)
1. a kind of utilization hydro-thermal and calcination method prepare the method that zinc ferrite nanometer sheet assembles hollow micron ball, it is characterised in that the party
What method was specifically realized by the following steps：
First, zinc acetate, nine water ferric nitrates, isopropanol and glycerine are well mixed, in transferring to hydrothermal reaction kettle, then in temperature
It is hydro-thermal reaction 10h~14h at 170 DEG C~190 DEG C to spend, before obtaining the solid micron ball of propyl alcohol iron and the assembling of propanol zinc nanometer sheet
Drive body；
The quality of the zinc acetate described in step one is (0.1g~0.3g) with the volume ratio of isopropanol:30mL；
The quality of nine water ferric nitrates described in step one is (0.3g~0.6g) with the volume ratio of isopropanol:30mL；
Glycerine and the volume ratio of isopropanol described in step one are (5~10):30；
2nd, in air atmosphere, the solid micron ball presoma for propyl alcohol iron and propanol zinc nanometer sheet being assembled is with 1 DEG C/min~4
DEG C/heating rate of min is warming up to 380 DEG C~420 DEG C, then calcine at being 380 DEG C~420 DEG C in air atmosphere and temperature 1h~
3h, obtains zinc ferrite nanometer sheet and assembles hollow micron ball.
2. a kind of utilization hydro-thermal according to claim 1 and calcination method prepare zinc ferrite nanometer sheet and assemble hollow micron ball
Method, it is characterised in that zinc acetate, nine water ferric nitrates, isopropanol and glycerine are well mixed in step one, transfer to water
In thermal response kettle, then temperature be 180 DEG C at hydro-thermal reaction 12h, obtain propyl alcohol iron and propanol zinc nanometer sheet assembling it is solid micro-
Rice ball presoma.
3. a kind of utilization hydro-thermal according to claim 1 and calcination method prepare zinc ferrite nanometer sheet and assemble hollow micron ball
Method, it is characterised in that the quality of the zinc acetate described in step one is (0.1g~0.2g) with the volume ratio of isopropanol:30mL.
4. a kind of utilization hydro-thermal according to claim 1 and calcination method prepare zinc ferrite nanometer sheet and assemble hollow micron ball
Method, it is characterised in that the quality of the zinc acetate described in step one is (0.2g~0.3g) with the volume ratio of isopropanol:30mL.
5. a kind of utilization hydro-thermal according to claim 1 and calcination method prepare zinc ferrite nanometer sheet and assemble hollow micron ball
Method, it is characterised in that the quality of nine water ferric nitrates described in step one is (0.3g~0.45g) with the volume ratio of isopropanol:
30mL。
6. a kind of utilization hydro-thermal according to claim 1 and calcination method prepare zinc ferrite nanometer sheet and assemble hollow micron ball
Method, it is characterised in that the quality of nine water ferric nitrates described in step one is (0.45g~0.6g) with the volume ratio of isopropanol:
30mL。
7. a kind of utilization hydro-thermal according to claim 1 and calcination method prepare zinc ferrite nanometer sheet and assemble hollow micron ball
Method, it is characterised in that glycerine and the volume ratio of isopropanol described in step one are (5~8):30.
8. a kind of utilization hydro-thermal according to claim 1 and calcination method prepare zinc ferrite nanometer sheet and assemble hollow micron ball
Method, it is characterised in that glycerine and the volume ratio of isopropanol described in step one are (8~10):30.
9. a kind of utilization hydro-thermal according to claim 1 and calcination method prepare zinc ferrite nanometer sheet and assemble hollow micron ball
Method, it is characterised in that in step 2 in air atmosphere, before the solid micron ball that propyl alcohol iron and propanol zinc nanometer sheet are assembled
The heating rate for driving body 1 DEG C/min~2 DEG C/min is warming up to 380 DEG C~400 DEG C, then air atmosphere and temperature be 380 DEG C~
1h~2h is calcined at 400 DEG C, zinc ferrite nanometer sheet is obtained and is assembled hollow micron ball.
