CN103413918B - A kind of synthetic method of anode material for lithium ion battery cobalt phosphate lithium - Google Patents
A kind of synthetic method of anode material for lithium ion battery cobalt phosphate lithium Download PDFInfo
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Abstract
The present invention discloses a kind of synthetic method of lithium ion battery positive pole material phosphoric acid cobalt lithium.Namely first cobalt acetate dissolving is made into the cobalt acetate aqueous solution in deionized water; Lithium hydroxide and sucrose dissolved are made into lithium hydroxide/sucrose mixed solution in deionized water; Phosphoric acid is added deionized water and is made into phosphoric acid solution; Then gained phosphoric acid solution is joined the cobalt acetate aqueous solution of gained, obtain claret emulsion, after stirring, lithium hydroxide/sucrose mixed solution is added in the red emulsion of above-mentioned obtained wine thereby, stirs, add nitric acid, obtain precursor aqueous solution; And then gained precursor aqueous solution is carried out spraying dry under stirring, obtain cobalt phosphate lithium powder presoma; Finally gained cobalt phosphate lithium powder presoma is put at control temperature is 600-750 DEG C and carry out vacuum calcining 16-26h, obtain the lithium ion battery positive pole material phosphoric acid cobalt lithium of spherical porous structure, height ratio capacity.
Description
Technical field
The present invention relates to a kind of synthetic method of anode material for lithium ion battery cobalt phosphate lithium material, particularly relate to a kind of synthetic method of anode material for lithium ion battery cobalt phosphate lithium material of spherical porous structure.
Background technology
Based on current serious energy crisis and pollution problem, countries in the world are paid much attention to Development of EV, also development electric motor car are classified as important development direction in China's 863 Program.As the research of the electrokinetic cell of onboard power, become the Main Bottleneck of power vehicle development.Prevailing battery system is lithium ion battery and nickel-hydrogen cell in the market, and they instead of nickel-cadmium cell and the lead-acid battery system of transmission gradually.Lithium ion battery because of its high voltage, high power capacity, have extended cycle life and the feature such as security performance is good, by extensive concern.
Along with the fast development of lithium ion battery, the anode material for lithium-ion batteries that high power capacity, security performance are good, with low cost becomes the focus of people's research.A.K.Padhi in 1997 etc. have studied the lithium ion battery of LiMPO4 material as anode material for lithium-ion batteries of use olivine structural at first, find that it has the advantages such as the specific capacity that security performance is good, cyclical stability is high, higher, cause the concern of many researchers.Wherein LiCoPO
4have orderly olivine-type structure, belong to rhombic system, space group is Pnmb, and cell parameter is a=5.992, b=10.202, c=4.669.At LiCoPO
4in crystal, oxygen atom is close heap hexagonal structure, and what phosphorus atoms occupied is tetrahedral interstice, and what lithium atom and cobalt atom occupied is octahedral interstice.The octahedra CoO of common edge
6c direction of principal axis passes through PO
4tetrahedron connects into chain structure.This cobalt phosphate lithium has highly stable lithium ion deintercalation behavior.LiCoPO
4the theoretical discharge specific capacity of positive electrode is 167mAh/g, and the electrode potential of relative lithium is 4.8V, is expected to become high power capacity of new generation, high-tension positive electrode.
The method of current synthesis cobalt phosphate lithium mainly contains high temperature solid phase synthesis, Low Temperature Solid-Phase synthetic method, microwave process for synthesizing, sol-gel synthesis method, hydrothermal synthesis method etc.
High temperature solid phase synthesis is a kind of method the most conventional in industry preparation, and the method is by reactant by measuring than mixed grinding, and compressing tablet, is then placed in high temperature furnace and sinters at air or inert gas atmosphere.As (J.PowerSources, 2005,144 (1): 226-230) such as J.Wolfenstine adopt high temperature solid-state method, with Li
2cO
3, CoC
2o
42H
2o and NH
4h
2pO
4for raw material, first at 375 DEG C, process 20h, after cooling in argon gas atmosphere stove, calcine 48h at 775 DEG C and obtain end product.Result of study shows to obtain complete degree of crystallinity, the crystal morphology of rule and the LiCoPO of uniform particle diameter
4.Charge-discharge test shows, under 0.2C multiplying power, first discharge specific capacity is 100mAh/g.
Low-temperature solid-phase method is a kind of solvent-free participation, reactant is two or more solid matters, and at room temperature can obtains the presoma of product, is then prepared the method for product by calcining presoma.Low-temperature solid-phase method has feature simple to operate, also has the advantage of soft chemical method concurrently, greatly reduces solid phase reaction temperature simultaneously, and product is significantly improved compared to conventional high-temperature solid phase method on properity and exterior appearance.NataliaN.Bramnik etc. (JSolidStateElectrochem, 2004,8:558-564) are with (NH
4)
2hPO
4, CoCl
2be raw material with LiOH, at 600 DEG C, calcine 24h obtain product.Adopt XRD and SEM and electrochemical property test to show, obtain crystal formation complete, uniform particle sizes pure phase LiCoPO
4, under 0.5C, record first discharge specific capacity is 125mAh/g, is 75% of theoretical capacity.
