CN110336013A - A kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping - Google Patents
A kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping Download PDFInfo
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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
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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
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/52—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
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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
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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
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- 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
Present invention relates particularly to a kind of preparation methods of rubidium cation doping acid nickel negative electrode material.Method includes the following steps: soluble cobalt, soluble nickel salt are dissolved in glycerine and the mixed solution of isopropyl alcohol by (1), hydro-thermal reaction occurs loaded on reaction kettle after mixing evenly, is cooled to room temperature, is centrifuged, washs, dries, obtain precursor powder；(2) rubidium salt is added in precursor powder, is calcined under atmosphere of inert gases after milling uniformly, after temperature drops to room temperature, the cobalt acid nickel negative electrode material of rubidium doping is obtained after milling uniformly.The rubidium cation doping acid nickel negative electrode material that the present invention is prepared, the radius of rubidium ion is larger, due to the doping of rubidium, so that the vacancy of material is more, so that ionic conductivity gets a promotion, is assembled into lithium ion battery, available superior high rate performance.
Description
Technical field
The invention belongs to field of lithium ion battery, and in particular to a kind of preparation side of the cobalt acid nickel negative electrode material of rubidium doping
Method.
Background technique
In recent years, wearable device and mixed power electric car become increasingly popular, and have largely pushed the energy
The innovation of conversion/memory technology.In various energy storage technologies, lithium ion battery (LIBs) is because its energy density is high, stable circulation
Property special attention good, pollution-free and by people, wherein negative electrode material is the key that influence battery performance and service life material
Material.
Although the intercalations negative electrode material such as graphite of commercial applications has the advantages that good stability at present, there is also reasons
By the small limitation of capacity, it is not able to satisfy the growing energy density demand of people.Cobalt acid nickel is that one kind of lithium ion battery is negative
Pole material has many advantages, such as that specific capacity is high, at low cost, pollution-free, safety is good, has broad application prospects.But simultaneously
The shortcomings that it also has conductivity low, and there are volume expansions in charge and discharge process.
For disadvantages mentioned above, there are three types of current mainstream solutions, and one is synthesis nano structural material, such as nanoparticles
Son, nanotube, nanofiber, nanometer rods etc. not only can increase the specific surface area of material, provide more active sites
Point, but also can effectively alleviate the influence of volume expansion bring；Another kind is the method for carbon material doping, cladding, carbon member
The electric conductivity of material not only can be improved in element, improves cycle performance, can also form a protective layer, effectively inhibits volume swollen
It is swollen；Finally one is element dopings, and some metallic element doping such as some nonmetalloids such as N, S or Al, Mn are entered, benefit
Host material property is inherently modified with hetero atom can greatly improve performance.
For example, CN 109273278A discloses a kind of preparation of cobalt acid nickel nano wire cladding carbon fiber flexible electrode material
Method, preparation process are as follows: PAN is dissolved in heating stirring in DMF, prepared polymer solution；Then method of electrostatic spinning is used
Flexible membranous carbon fiber precursor is prepared, flexible carbon fiber substrates is obtained after pre-oxidation, carbonization, then by solvent heat, makes cobalt
Sour nickel obtains the nanowire supported carbon fiber flexible electrode material of cobalt acid nickel after carbon fiber surface nucleating growth, calcining.The method
Prepared material combines the good cyclical stability of carbon material and the high energy density and specific capacitance of cobalt acid nickel, from entirety
On improve the chemical property of electrode.A kind of for another example nano-chip arrays cobalt acid nickel-carbon composite wood that CN108538611A is announced
Material and preparation method thereof, preparation process is as follows: wet tissue being ultrasonically treated, wet tissue fiber is dried to obtain；By nickel nitrate, nitric acid
Cobalt, urea and hexamethylenetetramine, which are added in ethanol water, obtains mixed liquor；After wet tissue fiber is impregnated in mixed liquor
It carries out hydro-thermal reaction and obtains the wet tissue fibrous matrix that load has Ni-Co presoma；Then the heating and calcining in mixed gas atmosphere
Reaction obtains nano-chip arrays cobalt acid nickel-carbon composite after cooling.It is all to apply nanostructure in conjunction with carbon material above
Method can also improve the electric conductivity of electrode material while with height ratio capacity, inhibit material volume expansion to be brought
Influence, but exist again forthright performance it is bad, manufacturing process is cumbersome, the bad control of product structure pattern, huge energy consumption lack
Point is not suitable for extensive production application.