10. it is as claimed in claim 1 to prepare the method that zinc ferrite nanometer sheet assembles hollow micron ball using hydro-thermal and calcination method
The zinc ferrite nanometer sheet of preparation assembles the application of hollow micron ball, it is characterised in that zinc ferrite nanometer sheet assembles hollow micron ball and makees
It is lithium ion battery negative material application.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611237945.0A CN106684376A (en) | 2016-12-28 | 2016-12-28 | Method for preparing zinc ferrite nanosheet assembled hollow microsphere by utilizing hydrothermal and calcination methods, and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611237945.0A CN106684376A (en) | 2016-12-28 | 2016-12-28 | Method for preparing zinc ferrite nanosheet assembled hollow microsphere by utilizing hydrothermal and calcination methods, and application |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106684376A true CN106684376A (en) | 2017-05-17 |
Family
ID=58872046
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611237945.0A Pending CN106684376A (en) | 2016-12-28 | 2016-12-28 | Method for preparing zinc ferrite nanosheet assembled hollow microsphere by utilizing hydrothermal and calcination methods, and application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106684376A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453774A (en) * | 2020-04-08 | 2020-07-28 | 安徽乐橙信息科技有限公司 | Preparation method, product and application of zinc ferrite nano flower-shaped negative electrode material |
| CN111484084A (en) * | 2020-04-02 | 2020-08-04 | 扬州大学 | Acetone gas-sensitive material and preparation method thereof |
| CN111675243A (en) * | 2020-06-11 | 2020-09-18 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method, product and application of zinc ferrite nanosheet negative electrode material |
| CN113135586A (en) * | 2021-04-21 | 2021-07-20 | 内蒙古大学 | Zinc oxide micron ball, electrode and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104569080A (en) * | 2015-01-30 | 2015-04-29 | 吉林大学 | Acetone gas sensor based on hollow spherical ZnFe2O4 nano material and preparation method thereof |
| CN105161701A (en) * | 2015-09-23 | 2015-12-16 | 西北工业大学 | Preparing method for polyaniline/hollow ZnFe2O4 composite negative electrode materials of lithium battery |
| CN106025271A (en) * | 2016-05-31 | 2016-10-12 | 山东玉皇新能源科技有限公司 | Preparation method of negative electrode material zinc ferrite |
-
2016
- 2016-12-28 CN CN201611237945.0A patent/CN106684376A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104569080A (en) * | 2015-01-30 | 2015-04-29 | 吉林大学 | Acetone gas sensor based on hollow spherical ZnFe2O4 nano material and preparation method thereof |
| CN105161701A (en) * | 2015-09-23 | 2015-12-16 | 西北工业大学 | Preparing method for polyaniline/hollow ZnFe2O4 composite negative electrode materials of lithium battery |
| CN106025271A (en) * | 2016-05-31 | 2016-10-12 | 山东玉皇新能源科技有限公司 | Preparation method of negative electrode material zinc ferrite |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111484084A (en) * | 2020-04-02 | 2020-08-04 | 扬州大学 | Acetone gas-sensitive material and preparation method thereof |
| CN111453774A (en) * | 2020-04-08 | 2020-07-28 | 安徽乐橙信息科技有限公司 | Preparation method, product and application of zinc ferrite nano flower-shaped negative electrode material |
| CN111675243A (en) * | 2020-06-11 | 2020-09-18 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method, product and application of zinc ferrite nanosheet negative electrode material |
| CN111675243B (en) * | 2020-06-11 | 2022-11-01 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of zinc ferrite nanosheet negative electrode material, product and application |
| CN113135586A (en) * | 2021-04-21 | 2021-07-20 | 内蒙古大学 | Zinc oxide micron ball, electrode and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105958042B (en) | A kind of fabricated in situ Li2MnO3The anode material for lithium-ion batteries and its synthetic method of coating modification | |
| CN105355880B (en) | A kind of LiFePO4/ C is modified the preparation method of tertiary cathode material | |
| CN103247777B (en) | Cobaltosic oxide multi-shell hollow sphere cathode material for lithium ion battery and preparation method thereof | |
| CN105470455A (en) | Modified lithium ion battery positive electrode material and preparation method therefor | |
| CN104466102B (en) | A kind of porous V2O5/C complex microspheres of positive electrode material of lithium secondary cell and preparation method thereof | |
| CN104409685B (en) | A kind of method for preparing the anode material for lithium-ion batteries with core shell structure | |
| CN106684376A (en) | Method for preparing zinc ferrite nanosheet assembled hollow microsphere by utilizing hydrothermal and calcination methods, and application | |
| CN105552369B (en) | The method for preparing three-dimensional porous niobic acid titanium oxide using template and its application in lithium ion battery | |
| CN108039472A (en) | A kind of preparation method and application of the hollow micron cube composite material of carbon coating zinc metastannate | |
| CN103151528A (en) | Method for preparing aluminum-doped zinc oxide coated lithium-ion battery positive-pole material | |
| CN105098158B (en) | A kind of lithium-enriched cathodic material of lithium ion battery of zirconium doping and preparation method thereof | |
| CN104852028A (en) | Lithium titanate/graphene composite cathode material for lithium ion battery | |
| CN104953124A (en) | Binder of silicon-carbide negative electrode material, negative electrode plate of silicon-carbide battery, manufacturing method of negative electrode plate, and silicon-carbide battery | |
| CN106384814B (en) | Co3V2O8The composite material and preparation method of C layers of cladding | |
| CN107681147A (en) | A kind of preparation method of solid electrolyte coating modification anode material for lithium-ion batteries and application | |
| CN109509874A (en) | A kind of preparation method of molybdenum trioxide cladding lithium-rich manganese-based anode material | |
| CN108376776A (en) | A kind of alternate core-shell structure ternary electrode material of lithium battery of height nickel and preparation method | |
| CN108039486A (en) | The hollow core shell structure vanadic anhydride anode electrode piece of tremelliform and its fastening lithium ionic cell preparation method | |
| CN109698303A (en) | A kind of electronic conductive material and its preparation and the application in lithium-sulfur cell coated separator | |
| CN104733725A (en) | Application and modified preparation method of manganese and lithium rich solid solution material | |
| CN103441239A (en) | Synthetic method for nanoscale ternary cathode material | |
| CN104241634B (en) | A kind of lithium ion battery richness lithium manganese anode material and preparation method thereof | |
| CN105047898A (en) | Twin-spherical lithium-rich cathode material of lithium ion secondary battery and preparation method thereof | |
| CN105914360A (en) | Method for preparing anode material of coated spinel lithium-rich lithium manganate | |
| CN101867036A (en) | Lithium-ion battery cathode material with long service life and high power as well as preparation method thereof |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170517 |