CN105591072A - Negative electrode piece of alpha-ZnMoO4 lithium ion battery and preparation method of negative electrode piece - Google Patents
Negative electrode piece of alpha-ZnMoO4 lithium ion battery and preparation method of negative electrode piece Download PDFInfo
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- H—ELECTRICITY
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H—ELECTRICITY
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- 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
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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
- H01M4/621—Binders
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Abstract
The invention discloses a negative electrode piece of an alpha-ZnMoO4 lithium ion battery and a preparation method of the negative electrode piece. The preparation method comprises the following steps: dissolving a zinc salt and molybdate at the mol ratio of 1 to 1 into distilled water respectively; dropwise adding a molybdate solution into the zinc salt solution, and further stirring and uniformly mixing; then standing and reacting at a room temperature; after a reaction is finished, centrifuging; taking a solid phase, and washing and drying; calcining in a high-temperature furnace to obtain a negative electrode material of the alpha-ZnMoO4 lithium ion battery; finally, after mixing the negative electrode material of the alpha-ZnMoO4 lithium ion battery, a binding agent and a conductive agent into paste and coating the paste on a copper foil; and drying and tableting to obtain the negative electrode piece of the alpha-ZnMoO4 lithium ion battery. The preparation method disclosed by the invention is simple and convenient, and has high yield, low cost and good crystallization degree; and the prepared negative electrode piece of the alpha-ZnMoO4 lithium ion battery has a wide development prospect.
Description
Technical field
The preparation method who the present invention relates to a kind of anode plate for lithium ionic cell, is specifically related to oneα-ZnMoO4Anode plate for lithium ionic cell and preparation method thereof.
Background technology
Quality is light, volume is little, operating voltage is high, energy density is high, output work because having for lithium ion batteryRate is large, charge efficiency is high and the advantage such as memory-less effect, has obtained in the field such as mobile phone, notebook computerApplication widely.
Lithium ion battery is made up of positive plate, negative plate, barrier film, electrolyte and shell conventionally. Wherein,Binding agent is for electrode active material being sticked to the macromolecular compound on collector. Its main workWith being bonding and keeping active material, intensifier electrode active material and conductive agent and active material and affluxElectronics between body contacts, and stablizes better the structure of pole piece, can be swollen for volume in charge and discharge processThe lithium ion battery plus-negative plate of swollen/contraction, requires binding agent can play certain buffering to this and doesWith. At present, the industrial binding agent of Kynoar (PVDF) as lithium ion battery, the N-of generally adoptingMethyl pyrrolidone (NMP) does dispersant. Because NMP price is more expensive, volatilization temperature is higher, andAnd the volatilization of organic solvent can cause certain environmental problem, therefore need the lithium of a kind of environmental protection of exploitation badlyIon battery negative plate.
Summary of the invention
The object of the present invention is to provide a kind of α-ZnMoO4Anode plate for lithium ionic cell and preparation side thereofMethod, the defect existing to overcome above-mentioned prior art, preparation technology of the present invention is simple, environmental protection, one-tenthThis is cheap, productive rate is high, and the charge and discharge potential of the electrode making is 0.01～3.5V, and coulomb efficiency is high firstIn 80%, specific capacity 50 still remains on 440mAhg after enclosing repeated charge-1。
For achieving the above object, the present invention adopts following technical scheme:
A kind of α-ZnMoO4The preparation method of anode plate for lithium ionic cell, comprises the following steps:
Step 1: the zinc salt that is 1:1 by mol ratio and molybdate are dissolved in respectively in distilled water, stirs and makes itFully dissolve;
Step 2: molybdate solution is dropwise added in zinc solution, after stirring, quiet at normal temperaturesPut reaction and obtain zinc molybdate persursor material;
Step 3: by after the zinc molybdate persursor material centrifugation obtaining in step 2, adopt the aqueous solutionAnd absolute ethanol washing, then dry and obtain zinc molybdate presoma;
Step 4: the zinc molybdate presoma that step 3 is obtained is put into high temperature furnace heat treatment, then natureAfter cool to room temperature, obtain α-ZnMoO4Lithium ion battery negative material;
Step 5: by α-ZnMoO4With binding agent, conductive agent in mass ratio 8:1:1 mix, grind through agateAlms bowl grinds evenly, after furnishing slurry, is coated on Copper Foil, and vacuum drying 12～24h, process through tablet press machineTo anode plate for lithium ionic cell.