Summary of the invention
The technical problem to be solved by the present invention is to provide a kind of rubidium doping in view of the deficiency of the prior art
Cobalt acid nickel negative electrode material preparation method, utilize the presoma bead for the cobalt acid nickel negative electrode material that hydro-thermal method is prepared, grain
Diameter is 400-900nm, and pattern is uniform, adulterates the biggish rubidium ion of radius subsequently through calcining, so that the vacancy of material is more, from
And ionic conductivity is got a promotion, it is assembled into lithium ion battery, available superior high rate performance.
The present invention solves above-mentioned technical problem by the following technical programs:
A kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping, key step are as follows:
Step 1: soluble cobalt, soluble nickel salt being dissolved in the mixed solution of glycerine and isopropanol, stirring is equal
It is even after loaded on reaction kettle carry out hydro-thermal reaction, be cooled to room temperature, be centrifuged, wash, dry after obtain precursor powder；
Step 2: rubidium salt will be added in precursor powder, calcined under protective gas atmosphere after milling uniformly, dropped to temperature
To after room temperature, to get the cobalt acid nickel negative electrode material adulterated to rubidium after milling uniformly.
According to the above scheme, the concentration of the nickel ion in step 1 mixed solution is 0.01-0.1mol/L, Ni2+: Co2+Rub
You are than being 1:2.
According to the above scheme, the volume ratio of glycerine and isopropanol is 1:10-1:5 in step 1.
According to the above scheme, soluble cobalt is any one in cobalt nitrate, cobaltous sulfate, cobalt chloride, cobalt acetate etc. in step 1
Kind, soluble nickel salt is any one in nickel nitrate, nickel sulfate, nickel chloride, nickel acetate etc..
According to the above scheme, hydrothermal temperature is 140-180 DEG C in step 1, reaction time 6-12h；It is preferred that 140-160
DEG C reaction 6-9h.
According to the above scheme, drying temperature is 60-80 DEG C in step 1, drying time 6-12h.
According to the above scheme, in step 2, the molar ratio of cobalt element is 1:10- in the rubidium element and soluble cobalt in rubidium salt
1:5。
According to the above scheme, in step 2, rubidium salt is any one in rubidium carbonate, rubidium hydroxide, rubidium chloride etc..
According to the above scheme, in step 2, protective gas is the inert gases such as nitrogen or argon gas.
According to the above scheme, in step 2, calcination process are as follows: under protective gas protection, with the heating rate of 1-5 DEG C/min
It rises in 550-850 DEG C of calcining 4-8h.
Compared with prior art, the beneficial effects of the present invention are:
1, the method that the present invention combines nanometer bead and element doping, the cobalt acid nickel presoma prepared first with hydro-thermal method
It is partial size in the bead of 400-900nm or so, pattern is single；Then by way of calcining, rubidium doping is entered, this method makes
Low raw-material cost, method are simple.
2, the present invention is dense in the mixed solution of glycerine and isopropanol by control dissolubility cobalt salt, soluble nickel salt
Degree, can control cobalt ions and nickel ion and glycerine association rate, and due to the effect of Ostwald ripening and hydrogen bond,
And then the particle size for forming presoma is controlled, and driven by surface energy minimization and principle, it is smooth that presoma will form surface
Nanometer bead.And in mixing rubidium calcination process, due to the release of the small molecules such as vapor, it will form surface and internal appearance be more
The final product of pore structure.
3, the rubidium cation doping acid nickel negative electrode material for the nanometer microspheric form that this method is prepared, large specific surface area, structure are steady
It is fixed, it is possible to provide the active site of lithium ion insertion abjection is more, thus chemical property is improved；Simultaneously because the doping of rubidium,
Crystal spacing is increased, is spread convenient for lithium ion, therefore high rate performance is also improved.
Detailed description of the invention
Fig. 1 is the presoma SEM figure of rubidium cation doping acid nickel negative electrode material in embodiment 1.
Fig. 2 is the SEM figure of rubidium cation doping acid nickel negative electrode material in embodiment 1.
Fig. 3 is curve of double curvature figure of the rubidium cation doping acid nickel negative electrode material under different current densities in embodiment 1.
Fig. 4 is cyclic curve figure of the cobalt acid nickel negative electrode material of rubidium doping in embodiment 1 under 1C current density.
Specific embodiment
Technical solution of the present invention is further illustrated below with reference to embodiment, but is not to be construed as the limit to technical solution
System.
