CN103682311A - Preparation method of ternary composite cathode material of lithium ion battery - Google Patents
Preparation method of ternary composite cathode material of lithium ion battery Download PDFInfo
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- CN103682311A CN103682311A CN201310640541.6A CN201310640541A CN103682311A CN 103682311 A CN103682311 A CN 103682311A CN 201310640541 A CN201310640541 A CN 201310640541A CN 103682311 A CN103682311 A CN 103682311A
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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
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
-
- 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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of a ternary composite cathode material of a lithium ion battery. The method includes respectively dissolving a nickel-containing compound, a cobalt-containing compound and a manganese-containing compound into water according to a stoichiometric ratio; adding an organic acid, adjusting the pH by using aqueous ammonia, and stirring continuously to obtain a transparent uniform solution; putting the solution in an electric furnace and heating with the furnace until the solution evaporates and boils to the critical point and then rapid spontaneous combustion occurs; subjecting powder obtained from combustion to thermal treatment to obtain a Ni[x]Co[y]Mn[1-x-y]O2 precursor; and uniformly mixing the precursor and a lithium-containing compound, and performing thermal treatment to obtain the ternary composite cathode material. According to the preparation method, a two-step method is utilized to prepare the ternary composite cathode material, thus reducing lithium-nickel mixing phenomena in the preparation process and improving the structural purity of the prepared ternary material. The ternary material precursor is synthesized rapidly and simply by utilization of a self-propagating combustion. The obtained product is low in cost, uniform in particle and stable in electrochemical performance, and is prone to industrial production.
Description
Technical field
The present invention relates to lithium ion battery field, particularly a kind of preparation method of lithium ion battery tri compound positive electrode.
Background technology
In recent years, due to lithium ion battery, to have high-energy-density, height ratio capacity and quality light, and in mobile phone, notebook computer and electric motor car, these need be widely used in the device of high electric energy as power.And positive electrode plays vital effect in lithium ion battery product forms.At present, commercial Li-ion batteries mainly adopts cobalt acid lithium (LiCoO
2) as positive electrode, still, owing to boring resource shortage, expensive and its toxicity is higher, the few cobalt of exploitation or become the important development direction of lithium ion battery without the novel anode material of cobalt.Since Ohzuku and Makimura propose LiN
i1/3co
1/3mn
1/3o
2stratiform transition metal oxide substituting cobalt acid lithium as positive electrode after, LiNi
xco
ymn
1-x-yo
2the functional material of this Ni of having, Co, tri-kinds of element cooperative effects of Mn has caused both at home and abroad to be paid close attention to widely.Due to stratiform ternary material LiNi
xco
ymn
1-x-yo
2concentrated LiCoO
2, LiMnO
2and LiNiO
2advantage separately, has the advantages such as height ratio capacity, low cost, stable cycle performance and fail safe are good.In addition LiNi,
xco
ymn
1-x-yo
2with LiCoO
2be all a-NaFeO
2type layer structure, belongs to R3m space, and discharge range wider (2.5～4.6 V) is considered to have most the positive electrode of the new type lithium ion battery of application prospect.
LiNi
xco
ymn
1-x-yo
2its chemical property of trielement composite material is easily prepared technogenic influence, and a key factor of restriction ternary material performance is the lithium nickel mixing phenomenon in preparation process, Ni
2+ionic radius and Li
+ionic radius is close, Ni
2+oriented Li
+the trend of migration, causes the Li deviating from charge and discharge process
+can not again embed, cause the loss of capacity.Current LiNi
xco
ymn
1-x-yo
2technology of preparing mainly contain solid-phase synthesis, chemical precipitation method, sol-gel process, ultrasonic spray pyrolysis etc.The whole bag of tricks has its pluses and minuses, and different preparation methods causes prepared compound to have very large difference at aspects such as structure, pattern, specific area and electrochemical properties.Solid-phase synthesis is because calcining heat is high, and calcination time is long, and energy consumption is large, and lithium loss is serious, is difficult to control stoichiometric proportion, easily form dephasign, so chemical property is not very stable; And chemical precipitation method needs that massive laundering is washed, filtration, complex operation, yield poorly, synthesis condition is larger to the structure of synthetic product and performance impact, Repeatability is bad; Sol-gel rule is that synthesis cycle is longer, and the difficulty of suitability for industrialized production is larger.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of lithium ion battery tri compound positive electrode be provided:
To achieve these goals, technical scheme of the present invention:
A kind of preparation method's of lithium ion battery tri compound positive electrode step is as follows:
(1) by soluble nickel salt, solubility cobalt salt, soluble manganese salt, by nickel, cobalt, manganese mol ratio, be x:y:(1-x-y) be dissolved in water, be stirred to and form homogeneous transparent solution; 0.1≤x≤0.8 wherein, 0.1≤y≤0.6,0.2≤x+y≤0.9;
(2) in homogeneous transparent solution, add organic acid as metal ion chelation agent; Organic acid amount of substance is 0.5 ~ 2.0:1 with the ratio of the total amount of substance of metal ion;
(3) add ammonia spirit, regulator solution PH to 5.5 ~ 11, are constantly stirred to formation uniform solution;
(4) described uniform solution is moved into evaporating dish and be placed on electric furnace, along with heating by electric cooker to uniform solution evaporation is boiled to spontaneous combustion rapidly after critical point; Then heat treatment 4 ~ 10 hours at 400 ~ 600 ℃, finally obtains ternary Ni
xco
ymn
1-x-yo
2oxidized metal predecessor;
(5) by described ternary Ni
xco
ymn
1-x-yo
2oxidized metal predecessor and lithium-containing compound in the total amount of substance of transition metal and elemental lithium amount of substance be 1:1.05 ratio stir mix after heat treatment 6 ~ 10 hours at 400 ~ 600 ℃, heat treatment obtains ternary LiNi after 6 ~ 14 hours at 600 ~ 950 ℃
xco
ymn
1-x-yo
2positive electrode.