Further, described molybdate is ammonium molybdate or sodium molybdate, and zinc salt is zinc nitrate or zinc chloride.
Further, in step 1, agitating mode is magnetic agitation, and mixing time is 10min.
Further, the rate of addition in step 2 is 1～3mL/min; Mixing time is 30min, quietPutting the reaction time is 1～5d.
Further, in step 3, centrifugal speed is 8000～9000r/min; Centrifugation time is 10～15min.
Further, while washing in step 3, alternately rinse 3～6 times with absolute ethyl alcohol and distilled water; DryTemperature is 60 DEG C.
Further, in step 4, high temperature furnace is Muffle furnace, and heat treatment temperature is 400～600 DEG C, the timeFor 40min～3h.
Further, in step 5, binding agent is sodium carboxymethylcellulose; Conductive agent is acetylene black.
Further, in step 5, coating thickness is 15～20 μ m; Vacuum drying temperature is 80～120 DEG C;Tablet press machine pressure is 80～120kg/cm2。
A kind of α-ZnMoO4Anode plate for lithium ionic cell, adopts above-mentioned α-ZnMoO4Lithium ion batteryThe preparation method of negative plate makes.
Compared with prior art, the present invention has following useful technique effect:
α-ZnMoO prepared by the present invention4Anode plate for lithium ionic cell, structure is tetragonal body, its molybdenum ionBe positioned at tetrahedral symmetrical centre, outside is by 4 O2-Surround, there is relatively good stability. DifferentIn other multicomponent transition metal oxides, α-ZnMoO4Can utilize two kinds of different electrochemical reactionsMechanism, the transformation mechanism between molybdenum element and lithium, zinc can carry out alloying reaction with lithium, thisTwo kinds of reactions can coexist in electrochemical lithium storage, and exist cooperative effect between them, can be commonPromote the raising of battery performance. In addition, the molybdenum resource output of China occupies second place of the world, utilizes suchResources advantage, developmental research zinc molybdate lithium ion battery negative material, tool is of great significance. WithTime, the present invention prepares α-ZnMoO4Anode plate for lithium ionic cell, taking sodium carboxymethylcellulose as binding agent,Reduce the internal resistance of interface impedance and the battery of electrode/electrolyte, improved the performance of battery, in addition, withWater is as dispersant, environmentally friendly, and low price, can play a role in energy conservation, thus realThe production of existing green non-pollution. Adopt the charge and discharge potential of the lithium ion battery that this negative plate makes to be0.01～3.5V, coulomb efficiency is higher than 80% first, and specific capacity 50 still remains on after enclosing repeated charge440mAhg-1。
Brief description of the drawings
Fig. 1 is α-ZnMoO prepared by embodiment 14The XRD collection of illustrative plates of lithium ion battery negative material;
Fig. 2 adopts the charge-discharge performance figure of the negative plate that makes of embodiment 1 for simulated battery.
