CN107492637B - A kind of porous carbon blended metal oxide and lithium ion battery prepared therefrom - Google Patents
A kind of porous carbon blended metal oxide and lithium ion battery prepared therefrom Download PDFInfo
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- CN107492637B CN107492637B CN201710587473.XA CN201710587473A CN107492637B CN 107492637 B CN107492637 B CN 107492637B CN 201710587473 A CN201710587473 A CN 201710587473A CN 107492637 B CN107492637 B CN 107492637B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of porous carbon blended metal oxide and lithium ion battery prepared therefrom, the porous carbon blended metal oxide the preparation method is as follows: the 1) preparation of 3,3 ', 5,5 '-azo benzene tetracarboxylic acids；2) preparation of Cu-MOF material；3) activation, calcining of Cu-MOF material.Lithium ion battery of the invention includes positive plate, negative electrode tab, diaphragm and electrolyte；The negative electrode tab includes following components: porous carbon blended metal oxide, conductive black and binder.Porous carbon blended metal oxide of the invention is in shuttle shape, and the cyclical stability and high rate performance of lithium ion battery can be promoted as lithium ion battery negative material；Lithium ion battery of the invention has many advantages, such as that coulombic efficiency is high, charging and discharging capacity is high, high rate performance is good, cycle performance is good.
Description
Technical field
The present invention relates to a kind of porous carbon blended metal oxide and lithium ion batteries prepared therefrom, belong to lithium-ion electric
Pool technology field.
Background technique
Lithium ion battery has many advantages, such as energy density height, output voltage height, memory-less effect, non-environmental-pollution, not only
It can be used for portable electronic device, be also used as the energy storage of the equipment such as electric powered motor power supply and solar energy or wind energy
Component has a good application prospect.Traditional lithium ion battery is generally using graphite as negative electrode material, with stratiform cobalt acid lithium
(LiCoO2) or LiFePO4 (LiFePO4) it is positive electrode, using nonaqueous lithium ion conducting medium as electrolyte.However, graphite-based
The theoretical specific capacity of negative electrode material only has 372mAh/g, it is difficult to which the requirement for meeting high capacity and fast charging and discharging needs the property found
It can better alternative materials.
In recent years, it was discovered by researchers that metal oxide negative electrode material has theoretical capacity height, good cycle, safety
The advantages that performance is high, be substitute graphite ideal material, but the generally existing poorly conductive of existing metal oxide negative electrode material,
The problems such as irreversible capacity is big, charge and discharge front and back volume change is big, structural collapse is also easy to produce in charge and discharge process and volume is swollen
Swollen effect will ultimately result in battery capacity decaying and reduced service life.Therefore, it is necessary to develop new metal oxide cathode material
Material is just able to satisfy actual demand.
Summary of the invention
The purpose of the present invention is to provide a kind of porous carbon blended metal oxide and lithium ion batteries prepared therefrom.
The technical solution used in the present invention is:
A kind of preparation method of porous carbon blended metal oxide, comprising the following steps:
1) 5- nitroisophthalic acid and zinc powder are dissolved in solvent I, sufficiently react, obtains 3,3 ', 5,5 '-azobenzene tetramethyls
Acid；
2) by Cu (NO3)2, polyvinylpyrrolidone and 3,3 ', 5,5 '-azo benzene tetracarboxylic acids are dissolved in solvent II, sufficiently anti-
It answers, obtains Cu-MOF material；
3) it by Cu-MOF material heat-activated, then is calcined, obtains porous carbon blended metal oxide.
The molar ratio of 5- nitroisophthalic acid, zinc powder described in step 1) is 3:(1~2).
Solvent I described in step 1) be second alcohol and water mixed solvent, wherein ethyl alcohol, water volume ratio be 1:(1~2).
The temperature reacted in step 1) is 90~110 DEG C, and the reaction time is 20~30h.
Cu (NO described in step 2)3)2, polyvinylpyrrolidone, 3,3 ', the molar ratios of 5,5 '-azo benzene tetracarboxylic acids is 3:
(0~1): (1~2).
Solvent II described in step 2) is the mixed solvent of n,N-Dimethylformamide and ethyl alcohol, wherein N, N- dimethyl methyl
Amide, ethyl alcohol volume ratio be 1:(1~2).
Reaction in step 2) carries out under conditions of microwave heating, and microwave power is 300~500W, reaction time 3
~7min.