Microwave heating utilizes heated material to absorb microwave, causes the polarization of molecule and atom, make molecule and atom produce violent friction, cause the rising of heated material temperature.Compared with traditional heating mode, it is fast that microwave heating method has heating rate, the advantage of homogeneous heating.(the ElectrochemistryCommunications such as H.H.Li, 2009,11:95-98), with CH3COOLi, (CH3COO) 2Co and (NH4) 2HPO4 is raw material, first preliminary treatment 2h at 350 DEG C, then heats 11min and obtains LiCoPO4 under the microwave of 2.45GHz, 700W.Test shows, the sample crystallinity of synthesis is good, without dephasign.At constant current 0.5C, voltage range is under 3.0 ~ 5.1V, and the battery first discharge specific capacity of this material is 93.3mAh/g, differs too large with theoretical capacity.
Hydro thermal method is a kind of method preparing superfine powder that development in recent years is got up, obtained product powder has that grain development is complete, particle size range narrowly distributing, material thing are mutually homogeneous, better crystallinity degree, purity advantages of higher, is subject to the attention of vast battery material researcher.(the RareMetals such as ZhaoYujuan, 2009,28 (2): 117-121), hydrothermal synthesis method is adopted to successfully synthesize the LiCoPO4 of rhombic system, electrochemical property test shows, adopt the material of the method synthesis under 0.5C multiplying power, initial charge specific capacity is 154mAh/g, but first discharge specific capacity is only 65mAh/g, distance applications also has very large distance.
By analyzing above and can finding, solid phase method sintering time is long, energy consumption is large, production efficiency is low, and the domain size distribution of product is wayward, and uniformity, consistency, reappearance are poor.The product of microwave process for synthesizing, hydrothermal synthesis method, general particle diameter is comparatively large, and be unfavorable for the migration of lithium ion, chemical property is undesirable.
In sum, all there is the specific capacity not high-technology problem of the cobalt phosphate lithium positive electrode of final gained in the synthetic method of above-mentioned various cobalt phosphate lithium positive electrodes.
Summary of the invention
The object of the invention is specific capacity in order to solve above-mentioned cobalt phosphate lithium positive electrode not high-technology problem etc. and provide a kind of synthetic method of lithium ion battery positive pole material phosphoric acid cobalt lithium, the specific capacity of the lithium ion battery positive pole material phosphoric acid cobalt lithium of the final gained of the method is higher.
Technical scheme of the present invention
A synthetic method for lithium ion anode material cobalt phosphate lithium, namely with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose etc. for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 38-46 part
Cobalt acetate 224-274 part
Phosphatase 11 05-126 part
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
(1), the cobalt acetate of 224-274 part is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 38-46 part and 15 parts is made into lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The phosphoric acid of 105-126 part is added 100 parts of deionized waters and be made into phosphoric acid solution;
(2), the phosphoric acid solution of step (1) gained is joined under stirring in the cobalt acetate aqueous solution of step (1) gained, obtain claret emulsion, after stirring, the lithium hydroxide of step (1) gained/sucrose mixed solution is joined in the claret emulsion of above-mentioned gained, stir, add the nitric acid of 15 parts, obtain precursor aqueous solution;
(3), by the precursor aqueous solution of step (2) gained under stirring, control leaving air temp is 105 DEG C and carries out spraying dry, obtains the cobalt phosphate lithium powder presoma of porous spherical structure;
(4), cobalt phosphate lithium powder presoma control temperature in vacuum furnace of the porous spherical structure of step (3) gained is 600-750 DEG C at carry out vacuum calcining 16-26h, obtain lithium ion battery positive pole material phosphoric acid cobalt lithium.
The shape characteristic of the lithium ion battery anode material lithium iron phosphate particle spherical in shape of above-mentioned gained, diameter is at 2-5 micron, this spheric granules is made up of more tiny cobalt phosphate lithium nano particle, the size of these nano particles is in 200-300 nanometer, around nano particle, there is the hole of obvious nano-scale, namely the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained is spherical porous structure, these nano apertures, as the capillary channel of electrolyte and material exchange lithium ion, thus the chemical property of cobalt phosphate lithium can be improved.
The averaged discharge specific capacity of the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained is 138-143mAh/g, initial charge specific capacity is 173-190mAh/g, first discharge specific capacity is 140-151mAh/g, circulation coulombic efficiency 75.8-84.4% first, 96.7-98.3% is compared in charging constant current, electric discharge mean voltage 4.70-4.75V, 4.5V is with upper mounting plate rate 92.2-93.4%.
beneficial effect of the present invention
The synthetic method of a kind of lithium ion anode material cobalt phosphate lithium of the present invention is spraying cracking process due to what adopt.Compared with prior art, after spraying cracking, obtain presenting of lithium ion anode material cobalt phosphate lithium product spherical, this spheric granules is made up of the nanometer cobalt phosphate lithium crystal grain of 100-200 nanosized, the cobalt phosphate lithium particle of this nano-scale decreases the distance of lithium ion mobility, is conducive to improving the specific capacity obtaining cobalt phosphate lithium material.Meanwhile, owing to there is gas purging in Pintsch process process, in the cobalt phosphate lithium positive electrode of acquisition, be present in the fine hole of a large amount of nanometers.The existence of this nano aperture, for the storage of electrolyte provides space, providing necessary capillary channel for carrying out lithium ion exchanged fast, being conducive to the multiplying power property improving material.