Detailed description of the invention
Below embodiments of the present invention are described in further detail:
A kind of α-ZnMoO4The preparation method of anode plate for lithium ionic cell, comprises the following steps:
Step 1: the zinc salt that is 1:1 by mol ratio and molybdate are dissolved in respectively in distilled water, magnetic agitation10min fully dissolves it, and wherein, molybdate is ammonium molybdate or sodium molybdate, and zinc salt is zinc nitrate or chlorineChange zinc;
Step 2: molybdate solution is dropwise added in zinc solution with the speed of 1～3mL/min, stir30min, leaves standstill at normal temperatures reaction 1～5d and obtains zinc molybdate persursor material;
Step 3: by centrifugal with 8000～9000r/min the zinc molybdate persursor material obtaining in step 2After 10～15min, adopt absolute ethyl alcohol and distilled water alternately to rinse 3～6 times, then in baking oven with 60 DEG CDry and obtain zinc molybdate presoma;
Step 4: the zinc molybdate presoma that step 3 is obtained is put into 400～600 DEG C of heat treatments of Muffle furnace40min～3h, obtains α-ZnMoO after then naturally cooling to room temperature4Lithium ion battery negative material;
Step 5: by α-ZnMoO4With binding agent, conductive agent in mass ratio 8:1:1 mix, grind through agateAlms bowl grinds evenly, after furnishing slurry, is coated on Copper Foil, and coating thickness is 15～20 μ m, then existsVacuum drying 12～24h at 80～120 DEG C, through tablet press machine with 80～120kg/cm2Pressure treatment obtain lithiumIon battery negative plate, wherein, binding agent is sodium carboxymethylcellulose; Conductive agent is acetylene black.
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
Step 1: the zinc nitrate that is 1:1 by mol ratio and sodium molybdate are dissolved in respectively in distilled water, and magnetic force stirsMixing 10min fully dissolves it;
Step 2: sodium molybdate solution is dropwise added in zinc nitrate solution with the speed of 1mL/min, stir30min, leaves standstill at normal temperatures reaction 5d and obtains zinc molybdate persursor material;
Step 3: by the zinc molybdate persursor material obtaining in step 2 with the centrifugal 10min of 8000r/minAfter, adopt absolute ethyl alcohol and distilled water alternately to rinse 4 times, then in baking oven, obtain with 60 DEG C of oven dryZinc molybdate presoma;
Step 4: the zinc molybdate presoma that step 3 is obtained is put into 600 DEG C of heat treatment 3h of Muffle furnace,Then after naturally cooling to room temperature, obtain α-ZnMoO4Lithium ion battery negative material;
Step 5: by α-ZnMoO4With sodium carboxymethylcellulose, acetylene black in mass ratio 8:1:1 mix,Grind evenly through agate mortar, after furnishing slurry, be coated on Copper Foil, coating thickness is 15 μ m, thenVacuum drying 24h at 120 DEG C, through tablet press machine with 100kg/cm2Pressure treatment obtain lithium ion batteryNegative plate.
Fig. 1 is the α-ZnMoO of preparation4XRD figure, as can be seen from Figure 1 the material of preparation is pureα-the ZnMoO of phase4。
Taking the anode plate for lithium ionic cell that obtains as negative pole, with 1mol/LLiPF6Three component mixed solvents(volume ratio vinyl carbonate EC: dimethyl carbonate DMC: diethyl carbonate EMC=1:1:1) isElectrolyte, microporous polypropylene membrane is barrier film, lithium sheet is that positive plate is assembled into simulated battery, to simulated batteryCarry out performance test, adopt the new prestige cell tester in Shenzhen to carry out charging and discharging capacity circulation to simulated batteryPerformance test, carries out the experiment of constant current charge-discharge specific capacity loop test with the current density of 100mA/g, fillsDischarge voltage is limited in 0.01～3.5V, and as shown in Figure 2, simulated battery first as shown in Figure 2 for resultCharge/discharge capacity is respectively 965mAhg-1And 1206mAhg-1, and coulomb efficiency is 80% first, circulation50 circles, specific capacity remains on 440mAhg-1Left and right, cyclicity and having good stability.
Embodiment 2
Step 1: the zinc chloride that is 1:1 by mol ratio and sodium molybdate are dissolved in respectively in distilled water, and magnetic force stirsMixing 10min fully dissolves it;
Step 2: sodium molybdate solution is dropwise added in liquor zinci chloridi with the speed of 2mL/min, stir30min, leaves standstill at normal temperatures reaction 1d and obtains zinc molybdate persursor material;
Step 3: by the zinc molybdate persursor material obtaining in step 2 with the centrifugal 10min of 8500r/minAfter, adopt absolute ethyl alcohol and distilled water alternately to rinse 5 times, then in baking oven, obtain with 60 DEG C of oven dryZinc molybdate presoma;
Step 4: the zinc molybdate presoma that step 3 is obtained is put into 500 DEG C of heat treatment 3h of Muffle furnace,Then after naturally cooling to room temperature, obtain α-ZnMoO4Lithium ion battery negative material;
Step 5: by α-ZnMoO4With sodium carboxymethylcellulose, acetylene black in mass ratio 8:1:1 mix,Grind evenly through agate mortar, after furnishing slurry, be coated on Copper Foil, coating thickness is 20 μ m, thenVacuum drying 12h at 80 DEG C, through tablet press machine with 120kg/cm2Pressure treatment obtain lithium ion batteryNegative plate.