The temperature of heat-activated is 110~130 DEG C in step 3), and activation time is 20~30h.
The temperature calcined in step 3) is 450~550 DEG C, and calcination time is 1~3h.
A kind of lithium ion battery, including positive plate, negative electrode tab, diaphragm and electrolyte；The negative electrode tab includes with the following group
Point: porous carbon blended metal oxide, conductive black and the binder of above method preparation.
The beneficial effects of the present invention are:
1) porous carbon blended metal oxide of the invention has special shuttle shape pattern, and it is negative to be used as lithium ion battery
Pole material had not only shortened transmission path of the lithium ion in charge and discharge process, but also was conducive to lithium ion and aoxidizes in carbon doping metals
The insertion and abjection on object surface, and volume of the carbon blended metal oxide in charge and discharge process can also be slowed down to a certain extent
Variation, can promote the high rate performance of lithium ion battery；
2) lithium ion battery of the invention is high with coulombic efficiency, charging and discharging capacity is high, high rate performance is good, cyclicity
Can be good the advantages that.
Detailed description of the invention
Fig. 1 is the SEM figure of the porous carbon blended metal oxide of embodiment 1.
Fig. 2 is the TEM figure of the porous carbon blended metal oxide of embodiment 1.
Fig. 3 is the powder diffraction and Raman spectrogram of the porous carbon blended metal oxide of embodiment 1.
Fig. 4 is the photoelectron spectroscopy figure of the porous carbon blended metal oxide of embodiment 1.
Fig. 5 is the absorption property and graph of pore diameter distribution of the porous carbon blended metal oxide of embodiment 1.
Fig. 6 is the cyclic voltammetry figure of the lithium ion battery of embodiment 1.
Fig. 7 is the constant current charge-discharge curve graph of the lithium ion battery of embodiment 1.
Fig. 8 is the cycle performance test chart of the lithium ion battery of embodiment 1.
Fig. 9 is the high rate performance test chart of the lithium ion battery of embodiment 1.
Specific embodiment
A kind of preparation method of porous carbon blended metal oxide, comprising the following steps:
1) 5- nitroisophthalic acid and zinc powder are dissolved in solvent I, sufficiently react, obtains 3,3 ', 5,5 '-azobenzene tetramethyls
Acid；
2) by Cu (NO3)2, polyvinylpyrrolidone and 3,3 ', 5,5 '-azo benzene tetracarboxylic acids are dissolved in solvent II, sufficiently anti-
It answers, obtains Cu-MOF material；
3) it by Cu-MOF material heat-activated, then is calcined, obtains porous carbon blended metal oxide.
Preferably, the molar ratio of 5- nitroisophthalic acid, zinc powder described in step 1) is 3:(1~2).
Preferably, solvent I described in step 1) be second alcohol and water mixed solvent, wherein ethyl alcohol, water volume ratio be 1:
(1~2).
Preferably, the temperature reacted in step 1) is 90~110 DEG C, and the reaction time is 20~30h.
Preferably, Cu (NO described in step 2)3)2, polyvinylpyrrolidone, 3,3 ', 5,5 '-azo benzene tetracarboxylic acids rub
You are than being 3:(0~1): (1~2).
Preferably, solvent II described in step 2) is the mixed solvent of n,N-Dimethylformamide and ethyl alcohol, wherein N, N-
Dimethylformamide, ethyl alcohol volume ratio be 1:(1~2).
Preferably, the reaction in step 2) carries out under conditions of microwave heating, and microwave power is 300~500W, reaction
Time is 3~7min.
Preferably, the temperature of heat-activated is 110~130 DEG C in step 3), and activation time is 20~30h.
Preferably, the temperature calcined in step 3) is 450~550 DEG C, and calcination time is 1~3h.
A kind of lithium ion battery, including positive plate, negative electrode tab, diaphragm and electrolyte；The negative electrode tab includes with the following group
Point: porous carbon blended metal oxide, conductive black and the binder of above method preparation.
Preferably, the porous carbon blended metal oxide, conductive black, binder mass ratio be 7:(1~2):
(1~2).
Preferably, the conductive black is Super P.
Preferably, the binder is Kynoar.
Preferably, the diaphragm is polyethylene diagrams.
Preferably, the electrolyte is by lithium hexafluoro phosphate, ethylene carbonate (EC), diethyl carbonate (DEC) and carbonic acid
Methyl ethyl ester (EMC) composition, the concentration of lithium hexafluoro phosphate are 1mol/L, ethylene carbonate, diethyl carbonate, methyl ethyl carbonate body
Product is than for than for 1:(1~2): (1~2).