Further, after the lithium ion battery positive pole material phosphoric acid cobalt lithium of the spherical porous structure of the synthetic method gained of lithium ion anode material cobalt phosphate lithium of the present invention is assembled into button cell, loop test is carried out under 0.5C, averaged discharge specific capacity is 138-143mAh/g, initial charge specific capacity is 173-190mAh/g, first discharge specific capacity is 140-151mAh/g, circulation coulombic efficiency 75.8-84.4% first, 96.7-98.3% is compared in charging constant current, electric discharge mean voltage 4.70-4.75V, 4.5V is with upper mounting plate rate 92.2-93.4%.These test results show, the lithium ion anode material cobalt phosphate lithium of above-mentioned spraying cracking synthetic method gained has good electrochemical properties, are expected to apply in electrokinetic cell field.
Accompanying drawing explanation
The XRD collection of illustrative plates of the lithium ion battery anode material lithium iron phosphate of Fig. 1, embodiment 1 gained;
The SEM figure of the lithium ion battery anode material lithium iron phosphate of Fig. 2, embodiment 1 gained;
The chemical property collection of illustrative plates of the lithium ion battery anode material lithium iron phosphate of Fig. 3, embodiment 1 gained.
Embodiment
Below by embodiment, also the present invention is described in detail by reference to the accompanying drawings, but do not limit the present invention.
The preparation of battery and the method for testing of chemical property
1., the preparation of battery anode slice
The lithium ion battery positive pole material phosphoric acid cobalt lithium obtained, conductive carbon powder, organic binder bond Kynoar (PVDF) are calculated according to mass ratio, i.e. lithium ion battery positive pole material phosphoric acid cobalt lithium: conductive carbon powder: organic binder bond Kynoar is obtain mixed powder after the ratio of 92:3:5 mixes, by this mixed powder 10 grams, add organic solvent 1-METHYLPYRROLIDONE (NMP) 12 grams, slurry is formed after abundant stirring, be coated on aluminium foil surface, after oven dry, repeatedly rolling, obtains battery anode slice;
2., battery assembling and performance test
2016 type half-cell assessments are used to obtain the chemical property of cobalt phosphate lithium.The battery anode slice that rolling is good is stamped into the disk of diameter 12 millimeters, after its quality of precise, the cobalt phosphate lithium quality calculated in pole piece is formed according to formula, use the import celgard barrier film of diameter 19 millimeters, use the metal lithium sheet of diameter 15 millimeters as negative pole, being assembled in glove box can test battery.
The specific capacity test of battery:
Wuhan Lan electricity company cell tester (Land2000) is used to carry out.Repeatedly loop test is carried out under 0.5C condition.
Spray drying device used in various embodiments of the present invention is the MOBILEMINOR disk–type spray dryer that Shanghai Shi Yuan biological plant engineering company produces.
embodiment 1
A synthetic method for lithium ion battery positive pole material phosphoric acid cobalt lithium, with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose and deionized water for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 42 parts
Cobalt acetate 249 parts
Phosphatase 11 15 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
(1), the cobalt acetate of 249 parts is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 42 parts and 15 parts is made into lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The deionized water that the phosphoric acid of 115 parts adds 100 parts is made into phosphoric acid solution;
(2), by the phosphoric acid solution of step (1) gained, the cobalt acetate aqueous solution of step (1) gained is joined under stirring, obtain claret emulsion, after stirring, the lithium hydroxide of step (1) gained/sucrose mixed solution is joined in this claret emulsion of gained, stir, then add the nitric acid of 15 parts and stir, obtaining precursor aqueous solution;
(3), by the precursor aqueous solution of step (2) gained under stirring, control leaving air temp is 105 DEG C and carries out spraying dry, obtains the cobalt phosphate lithium powder presoma of porous spherical;
(4), by the cobalt phosphate lithium powder presoma of the porous spherical of step (3) gained be placed in quartz ampoule, and then quartz ampoule is placed in vacuum furnace, control temperature is carry out vacuum calcining 21h at 680 DEG C, obtains lithium ion battery positive pole material phosphoric acid cobalt lithium.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained is detected by X-ray diffractometer (XRD, Rigaku Rigaku), and the XRD test result of gained is as Fig. 1.Can find out in Fig. 1 that diffraction maximums all in this collection of illustrative plates can be demarcated as the diffraction maximum of cobalt phosphate lithium, namely do not have the peak position of other materials to occur, show that the final material of the synthetic method gained of above-mentioned lithium ion battery positive pole material phosphoric acid cobalt lithium is pure phase cobalt phosphate lithium.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained, use ESEM (SEM, NEC 6700F) to carry out Shape measure, the SEM observed result of gained is as Fig. 2.As can be seen from Figure 2, the lithium ion battery anode material lithium iron phosphate of gained presents the shape characteristic of spheric granules, and diameter is at 2-5 micron.This spheric granules is made up of more tiny cobalt phosphate lithium nano particle, and the size of these nano particles is in 200-300 nanometer.Around nano particle, there is the hole of obvious nano-scale, namely the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained is spherical porous structure, these nano apertures, as the capillary channel of electrolyte and material exchange lithium ion, thus the chemical property of cobalt phosphate lithium can be improved.