Described soluble nickel salt is nickel nitrate or nickel acetate; Described solubility cobalt salt is cobalt nitrate or cobalt acetate; Described soluble manganese salt is manganese nitrate or manganese acetate.
Described organic acid is citric acid, urea, ammonium acetate or hydrazine.
Described lithium-containing compound is lithium hydroxide or lithium acetate.
Compared with prior art, the present invention has following characteristics:
1. by by wet chemistry method with certainly spread low-temperature combustion method combination, the reaction time is short, easy and simple to handle, production cost is low, and product cut size is little, stable electrochemical property.
2. by two-step method, first prepare ternary material oxidation predecessor, then prepare ternary material, effectively reduce the lithium nickel mixing phenomenon in preparation process, improve the ternary material structural purity of preparation, thereby improve structural stability.
Specific embodiments
Below by embodiment, the present invention is described in further detail, but the scope not limiting the present invention in any way.
Embodiment mono-:
A kind of LiNi
1/3co
1/3mn
1/3o
2the method of lithium ion battery tri compound positive electrode: respectively 0.02mol tetra-water manganese nitrates, 0.02mol cobalt nitrate hexahydrate, 0.02mol six water nickel nitrates are dissolved in the aqueous solution successively, stir and form the homogeneous aqueous solution, under constantly stirring, add 0.03mol citric acid, stir and after 5 minutes, form the lilac solution of transparent and homogeneous, then slowly in solution, drip concentrated ammonia liquor, regulator solution PH=7, forms the deep purple solution of homogeneous by solution stirring after one hour; Solution is transferred to evaporating dish and be placed on electric furnace, along with heating by electric cooker solution evaporation is boiled to spontaneous combustion rapidly after critical point, produce dark-coloured bulk powder, the time is about 30 minutes; By the heat treatment 4 hours at 600 ℃ of gained powder, obtain ternary NiCoMnO
4oxidation predecessor; Take 0.005mol (1.1828g) NiCoMnO
4oxidation predecessor and 0.0158mol (0.6609g) LiOHH
2o stirs 1h, heat treatment 10 hours at 400 ℃ after fully mixing, and heat treatment obtains ternary LiNi after 14 hours at 600 ℃
1/3co
1/3mn
1/3o
2positive electrode.
Embodiment bis-:
A kind of LiNi
0.1co
0.1mn
0.8o
2the method of lithium ion battery tri compound positive electrode: respectively 0.006mol tetra-water manganese nitrates, 0.006mol cobalt nitrate hexahydrate, 0.048mol six water nickel nitrates are dissolved in the aqueous solution successively, stir and form the homogeneous aqueous solution, under constantly stirring, add 0.045mol citric acid, stir and after 5 minutes, form the lilac solution of transparent and homogeneous, then slowly in solution, drip concentrated ammonia liquor, regulator solution PH ~ 5.5, form the deep purple solution of homogeneous by solution stirring after one hour; Solution is transferred to evaporating dish and be placed on electric furnace, along with heating by electric cooker solution evaporation is boiled to spontaneous combustion rapidly after critical point, produce dark-coloured bulk powder, the time is about 30 minutes; By the heat treatment 6 hours at 600 ℃ of gained powder, obtain ternary Ni
0.1co
0.1mn
0.8o
2oxidation predecessor; Take 0.05mol (4.3857g) Ni
0.1co
0.1mn
0.8o
2oxidation predecessor and 0.0158mol (1.6063g) CH3COOLi2H
2o stirs 1h, heat treatment 8 hours at 500 ℃ after fully mixing, and heat treatment obtains ternary LiNi after 12 hours at 700 ℃
0.1co
0.1mn
0.8o
2positive electrode.