The present invention will be further explained combined with specific embodiments below and explanation.
Embodiment 1:
A kind of preparation method of porous carbon blended metal oxide, comprising the following steps:
1) preparation of 3,3 ', 5,5 '-azo of organic ligand benzene tetracarboxylic acid: by the 5- nitroisophthalic acid of 0.3mmol and
Round-bottomed flask is added in the zinc powder of 0.125mmol, adds mixed solvent (ethyl alcohol, H of the second alcohol and water of 25mL2The volume ratio of O is
1:1), being placed in 100 DEG C of reactions in oil bath pan, for 24 hours, filter residue is dissolved in the NaOH solution of 1mol/L by filtering, is filtered, and adjusts filter
The pH value of liquid is precipitated precipitating, filters, drying obtains the 3 of Chinese red, 3 ', 5,5 '-azo benzene tetracarboxylic acids, the side of reaction to acidity
Formula is as follows:
2) preparation of Cu-MOF material: by the Cu (NO of 0.3mmol3)2, 0.001mmol PVP and 0.1mmol 3,3 ',
5,5 '-azo benzene tetracarboxylic acids are dissolved in the DMF and H of 25mL2O mixed solvent (DMF, H2The volume ratio of O is 1:2) in, it is placed in microwave
400W heating reaction 5min, centrifuge washing obtain Cu-MOF material in reactor；
3) activation, calcining of Cu-MOF material: the Cu-MOF material of step 2) is placed at 110 DEG C and is heated for 24 hours, visitor is removed
Body molecule, then 500 DEG C of calcining 2h in tube furnace, obtain porous carbon blended metal oxide.
A kind of preparation method of lithium ion battery, comprising the following steps:
1) by above-mentioned steps preparation porous carbon blended metal oxide, conductive black Super P, Kynoar according to
Mass ratio 7:2:1 is uniformly mixed, and obtains negative electrode material, then be prepared into negative electrode tab；
2) lithium hexafluoro phosphate, ethylene carbonate (EC), diethyl carbonate (DEC) and methyl ethyl carbonate (EMC) are mixed equal
Even, the concentration of lithium hexafluoro phosphate is 1mol/L, ethylene carbonate, diethyl carbonate, methyl ethyl carbonate volume ratio be 1:1:1,
Obtain electrolyte；
3) positive plate and polyethylene diagrams are got out, positive plate, negative electrode tab, diaphragm and electrolyte are assembled into lithium-ion electric
Pond.
The SEM of porous carbon blended metal oxide manufactured in the present embodiment schemes as shown in Figure 1, TEM schemes as shown in Fig. 2, powder
Last diffraction and Raman spectrogram as shown in figure 3, photoelectron spectroscopy (XPS) figure as shown in figure 4, absorption property and graph of pore diameter distribution such as
Shown in Fig. 5.
From Fig. 1 and Fig. 2: porous carbon blended metal oxide has shuttle shape pattern, and is hollow structure.
As shown in Figure 3: porous carbon blended metal oxide is made of copper oxide and agraphitic carbon.
As shown in Figure 4: the copper oxide in porous carbon blended metal oxide is+divalent copper, is free of cuprous oxide.
As shown in Figure 5: the microcellular structure of porous carbon blended metal oxide is abundant, and specific surface area is high.
The cyclic voltammetry figure of lithium ion battery manufactured in the present embodiment as shown in Figure 6 (be followed successively by the 1st from outside to inside,
2, the curve of 3,4 tests), constant current charge-discharge curve graph (is followed successively by the 1st, 2,3,50,100 survey as shown in Figure 7 from right to left
The curve of examination), cycle performance test chart is as shown in figure 8, high rate performance test chart is as shown in Figure 9.
As shown in Figure 6: the lithium ion battery prepared by the porous carbon blended metal oxide of the present embodiment is tested in the first run
Middle there are a redox peaks, and this peak disappears in second and third wheel test, this is attributed to an irreversible process, i.e.,
SEI film is formed in electrode surface.
As shown in Figure 7: by the charge and discharge level of lithium ion battery prepared by the porous carbon blended metal oxide of the present embodiment
Platform has relatively low charge and discharge platform in 1V or so, illustrates that porous carbon blended metal oxide has good electrochemistry
Energy.