Use half-cell method to be assembled into button-shaped 2016 batteries the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained to test the charge-discharge performance of this battery under the multiplying power of 0.5C, front 5 discharge and recharge results are as Fig. 3, as can be seen from Figure 3, averaged discharge specific capacity is 140mAh/g, initial charge specific capacity is 190mAh/g, first discharge specific capacity is 144mAh/g, circulation coulombic efficiency 75.8% first, charging constant current is than 97.4%, electric discharge mean voltage 4.72V, 4.5V is with upper mounting plate rate 92.2%.Show thus, the lithium ion battery anode material lithium iron phosphate of above-mentioned synthetic method gained has good electrochemical properties, can apply in electrokinetic cell field.
embodiment 2
A synthetic method for lithium ion battery positive pole material phosphoric acid cobalt lithium, namely with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose and deionized water for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 38 parts
Cobalt acetate 224 parts
Phosphatase 11 05 part
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
(1), the cobalt acetate of 224 parts is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 38 parts and 15 parts is made into lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The deionized water that the phosphoric acid of 105 parts adds 100 parts is made into phosphoric acid solution;
(2), by the phosphoric acid solution of step (1) gained, the cobalt acetate aqueous solution of step (1) gained is joined under stirring, obtain claret emulsion, after stirring, the lithium hydroxide of step (1) gained/sucrose mixed solution is joined in the claret emulsion of gained, stir, then add the nitric acid of 15 parts and stir, obtaining precursor aqueous solution;
(3), by the precursor aqueous solution of step (2) gained under stirring, control leaving air temp is 105 DEG C and carries out spraying dry, obtains the cobalt phosphate lithium powder presoma of porous spherical;
(4), by the cobalt phosphate lithium powder presoma of the porous spherical of step (3) gained be placed in quartz ampoule, and then quartz ampoule is placed in vacuum furnace, control temperature is carry out vacuum calcining 26h at 600 DEG C, obtains lithium ion battery positive pole material phosphoric acid cobalt lithium.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses X-ray diffractometer (XRD, Rigaku Rigaku) test, result is similar to Fig. 1, do not find the diffraction maximum of other thing phases, show that the final material of the synthetic method gained of above-mentioned lithium ion battery positive pole material phosphoric acid cobalt lithium is pure phase cobalt phosphate lithium material.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses ESEM (SEM, NEC 6700F) to carry out SEM observation, and result is similar to Fig. 2, has the internal structure of spheric granules external appearance characteristic and nanoporous equally.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained makes battery pole piece according to the method for embodiment 1, under the multiplying power of 0.5C, the charge-discharge performance of this battery is tested, result shows, the averaged discharge specific capacity of the lithium ion battery positive pole material phosphoric acid cobalt lithium of gained is 143mAh/g, initial charge specific capacity is 182mAh/g, first discharge specific capacity is 148mAh/g, circulation coulombic efficiency 81.3% first, charging constant current is than 97.8%, electric discharge mean voltage 4.75V, 4.5V is with upper mounting plate rate 93.1%.This shows that the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained has good electrochemical properties.
embodiment 3
A synthetic method for lithium ion battery positive pole material phosphoric acid cobalt lithium, namely with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose and deionized water for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 46 parts
Cobalt acetate 274 parts
Phosphatase 11 26 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
(1), the cobalt acetate of 274 parts is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 46 parts and 15 parts is mixed with lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The deionized water that the phosphoric acid of 126 parts adds 100 parts is made into phosphoric acid solution;
(2), by the phosphoric acid solution of step (1) gained, the cobalt acetate aqueous solution of step (1) gained is joined under stirring, obtain claret emulsion, after stirring, the lithium hydroxide of step (1) gained/sucrose mixed solution is joined in the claret emulsion of gained, stir, then add the nitric acid of 15 parts and stir, obtaining precursor aqueous solution;
(3), by the precursor aqueous solution of step (2) gained under stirring, control leaving air temp is 105 DEG C and carries out spraying dry, obtains the cobalt phosphate lithium powder presoma of porous spherical;
(4), by the cobalt phosphate lithium powder presoma of the porous spherical of step (3) gained be placed in quartz ampoule, and then quartz ampoule is placed in vacuum furnace, control temperature is carry out vacuum calcining 16h at 750 DEG C, obtains lithium ion battery positive pole material phosphoric acid cobalt lithium.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses X-ray diffractometer (XRD, Rigaku Rigaku) test, result is similar to Fig. 1, do not find the diffraction maximum of other thing phases, show that the final material of the synthetic method gained of above-mentioned lithium ion battery positive pole material phosphoric acid cobalt lithium is pure phase cobalt phosphate lithium material.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses ESEM (SEM, NEC 6700F) to carry out SEM observation, and result is similar to Fig. 2, has the internal structure of spheric granules external appearance characteristic and nanoporous equally.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained makes battery pole piece according to the method for embodiment 1, under the multiplying power of 0.5C, the charge-discharge performance of this battery is tested, result shows, the averaged discharge specific capacity of the lithium ion battery positive pole material phosphoric acid cobalt lithium of gained is 138mAh/g, initial charge specific capacity is 178mAh/g, first discharge specific capacity is 141mAh/g, circulation coulombic efficiency 79.2% first, charging constant current is than 97.6%, electric discharge mean voltage 4.74V, 4.5V is with upper mounting plate rate 92.9%.This shows that the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained has good electrochemical properties.