Embodiment 1
A kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping, the specific steps are as follows:
(1) cobalt nitrate, nickel nitrate are dissolved in glycerine and the mixed solution of isopropyl alcohol, Ni in mixed solution
(NO3)2Concentration be 0.1mol, the volume ratio of glycerine and isopropanol is 1:5, and Ni ion: the molar ratio of Co ion is 1:2, is stirred
React 12h at 180 DEG C loaded on reaction kettle after mixing uniformly, be cooled to room temperature, wash, dry after obtain precursor powder；
(2) rubidium carbonate will be continuously added in precursor powder, the molar ratio of Rb element and Co element is 1:5, is milled uniformly
Afterwards under argon atmosphere, 850 DEG C of calcining 8h are warming up to the rate of 5 DEG C/min, after temperature drops to room temperature, after milling uniformly
The cobalt acid nickel negative electrode material adulterated to rubidium.
By above-mentioned rubidium cation doping acid nickel negative electrode material with acetylene black, binder PVDF 8:1:1 in mass ratio is with slurry and coats
Negative electrode tab is made in copper foil current collector, 80 DEG C of dry 12h, are then transferred into the glove box full of argon gas under vacuum conditions
In.It is to electrode with metal lithium sheet, Celgard 2400 is diaphragm, the ethylene carbonate and carbonic acid two of 1mol/L lithium hexafluoro phosphate
Methyl esters (ethylene carbonate and dimethyl carbonate volume ratio 1:1) mixed solution is electrolyte, is assembled into CR2016 button electricity respectively
Pond.It is tested with blue electric system, after 500 circles are recycled under the current density of 500 μ A/mg, still there is 755mAhg-1Appearance
Amount, capacity retention ratio is about 77%；Then respectively with the electricity of 200 μ A/mg, 500 μ A/mg, 1000 μ A/mg and 2000 μ A/mg
Current density tests high rate performance, has respectively obtained 821mAhg-1、801mAh·g-1、733mAh·g-1、512mAh·g-1Appearance
Amount.
By Fig. 1 and Fig. 2 it is found that the presoma synthesized in embodiment 1 is partial size in the nanometer bead of 400-900nm, mixing
When rubidium is calcined, since presoma can decompose, some small molecules such as vapor are released, so that the surface of entire nanometer bead is thicker
Rough, active site becomes more, forms structure shown in Fig. 2.
Embodiment 2
A kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping, the specific steps are as follows:
(1) cobalt chloride, nickel chloride are dissolved in the mixed solution of glycerine and isopropanol, NiCl in mixed solution2's
Concentration is 0.01mol, and the volume ratio of glycerine and isopropanol is 1:10, and Ni ion: the molar ratio of Co ion is 1:2, and stirring is equal
React 6h at 140 DEG C loaded on reaction kettle after even, be cooled to room temperature, wash, dry after obtain precursor powder；
(2) rubidium chloride will be continuously added in precursor powder, the molar ratio of Rb element and Co element is 1:10, is milled uniformly
Afterwards under argon atmosphere, 550 DEG C of calcining 4h are warming up to the rate of 1 DEG C/min, after temperature drops to room temperature, after milling uniformly
The cobalt acid nickel negative electrode material adulterated to rubidium.
Above-mentioned rubidium cation doping acid nickel electrode material and embodiment 1 are assembled into battery under the same conditions, with blue electric system
It is tested, after 500 circles are recycled under the current density of 500 μ A/mg, there is 812mAhg-1Capacity, capacity retention ratio is big
About 82.8%；Then multiplying power is tested with the current density of 200 μ A/mg, 500 μ A/mg, 1000 μ A/mg and 2000 μ A/mg respectively
Performance has respectively obtained 899mAhg-1、850mAh·g-1、764mAh·g-1、545mAh·g-1Capacity.
Embodiment 3
A kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping, the specific steps are as follows:
(1) cobaltous sulfate, nickel sulfate are dissolved in glycerine and the mixed solution of isopropyl alcohol, NiSO in mixed solution4
Concentration be 0.01mol, the volume ratio of glycerine and isopropanol is 1:7, and Ni ion: the molar ratio of Co ion is 1:2, and stirring is equal
React 9h at 160 DEG C loaded on reaction kettle after even, be cooled to room temperature, wash, dry after obtain precursor powder；
(2) rubidium hydroxide will be continuously added in precursor powder, the molar ratio of Rb element and Co element is 1:7, is milled
After even under argon atmosphere, 700 DEG C of calcining 6h are warming up to the rate of 2.5 DEG C/min, after temperature drops to room temperature, are milled uniformly
The cobalt acid nickel negative electrode material of rubidium doping is obtained afterwards.