As shown in Figure 8: being shown well by lithium ion battery prepared by the porous carbon blended metal oxide of the present embodiment
Charge-discharge performance, current density be 100mA/g when, for the first time electric discharge can reach 1259mAh/g, by 100 charge and discharge
Circulation, specific capacity can be stablized in 800mAh/g or so, and coulombic efficiency is higher, shows good chemical property.
As shown in Figure 9: the lithium ion battery prepared by the porous carbon blended metal oxide of the present embodiment is in charge and discharge electricity
When current density 100mA/g, specific capacity maintains 800mAh/g or so after recycling 100 times, in charging and discharging currents density 500mA/g
When, specific capacities maintain 600mAh/g or so after recycling 100 times, and decaying is too many, embody good times of material it is forthright
Energy.
Embodiment 2:
A kind of preparation method of porous carbon blended metal oxide, comprising the following steps:
1) preparation of 3,3 ', 5,5 '-azo of organic ligand benzene tetracarboxylic acid: by the 5- nitroisophthalic acid of 0.6mmol and
Round-bottomed flask is added in the zinc powder of 0.2mmol, adds mixed solvent (ethyl alcohol, H of the second alcohol and water of 50mL2The volume ratio of O is 1:
2) 110 DEG C of reaction 20h in oil bath pan, are placed in, filters, filter residue is dissolved in the NaOH solution of 1mol/L, are filtered, filtrate is adjusted
PH value to acidity, precipitating is precipitated, filters, drying obtains the 3 of Chinese red, 3 ', 5,5 '-azo benzene tetracarboxylic acids；
2) preparation of Cu-MOF material: by the Cu (NO of 0.6mmol3)2, 0.1mmol PVP and 0.3mmol 3,3 ', 5,
5 '-azo benzene tetracarboxylic acids are dissolved in the DMF and H of 50mL2O mixed solvent (DMF, H2The volume ratio of O is 1:1.5) in, it is placed in microwave
350W heating reaction 7min, centrifuge washing obtain Cu-MOF material in reactor；
3) activation, calcining of Cu-MOF material: the Cu-MOF material of step 2) is placed at 120 DEG C and heats 30h, removes visitor
Body molecule, then 550 DEG C of calcining 1h in tube furnace, obtain porous carbon blended metal oxide.
A kind of preparation method of lithium ion battery, comprising the following steps:
1) by above-mentioned steps preparation porous carbon blended metal oxide, conductive black Super P, Kynoar according to
Mass ratio 7:1:2 is uniformly mixed, and obtains negative electrode material, then be prepared into negative electrode tab；
2) lithium hexafluoro phosphate, ethylene carbonate (EC), diethyl carbonate (DEC) and methyl ethyl carbonate (EMC) are mixed equal
Even, the concentration of lithium hexafluoro phosphate is 1mol/L, ethylene carbonate, diethyl carbonate, methyl ethyl carbonate volume ratio be 1:1:1,
Obtain electrolyte；
3) positive plate and polyethylene diagrams are got out, positive plate, negative electrode tab, diaphragm and electrolyte are assembled into lithium-ion electric
Pond.
Embodiment 3:
A kind of preparation method of porous carbon blended metal oxide, comprising the following steps:
1) preparation of 3,3 ', 5,5 '-azo of organic ligand benzene tetracarboxylic acid: by the 5- nitroisophthalic acid of 1.2mmol and
Round-bottomed flask is added in the zinc powder of 0.8mmol, adds mixed solvent (ethyl alcohol, H of the second alcohol and water of 100mL2The volume ratio of O is
1:1.5), 90 DEG C of reaction 30h in oil bath pan are placed in, filters, filter residue is dissolved in the NaOH solution of 1mol/L, are filtered, are adjusted
The pH value of filtrate is precipitated precipitating, filters, drying obtains the 3 of Chinese red, 3 ', 5,5 '-azo benzene tetracarboxylic acids to acidity；
2) preparation of Cu-MOF material: by the Cu (NO of 1.2mmol3)2, 0.4mmol PVP and 0.8mmol 3,3 ', 5,
5 '-azo benzene tetracarboxylic acids are dissolved in the DMF and H of 100mL2O mixed solvent (DMF, H2The volume ratio of O is 1:1) in, it is placed in microwave
500W heating reaction 3min, centrifuge washing obtain Cu-MOF material in reactor；
3) activation, calcining of Cu-MOF material: the Cu-MOF material of step 2) is placed at 130 DEG C and heats 20h, removes visitor
Body molecule, then 450 DEG C of calcining 3h in tube furnace, obtain porous carbon blended metal oxide.