Embodiment 3
Step 1: the zinc nitrate that is 1:1 by mol ratio and ammonium molybdate are dissolved in respectively in distilled water, and magnetic force stirsMixing 10min fully dissolves it;
Step 2: ammonium molybdate solution is dropwise added in zinc nitrate solution with the speed of 3mL/min, stir30min, leaves standstill at normal temperatures reaction 3d and obtains zinc molybdate persursor material;
Step 3: by the zinc molybdate persursor material obtaining in step 2 with the centrifugal 15min of 9000r/minAfter, adopt absolute ethyl alcohol and distilled water alternately to rinse 6 times, then in baking oven, obtain with 60 DEG C of oven dryZinc molybdate presoma;
Step 4: the zinc molybdate presoma that step 3 is obtained is put into 400 DEG C of heat treatment 3h of Muffle furnace,Then after naturally cooling to room temperature, obtain α-ZnMoO4Lithium ion battery negative material;
Step 5: by α-ZnMoO4Mix by weight 8:1:1 with sodium carboxymethylcellulose, acetylene black,Grind evenly through agate mortar, after furnishing slurry, be coated on Copper Foil, coating thickness is 18 μ m, thenVacuum drying 18h at 100 DEG C, through tablet press machine with 80kg/cm2Pressure treatment obtain lithium ion batteryNegative plate.
Embodiment 4
Step 1: the zinc chloride that is 1:1 by mol ratio and sodium molybdate are dissolved in respectively in distilled water, and magnetic force stirsMixing 10min fully dissolves it;
Step 2: sodium molybdate solution is dropwise added in liquor zinci chloridi with the speed of 1mL/min, stir30min, leaves standstill at normal temperatures reaction 5d and obtains zinc molybdate persursor material;
Step 3: by the zinc molybdate persursor material obtaining in step 2 with the centrifugal 10min of 8000r/minAfter, adopt absolute ethyl alcohol and distilled water alternately to rinse 6 times, then in baking oven, obtain with 60 DEG C of oven dryZinc molybdate presoma;
Step 4: the zinc molybdate presoma that step 3 is obtained is put into 550 DEG C of heat treatments of Muffle furnace40min, obtains α-ZnMoO after then naturally cooling to room temperature4Lithium ion battery negative material;
Step 5: by α-ZnMoO4Mix by weight 8:1:1 with sodium carboxymethylcellulose, acetylene black,Grind evenly through agate mortar, after furnishing slurry, be coated on Copper Foil, coating thickness is 16 μ m, thenVacuum drying 20h at 100 DEG C, through tablet press machine with 100kg/cm2Pressure treatment obtain lithium ion batteryNegative plate.
Claims (10)
1. a α-ZnMoO4The preparation method of anode plate for lithium ionic cell, is characterized in that, comprise withLower step:
Step 1: the zinc salt that is 1:1 by mol ratio and molybdate are dissolved in respectively in distilled water, stirs and makes itFully dissolve;
Step 2: molybdate solution is dropwise added in zinc solution, after stirring, quiet at normal temperaturesPut reaction and obtain zinc molybdate persursor material;
Step 3: by after the zinc molybdate persursor material centrifugation obtaining in step 2, adopt the aqueous solutionAnd absolute ethanol washing, then dry and obtain zinc molybdate presoma;
Step 4: the zinc molybdate presoma that step 3 is obtained is put into high temperature furnace heat treatment, then natureAfter cool to room temperature, obtain α-ZnMoO4Lithium ion battery negative material;
Step 5: by α-ZnMoO4With binding agent, conductive agent in mass ratio 8:1:1 mix, grind through agateAlms bowl grinds evenly, after furnishing slurry, is coated on Copper Foil, and vacuum drying 12～24h, process through tablet press machineTo anode plate for lithium ionic cell.