Above-mentioned rubidium cation doping acid nickel electrode material is assembled into battery, is tested with blue electric system, 500 μ A/mg's
Under current density after 500 circle of circulation, still there is 695mAhg-1Capacity, capacity retention ratio is about 71%；Then respectively with
The current density test high rate performance of 200 μ A/mg, 500 μ A/mg, 1000 μ A/mg and 2000 μ A/mg, respectively obtain
755mAh·g-1、712mAh·g-1、688mAh·g-1、450mAh·g-1Capacity.
Embodiment 4
A kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping, the specific steps are as follows:
(1) cobalt nitrate, nickel nitrate are dissolved in glycerine and the mixed solution of isopropyl alcohol, Ni in mixed solution
(NO3)2Concentration be 0.01mol, the volume ratio of glycerine and isopropanol is 1:7, and Ni ion: the molar ratio of Co ion is 1:2,
React 6h at 140 DEG C loaded on reaction kettle after mixing evenly, be cooled to room temperature, wash, dry after obtain precursor powder；
(2) rubidium carbonate will be continuously added in precursor powder, the molar ratio of Rb element and Co element is 1:5, is milled uniformly
Afterwards under argon atmosphere, 700 DEG C of calcining 4h are warming up to the rate of 2.5 DEG C/min, after temperature drops to room temperature, after milling uniformly
Obtain the cobalt acid nickel negative electrode material of rubidium doping.
Above-mentioned rubidium cation doping acid nickel electrode material is assembled into battery, is tested with blue electric system, 500 μ A/mg's
Under current density after 500 circle of circulation, still there is 715mAhg-1Capacity, capacity retention ratio is about 73%；Then respectively with
The current density test high rate performance of 200 μ A/mg, 500 μ A/mg, 1000 μ A/mg and 2000 μ A/mg, respectively obtain
804mAh·g-1、734mAh·g-1、664mAh·g-1、456mAh·g-1Capacity.
The above is only the specific embodiment of the application, it is noted that for the ordinary skill people of the art
For member, under the premise of not departing from the application principle, several improvements and modifications can also be made, these improvements and modifications are also answered
It is considered as the protection scope of the application.
Claims (10)
1. a kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping, it is characterised in that key step is as follows:
Step 1: soluble cobalt, soluble nickel salt being dissolved in the mixed solution of glycerine and isopropanol, after mixing evenly
Loaded on reaction kettle occur hydro-thermal reaction, be cooled to room temperature, be centrifuged, wash, dry after obtain precursor powder；
Step 2: rubidium salt will be added in precursor powder, calcined under protective gas atmosphere after milling uniformly, drop to room to temperature
Wen Hou, to get the cobalt acid nickel negative electrode material adulterated to rubidium after milling uniformly.
2. a kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping according to claim 1, it is characterised in that step 1
The concentration of nickel ion in mixed solution is 0.01-0.1mol/L, Ni2+: Co2+Molar ratio be 1:2.
3. a kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping according to claim 1, it is characterised in that step 1
The volume ratio of middle glycerine and isopropanol is 1:10-1:5.
4. a kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping according to claim 1, it is characterised in that step 1
Middle soluble cobalt is cobalt nitrate, cobaltous sulfate, cobalt chloride, any one in cobalt acetate, and soluble nickel salt is nickel nitrate, sulfuric acid
Nickel, nickel chloride, any one in nickel acetate.
5. a kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping according to claim 1, it is characterised in that step 1
Middle hydrothermal temperature is 140-180 DEG C, reaction time 6-12h.
6. a kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping according to claim 1, it is characterised in that step 1
Middle drying temperature is 60-80 DEG C, drying time 6-12h.
7. a kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping according to claim 1, it is characterised in that step 2
In, the molar ratio of cobalt element is 1:10-1:5 in the rubidium element and soluble cobalt in rubidium salt.
8. a kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping according to claim 1, it is characterised in that step 2
In, rubidium salt is rubidium carbonate, rubidium hydroxide, any one in rubidium chloride.
9. a kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping according to claim 1, it is characterised in that step 2
In, protective gas is nitrogen or inert gas.
10. a kind of preparation method of the cobalt acid nickel negative electrode material of rubidium doping according to claim 1, it is characterised in that step
In 2, calcination process are as follows: under protective gas protection, risen to the heating rate of 1-5 DEG C/min in 550-850 DEG C of calcining 4-8h.
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| CN114512662A (en) * | 2022-03-02 | 2022-05-17 | 芜湖天弋能源科技有限公司 | Lithium ion battery anode material and preparation method thereof, and lithium ion battery |
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Application publication date: 20191015 |