embodiment 4
A synthetic method for lithium ion battery positive pole material phosphoric acid cobalt lithium, namely with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose and deionized water for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 46 parts
Cobalt acetate 224 parts
Phosphatase 11 15 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
(1), the cobalt acetate of 224 parts is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 46 parts and 15 parts is made into lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The deionized water that the phosphoric acid of 115 parts adds 100 parts is made into phosphoric acid solution;
(2), by the phosphoric acid solution of step (1) gained, the cobalt acetate aqueous solution of step (1) gained is joined under stirring, obtain claret emulsion, after stirring, the lithium hydroxide of step (1) gained/sucrose mixed solution is joined in the claret emulsion of gained, stir, then add the nitric acid of 15 parts and stir, obtaining precursor aqueous solution;
(3), by the precursor aqueous solution of step (2) gained under stirring, control leaving air temp is 105 DEG C and carries out spraying dry, obtains the cobalt phosphate lithium powder presoma of porous spherical;
(4), by the cobalt phosphate lithium powder presoma of the porous spherical of step (3) gained be placed in quartz ampoule, and then quartz ampoule is placed in vacuum furnace, control temperature is carry out vacuum calcining 26h at 680 DEG C, obtains lithium ion battery positive pole material phosphoric acid cobalt lithium.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses X-ray diffractometer (XRD, Rigaku Rigaku) test, result is similar to Fig. 1, do not find the diffraction maximum of other thing phases, show that the final material of the synthetic method gained of above-mentioned lithium ion battery positive pole material phosphoric acid cobalt lithium is pure phase cobalt phosphate lithium material.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses ESEM (SEM, NEC 6700F) to carry out SEM observation, and result is similar to Fig. 2, has the internal structure of spheric granules external appearance characteristic and nanoporous equally.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained makes battery pole piece according to the method for embodiment 1, under the multiplying power of 0.5C, the charge-discharge performance of this battery is tested, result shows, the averaged discharge specific capacity of the lithium ion battery positive pole material phosphoric acid cobalt lithium of gained is 142mAh/g, initial charge specific capacity is 181mAh/g, first discharge specific capacity is 147mAh/g, circulation coulombic efficiency 81.2% first, charging constant current is than 98.2%, electric discharge mean voltage 4.70V, 4.5V is with upper mounting plate rate 93.4%.This shows that the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained has good electrochemical properties.
embodiment 5
A synthetic method for lithium ion battery positive pole material phosphoric acid cobalt lithium, namely with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose and deionized water for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 38 parts
Cobalt acetate 249 parts
Phosphatase 11 26 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
(1), the cobalt acetate of 249 parts is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 38 parts and 15 parts is made into lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The deionized water that the phosphoric acid of 126 parts adds 100 parts is made into phosphoric acid solution;
(2), by the phosphoric acid solution of step (1) gained, the cobalt acetate aqueous solution of step (1) gained is joined under stirring, obtain claret emulsion, after stirring, the lithium hydroxide of step (1) gained/sucrose mixed solution is joined in the claret emulsion of gained, stir, then add the nitric acid of 15 parts and stir, obtaining precursor aqueous solution;
(3), by the precursor aqueous solution of step (2) gained under stirring, control leaving air temp is 105 DEG C and carries out spraying dry, obtains the cobalt phosphate lithium powder presoma of porous spherical;
(4), by the cobalt phosphate lithium powder presoma of the porous spherical of step (3) gained be placed in quartz ampoule, and then quartz ampoule is placed in vacuum furnace, control temperature is carry out vacuum calcining 21h at 750 DEG C, obtains lithium ion battery positive pole material phosphoric acid cobalt lithium.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses X-ray diffractometer (XRD, Rigaku Rigaku) test, result is similar to Fig. 1, do not find the diffraction maximum of other thing phases, show that the final material of the synthetic method gained of above-mentioned lithium ion battery positive pole material phosphoric acid cobalt lithium is pure phase cobalt phosphate lithium material.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses ESEM (SEM, NEC 6700F) to carry out SEM observation, and result is similar to Fig. 2, has the internal structure of spheric granules external appearance characteristic and nanoporous equally.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained makes battery pole piece according to the method for embodiment 1, under the multiplying power of 0.5C, the charge-discharge performance of this battery is tested, result shows, the averaged discharge specific capacity of the lithium ion battery positive pole material phosphoric acid cobalt lithium of gained is 136mAh/g, initial charge specific capacity is 184mAh/g, first discharge specific capacity is 140mAh/g, circulation coulombic efficiency 76.1% first, charging constant current is than 96.7%, electric discharge mean voltage 4.67V, 4.5V is with upper mounting plate rate 92.4%.This shows that the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained has good electrochemical properties.