2. a kind of α-ZnMoO according to claim 14The preparation side of anode plate for lithium ionic cellMethod, is characterized in that, described molybdate is ammonium molybdate or sodium molybdate, and zinc salt is zinc nitrate or zinc chloride.
3. a kind of α-ZnMoO according to claim 14The preparation side of anode plate for lithium ionic cellMethod, is characterized in that, in step 1, agitating mode is magnetic agitation, and mixing time is 10min.
4. a kind of α-ZnMoO according to claim 14The preparation side of anode plate for lithium ionic cellMethod, is characterized in that, the rate of addition in step 2 is 1～3mL/min; Mixing time is 30min,The standing reaction time is 1～5d.
5. a kind of α-ZnMoO according to claim 14The preparation side of anode plate for lithium ionic cellMethod, is characterized in that, in step 3, centrifugal speed is 8000～9000r/min; Centrifugation time is10～15min。
6. a kind of α-ZnMoO according to claim 14The preparation side of anode plate for lithium ionic cellMethod, is characterized in that, while washing, alternately rinses 3～6 times with absolute ethyl alcohol and distilled water in step 3; DryDry temperature is 60 DEG C.
7. a kind of α-ZnMoO according to claim 14The preparation side of anode plate for lithium ionic cellMethod, is characterized in that, in step 4, high temperature furnace is Muffle furnace, and heat treatment temperature is 400～600 DEG C, timeBetween be 40min～3h.
8. a kind of α-ZnMoO according to claim 14The preparation side of anode plate for lithium ionic cellMethod, is characterized in that, in step 5, binding agent is sodium carboxymethylcellulose; Conductive agent is acetylene black.
9. a kind of α-ZnMoO according to claim 14The preparation side of anode plate for lithium ionic cellMethod, is characterized in that, in step 5, coating thickness is 15～20 μ m; Vacuum drying temperature is 80～120 DEG C;Tablet press machine pressure is 80～120kg/cm2。
10. a α-ZnMoO4Anode plate for lithium ionic cell, is characterized in that, adopts claim 1～9α-ZnMoO described in any one4The preparation method of anode plate for lithium ionic cell makes.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106129393A (en) * | 2016-08-29 | 2016-11-16 | 陕西科技大学 | A kind of ZnMoO40.8H2o lithium ion battery negative material and preparation method thereof |
| CN106169575A (en) * | 2016-08-29 | 2016-11-30 | 陕西科技大学 | A kind of ZnMoO40.8H2o anode plate for lithium ionic cell and preparation method thereof |
| CN106571467A (en) * | 2016-11-04 | 2017-04-19 | 深圳市川马电子股份有限公司 | Preparation method and application of chromium molybdate |
| CN109830545A (en) * | 2019-02-14 | 2019-05-31 | 中国科学院半导体研究所 | A kind of aluminum-doped zinc oxide films surface modifying material, preparation method and battery |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106129393A (en) * | 2016-08-29 | 2016-11-16 | 陕西科技大学 | A kind of ZnMoO40.8H2o lithium ion battery negative material and preparation method thereof |
| CN106169575A (en) * | 2016-08-29 | 2016-11-30 | 陕西科技大学 | A kind of ZnMoO40.8H2o anode plate for lithium ionic cell and preparation method thereof |
| CN106571467A (en) * | 2016-11-04 | 2017-04-19 | 深圳市川马电子股份有限公司 | Preparation method and application of chromium molybdate |
| CN109830545A (en) * | 2019-02-14 | 2019-05-31 | 中国科学院半导体研究所 | A kind of aluminum-doped zinc oxide films surface modifying material, preparation method and battery |
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| C06 | Publication | ||
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Application publication date: 20160518 |