A kind of preparation method of lithium ion battery, comprising the following steps:
1) by above-mentioned steps preparation porous carbon blended metal oxide, conductive black Super P, Kynoar according to
Mass ratio 7:1:2 is uniformly mixed, and obtains negative electrode material, then be prepared into negative electrode tab；
2) lithium hexafluoro phosphate, ethylene carbonate (EC), diethyl carbonate (DEC) and methyl ethyl carbonate (EMC) are mixed equal
Even, the concentration of lithium hexafluoro phosphate is 1mol/L, ethylene carbonate, diethyl carbonate, methyl ethyl carbonate volume ratio be 1:1:1,
Obtain electrolyte；
3) positive plate and polyethylene diagrams are got out, positive plate, negative electrode tab, diaphragm and electrolyte are assembled into lithium-ion electric
Pond.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of preparation method of porous carbon blended metal oxide, it is characterised in that: the following steps are included:
1) 5- nitroisophthalic acid and zinc powder are dissolved in solvent I, sufficiently react, obtains 3,3 ', 5,5 '-azo benzene tetracarboxylic acids；
2) by Cu (NO3)2, polyvinylpyrrolidone and 3,3 ', 5,5 '-azo benzene tetracarboxylic acids are dissolved in solvent II, sufficiently react, obtain
To Cu-MOF material；
3) it by Cu-MOF material heat-activated, then is calcined, obtains porous carbon blended metal oxide；
Solvent I described in step 1) be second alcohol and water mixed solvent, wherein ethyl alcohol, water volume ratio be 1:(1~2)；
Solvent II described in step 2) is the mixed solvent of n,N-Dimethylformamide and ethyl alcohol, wherein N, N- dimethyl formyl
Amine, ethyl alcohol volume ratio be 1:(1~2).
2. preparation method according to claim 1, it is characterised in that: 5- nitroisophthalic acid, zinc described in step 1)
The molar ratio of powder is 3:(1~2).
3. preparation method according to claim 1, it is characterised in that: the temperature reacted in step 1) is 90~110 DEG C, instead
It is 20~30h between seasonable.
4. preparation method according to claim 1, it is characterised in that: Cu (NO described in step 2)3)2, polyvinylpyrrolidine
Ketone, 3,3 ', the molar ratio of 5,5 '-azo benzene tetracarboxylic acids are 3:(0~1): (1~2).
5. preparation method according to claim 1, it is characterised in that: the reaction in step 2) is under conditions of microwave heating
It carries out, microwave power is 300~500W, and the reaction time is 3~7min.
6. preparation method according to claim 1, it is characterised in that: the temperature of heat-activated is 110~130 in step 3)
DEG C, activation time is 20~30h；The temperature calcined in step 3) is 450~550 DEG C, and calcination time is 1~3h.
7. the porous carbon blended metal oxide of any one of claim 1~6 the method preparation.
8. a kind of lithium ion battery, it is characterised in that: including positive plate, negative electrode tab, diaphragm and electrolyte；The negative electrode tab packet
Include following components: porous carbon blended metal oxide, conductive black and binder as claimed in claim 7.
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| GB2573886A (en) * | 2018-04-25 | 2019-11-20 | Vapor Point Llc | Process of preparing metal-organic framework material |
| CN108559097B (en) * | 2018-04-28 | 2020-10-02 | 中北大学 | 3,3',5,5' -azoxybenzenetetracarboxylic acid europium (III) metal coordination polymer and synthetic method and application thereof |
| CN109092364B (en) * | 2018-08-20 | 2021-06-22 | 宁波大学 | Copper metal organic framework mimic enzyme material and preparation and application thereof |
| CN109433267B (en) * | 2018-10-31 | 2021-11-23 | 河南立诺制药有限公司 | Preparation method of sertindole intermediate for resisting delayed dyskinesia |
| CN110743502A (en) * | 2019-10-24 | 2020-02-04 | 莫林祥 | Based on Fe3O4-Co-based MOFs magnetic composite adsorption material and preparation method thereof |
| CN111180749B (en) * | 2020-01-03 | 2021-08-17 | 华中科技大学 | Air electrode of metal-air battery and preparation method thereof |
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