embodiment 6
A synthetic method for lithium ion battery positive pole material phosphoric acid cobalt lithium, namely with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose and deionized water for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 42 parts
Cobalt acetate 274 parts
Phosphatase 11 05 part
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
Specifically comprise the steps:
(1), the cobalt acetate of 274 parts is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 42 parts and 15 parts is made into lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The deionized water that the phosphoric acid of 105 parts adds 100 parts is made into phosphoric acid solution;
(2), by the phosphoric acid solution of step (1) gained, the cobalt acetate solution of step (1) gained is joined under stirring, obtain claret emulsion, after stirring, the lithium hydroxide of step (1) gained/sucrose mixed solution is joined in the claret emulsion of gained, stir, then add the nitric acid of 15 parts and stir, obtaining precursor aqueous solution;
(3), by the precursor aqueous solution of step (2) gained under stirring, control leaving air temp is 105 DEG C and carries out spraying dry, obtains the cobalt phosphate lithium powder presoma of porous spherical;
(4), by the cobalt phosphate lithium powder presoma of the porous spherical of step (3) gained be placed in quartz ampoule, and then quartz ampoule is placed in vacuum furnace, control temperature is carry out vacuum calcining 21h at 600 DEG C, obtains lithium ion battery positive pole material phosphoric acid cobalt lithium.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses X-ray diffractometer (XRD, Rigaku Rigaku) test, result is similar to Fig. 1, do not find the diffraction maximum of other thing phases, show that the final material of the synthetic method gained of above-mentioned lithium ion battery positive pole material phosphoric acid cobalt lithium is pure phase cobalt phosphate lithium material.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses ESEM (SEM, NEC 6700F) to carry out SEM observation, and result is similar to Fig. 2, has the internal structure of spheric granules external appearance characteristic and nanoporous equally.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained makes battery pole piece according to the method for embodiment 1, under the multiplying power of 0.5C, the charge-discharge performance of this battery is tested, result shows, the averaged discharge specific capacity of the lithium ion battery positive pole material phosphoric acid cobalt lithium of gained is 142mAh/g, initial charge specific capacity is 176mAh/g, first discharge specific capacity is 148mAh/g, circulation coulombic efficiency 84.1% first, charging constant current is than 97.1%, electric discharge mean voltage 4.73V, 4.5V is with upper mounting plate rate 92.8%.This shows that the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained has good electrochemical properties.
embodiment 7
A synthetic method for lithium ion battery positive pole material phosphoric acid cobalt lithium, namely with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose and deionized water for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 38 parts
Cobalt acetate 249 parts
Phosphatase 11 05 part
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
(1), the cobalt acetate of 249 parts is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 38 parts and 15 parts is made into lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The deionized water that the phosphoric acid of 105 parts adds 100 parts is made into phosphoric acid solution;
(2), by the phosphoric acid solution of step (1) gained, the cobalt acetate aqueous solution of step (1) gained is joined under stirring, obtain claret emulsion, after stirring, the lithium hydroxide of step (1) gained/sucrose mixed solution is joined in the claret emulsion of gained, stir, then add the nitric acid of 15 parts and stir, obtaining precursor aqueous solution;
(3), by the precursor aqueous solution of step (2) gained under stirring, control leaving air temp is 105 DEG C and carries out spraying dry, obtains the cobalt phosphate lithium powder presoma of porous spherical;
(4), by the cobalt phosphate lithium powder presoma of the porous spherical of step (3) gained be placed in quartz ampoule, and then quartz ampoule is placed in vacuum furnace, control temperature is carry out vacuum calcining 16h at 750 DEG C, obtains lithium ion battery positive pole material phosphoric acid cobalt lithium.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses X-ray diffractometer (XRD, Rigaku Rigaku) test, result is similar to Fig. 1, do not find the diffraction maximum of other thing phases, show that the final material of the synthetic method gained of above-mentioned lithium ion battery positive pole material phosphoric acid cobalt lithium is pure phase cobalt phosphate lithium material.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses ESEM (SEM, NEC 6700F) to carry out SEM observation, and result is similar to Fig. 2, has the internal structure of spheric granules external appearance characteristic and nanoporous equally.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained makes battery pole piece according to the method for embodiment 1, under the multiplying power of 0.5C, the charge-discharge performance of this battery is tested, result shows, the averaged discharge specific capacity of the lithium ion battery positive pole material phosphoric acid cobalt lithium of gained is 140mAh/g, initial charge specific capacity is 173mAh/g, first discharge specific capacity is 146mAh/g, circulation coulombic efficiency 84.4% first, charging constant current is than 98.3%, electric discharge mean voltage 4.68V, 4.5V is with upper mounting plate rate 93.2%.This shows that the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained has good electrochemical properties.
embodiment 8
A synthetic method for lithium ion battery positive pole material phosphoric acid cobalt lithium, namely with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose and deionized water for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 38 parts
Cobalt acetate 249 parts
Phosphatase 11 26 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
Specifically comprise the steps:
(1), the cobalt acetate of 249 parts is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 38 parts and 15 parts is made into lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The deionized water that the phosphoric acid of 126 parts adds 100 parts is made into phosphoric acid solution;
(2), by the phosphoric acid solution of step (1) gained, the cobalt acetate aqueous solution of step (1) gained is joined under stirring, obtain claret emulsion, after stirring, the lithium hydroxide of step (1) gained/sucrose mixed solution is joined in the claret emulsion of gained, stir, then add the nitric acid of 15 parts and stir, obtaining precursor aqueous solution;
(3), by the precursor aqueous solution of step (2) gained under stirring, control leaving air temp is 105 DEG C and carries out spraying dry, obtains the cobalt phosphate lithium powder presoma of porous spherical;
(4), the cobalt phosphate lithium powder presoma of the porous spherical of step (1) gained is placed in quartz ampoule, and then quartz ampoule is placed in vacuum furnace, control temperature is carry out high-temperature vacuum calcining 16h at 600 DEG C, obtains lithium ion battery positive pole material phosphoric acid cobalt lithium.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses X-ray diffractometer (XRD, Rigaku Rigaku) test, result is similar to Fig. 1, do not find the diffraction maximum of other thing phases, show that the final material of the synthetic method gained of above-mentioned lithium ion battery positive pole material phosphoric acid cobalt lithium is pure phase cobalt phosphate lithium material.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses ESEM (SEM, NEC 6700F) to carry out SEM observation, and result is similar to Fig. 2, has the internal structure of spheric granules external appearance characteristic and nanoporous equally.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained makes battery pole piece according to the method for embodiment 1, under the multiplying power of 0.5C, the charge-discharge performance of this battery is tested, result shows, the averaged discharge specific capacity of the lithium ion battery positive pole material phosphoric acid cobalt lithium of gained is 143mAh/g, initial charge specific capacity is 178mAh/g, first discharge specific capacity is 151mAh/g, circulation coulombic efficiency 80.3% first, charging constant current is than 97.8%, electric discharge mean voltage 4.72V, 4.5V is with upper mounting plate rate 92.6%.This shows that the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained has good electrochemical properties.
embodiment 9
A synthetic method for lithium ion battery positive pole material phosphoric acid cobalt lithium, namely with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose and deionized water for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 42 parts
Cobalt acetate 249 parts
Phosphatase 11 15 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
(1), the cobalt acetate of 249 parts is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 42 parts and 15 parts is made into lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The deionized water that the phosphoric acid of 115 parts adds 100 parts is made into phosphoric acid solution;
(2), by the phosphoric acid solution of step (1) gained, the cobalt acetate aqueous solution of step (1) gained is joined under stirring, obtain claret emulsion, after stirring, the lithium hydroxide of step (1) gained/sucrose mixed solution is joined in the claret emulsion of gained, stir, then add the nitric acid of 15 parts and stir, obtaining precursor aqueous solution;
(3), by the precursor aqueous solution of step (2) gained under stirring, control leaving air temp is 105 DEG C and carries out spraying dry, obtains the cobalt phosphate lithium powder presoma of porous spherical;
(4), by the cobalt phosphate lithium powder presoma of the porous spherical of step (3) gained be placed in quartz ampoule, and then quartz ampoule is placed in vacuum furnace, control temperature is carry out vacuum calcining 26h at 750 DEG C, obtains lithium ion battery positive pole material phosphoric acid cobalt lithium.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses X-ray diffractometer (XRD, Rigaku Rigaku) test, result is similar to Fig. 1, do not find the diffraction maximum of other thing phases, show that the final material of the synthetic method gained of above-mentioned lithium ion battery positive pole material phosphoric acid cobalt lithium is pure phase cobalt phosphate lithium material.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained uses ESEM (SEM, NEC 6700F) to carry out SEM observation, and result is similar to Fig. 2, has the internal structure of spheric granules external appearance characteristic and nanoporous equally.
The lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained makes battery pole piece according to the method for embodiment 1, under the multiplying power of 0.5C, the charge-discharge performance of this battery is tested, result shows, the averaged discharge specific capacity of the lithium ion battery positive pole material phosphoric acid cobalt lithium of gained is 138mAh/g, initial charge specific capacity is 183mAh/g, first discharge specific capacity is 151mAh/g, circulation coulombic efficiency 82.5% first, charging constant current is than 97.1%, electric discharge mean voltage 4.75V, 4.5V is with upper mounting plate rate 92.6%.This shows that the lithium ion battery positive pole material phosphoric acid cobalt lithium of above-mentioned gained has good electrochemical properties.
In sum, the synthetic method of a kind of lithium ion battery positive pole material phosphoric acid cobalt lithium of the present invention, namely using cobalt acetate, lithium hydroxide, phosphoric acid etc. as raw material, the lithium ion battery positive pole material phosphoric acid cobalt lithium obtained by the step such as spraying dry and vacuum calcining is pure phase cobalt phosphate.And this synthetic method operating process is simple.The lithium ion battery positive pole material phosphoric acid cobalt lithium of gained presents porous spherical structure, and pore size is even, and pattern is unified, for lithium ion exchanged provides capillary channel.Electrochemical property test structure shows, this lithium ion battery positive pole material phosphoric acid cobalt lithium has good chemical property, can be applied in electrokinetic cell field.
Foregoing be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.
Claims (10)
1. a synthetic method for lithium ion battery positive pole material phosphoric acid cobalt lithium, is characterized in that, with lithium hydroxide, cobalt acetate, phosphoric acid, nitric acid, sucrose and deionized water for raw material, described raw material is calculated according to the mass fraction, its composition and content as follows:
Lithium hydroxide 38-46 part
Cobalt acetate 224-274 part
Phosphatase 11 05-126 part
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Its synthetic method specifically comprises the steps:
1) cobalt acetate of 224-274 part is dissolved in the deionized water of 300 parts and is made into the cobalt acetate aqueous solution;
The sucrose dissolved of the lithium hydroxide of 38-46 part and 15 parts is made into lithium hydroxide/sucrose mixed solution in the deionized water of 250 parts;
The phosphoric acid of 105-126 part is added 100 parts of deionized waters and be made into phosphoric acid solution;
2) phosphoric acid solution of step 1) gained is joined in the cobalt acetate aqueous solution of step 1) gained under stirring, obtain claret emulsion, after stirring, the lithium hydroxide of step 1) gained/sucrose mixed solution is joined in described claret emulsion, stir, add the nitric acid of 15 parts, obtain precursor aqueous solution;
3) by step 2) precursor aqueous solution of gained under stirring, control leaving air temp and be 105 DEG C and carry out spraying dry, obtain the cobalt phosphate lithium powder presoma of porous spherical structure;
4) carry out vacuum calcining 16-26h at cobalt phosphate lithium powder presoma control temperature in vacuum furnace of the porous spherical structure of step 3) gained being 600-750 DEG C, obtain lithium ion battery positive pole material phosphoric acid cobalt lithium.
2. the synthetic method of a kind of lithium ion battery positive pole material phosphoric acid cobalt lithium as claimed in claim 1, is characterized in that described raw material, calculates according to the mass fraction, its composition and content as follows:
Lithium hydroxide 42 parts
Cobalt acetate 249 parts
Phosphatase 11 15 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts
Vacuum calcining described in step 4), namely control temperature is 680 DEG C, and the time is 21h.
3. the synthetic method of a kind of lithium ion battery positive pole material phosphoric acid cobalt lithium as claimed in claim 1, is characterized in that described raw material, calculates according to the mass fraction, its composition and content as follows:
Lithium hydroxide 38 parts
Cobalt acetate 224 parts
Phosphatase 11 05 part
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Vacuum calcining described in step 4), namely control temperature is 600 DEG C, and the time is 26h.
4. the synthetic method of a kind of lithium ion battery positive pole material phosphoric acid cobalt lithium as claimed in claim 1, is characterized in that described raw material, calculates according to the mass fraction, its composition and content as follows:
Lithium hydroxide 46 parts
Cobalt acetate 274 parts
Phosphatase 11 26 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Vacuum calcining described in step 4), namely control temperature is 750 DEG C, and the time is 16h.
5. the synthetic method of a kind of lithium ion battery positive pole material phosphoric acid cobalt lithium as claimed in claim 1, is characterized in that described raw material, calculates according to the mass fraction, its composition and content as follows:
Lithium hydroxide 46 parts
Cobalt acetate 224 parts
Phosphatase 11 15 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts
Vacuum calcining described in step 4), namely control temperature is 680 DEG C, and the time is 26h.
6. the synthetic method of a kind of lithium ion battery positive pole material phosphoric acid cobalt lithium as claimed in claim 1, is characterized in that described raw material, calculates according to the mass fraction, its composition and content as follows:
Lithium hydroxide 38 parts
Cobalt acetate 249 parts
Phosphatase 11 26 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Vacuum calcining described in step 4), namely control temperature is 750 DEG C, and the time is 21h.
7. the synthetic method of a kind of lithium ion battery positive pole material phosphoric acid cobalt lithium as claimed in claim 1, is characterized in that described raw material, calculates according to the mass fraction, its composition and content as follows:
Lithium hydroxide 42 parts
Cobalt acetate 274 parts
Phosphatase 11 05 part
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Vacuum calcining described in step 4), namely control temperature is 600 DEG C, and the time is 21h.
8. the synthetic method of a kind of lithium ion battery positive pole material phosphoric acid cobalt lithium as claimed in claim 1, is characterized in that described raw material, calculates according to the mass fraction, its composition and content as follows:
Lithium hydroxide 38 parts
Cobalt acetate 249 parts
Phosphatase 11 05 part
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Vacuum calcining described in step 4), namely control temperature is 750 DEG C, and the time is 16h.
9. the synthetic method of a kind of lithium ion battery positive pole material phosphoric acid cobalt lithium as claimed in claim 1, is characterized in that described raw material, calculates according to the mass fraction, its composition and content as follows:
Lithium hydroxide 38 parts
Cobalt acetate 249 parts
Phosphatase 11 26 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Vacuum calcining described in step 4), namely control temperature is 600 DEG C, and the time is 16h.
10. the synthetic method of a kind of lithium ion battery positive pole material phosphoric acid cobalt lithium as claimed in claim 1, is characterized in that described raw material, calculates according to the mass fraction, its composition and content as follows:
Lithium hydroxide 42 parts
Cobalt acetate 249 parts
Phosphatase 11 15 parts
15 parts, nitric acid
Sucrose 15 parts
Deionized water 650 parts;
Vacuum calcining described in step 4), namely control temperature is 750 DEG C, and the time is 26h.
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