Embodiment tri-:
A kind of LiNi
0.4co
0.2mn
0.4o
2the method of lithium ion battery tri compound positive electrode: respectively 0.04mol tetra-water acetic acid manganese, 0.02mol Cobalt diacetate tetrahydrate, 0.04mol tetra-water acetic acid nickel are dissolved in the aqueous solution successively, stir and form the homogeneous aqueous solution, under constantly stirring, add 0.1mol urea, stir and after 5 minutes, form the lilac solution of transparent and homogeneous, then slowly in solution, drip concentrated ammonia liquor, regulator solution PH=8, forms the deep purple solution of homogeneous by solution stirring after one hour; Solution is transferred to evaporating dish and be placed on electric furnace, along with heating by electric cooker solution evaporation is boiled to spontaneous combustion rapidly after critical point, produce dark-coloured bulk powder, the time is about 30 minutes; By the heat treatment 8 hours at 500 ℃ of gained powder, obtain ternary Ni
0.4co
0.2mn
0.4o
2oxidation predecessor; Take 0.05mol (4.4619g) Ni
0.4co
0.2mn
0.4o
2oxidation predecessor and 0.0525mol (2.2029g) LiOHH
2o stirs 1h, heat treatment 8 hours at 600 ℃ after fully mixing, and heat treatment obtains ternary LiNi after 10 hours at 800 ℃
0.4co
0.2mn
0.4o
2positive electrode.
Embodiment tetra-:
A kind of LiNi
0.8co
0.1mn
0.1o
2the method of lithium ion battery tri compound positive electrode: respectively 0.08mol tetra-water acetic acid manganese, 0.01mol Cobalt diacetate tetrahydrate, 0.01mol tetra-water acetic acid nickel are dissolved in the aqueous solution successively, stir and form the homogeneous aqueous solution, after adding 0.125mol ammonium acetate to stir 5 minutes, form the lilac solution of transparent and homogeneous under constantly stirring, then slowly in solution, drip concentrated ammonia liquor, regulator solution PH=9, forms the deep purple solution of homogeneous by solution stirring after one hour; Solution is transferred to evaporating dish and be placed on electric furnace, along with heating by electric cooker solution evaporation is boiled to spontaneous combustion rapidly after critical point, produce dark-coloured bulk powder, the time is about 30 minutes; By the heat treatment 10 hours at 400 ℃ of gained powder, obtain ternary Ni
0.8co
0.1mn
0.1o
2oxidation predecessor; Take 0.05mol (4.4517g) Ni
0.8co
0.1mn
0.1o
2oxidation predecessor and 0.0525mol (5.3545g) CH3COOLi2H
2o stirs 1h, heat treatment 6 hours at 600 ℃ after fully mixing, and heat treatment obtains ternary LiNi after 8 hours at 900 ℃
0.8co
0.1mn
0.1o
2positive electrode.
Embodiment five:
A kind of LiNi
0.2co
0.5mn
0.3o
2the method of lithium ion battery tri compound positive electrode: respectively 0.03mol tetra-water manganese nitrates, 0.05mol cobalt nitrate hexahydrate, 0.02mol six water nickel nitrates are dissolved in the aqueous solution successively, stir and form the homogeneous aqueous solution, under constantly stirring, add 0.15mol hydrazine, stir and after 5 minutes, form the lilac solution of transparent and homogeneous, then slowly in solution, drip concentrated ammonia liquor, regulator solution PH=10, forms the deep purple solution of homogeneous by solution stirring after one hour; Solution is transferred to evaporating dish and be placed on electric furnace, along with heating by electric cooker solution evaporation is boiled to spontaneous combustion rapidly after critical point, produce dark-coloured bulk powder, the time is about 30 minutes; By the heat treatment 4 hours at 600 ℃ of gained powder, obtain ternary Ni
0.2co
0.5mn
0.3o
2oxidation predecessor; Take 0.05mol (4.4843g) Ni
0.2co
0.5mn
0.3o
2oxidation predecessor and 0.0525mol (2.2029g) LiOHH
2o stirs 1h, heat treatment 10 hours at 400 ℃ after fully mixing, and heat treatment obtains ternary LiNi after 6 hours at 950 ℃
0.2co
0.5mn
0.3o
2positive electrode.
Embodiment six:
A kind of LiNi
0.2co
0.5mn
0.3o
2the method of lithium ion battery tri compound positive electrode: respectively 0.03mol tetra-water manganese nitrates, 0.05mol cobalt nitrate hexahydrate, 0.02mol six water nickel nitrates are dissolved in the aqueous solution successively, stir and form the homogeneous aqueous solution, under constantly stirring, add 0.175mol urea, stir and after 5 minutes, form the lilac solution of transparent and homogeneous, then slowly in solution, drip concentrated ammonia liquor, regulator solution PH=11, forms the deep purple solution of homogeneous by solution stirring after one hour; Solution is transferred to evaporating dish and be placed on electric furnace, along with heating by electric cooker solution evaporation is boiled to spontaneous combustion rapidly after critical point, produce dark-coloured bulk powder, the time is about 30 minutes; By the heat treatment 6 hours at 600 ℃ of gained powder, obtain ternary Ni
0.2co
0.5mn
0.3o
2oxidation predecessor; Take 0.05mol (4.4843g) Ni
0.2co
0.5mn
0.3o
2oxidation predecessor and 0.0525mol (5.3545g) CH3COOLi2H
2o stirs 1h, heat treatment 8 hours at 500 ℃ after fully mixing, and heat treatment obtains ternary LiNi after 10 hours at 900 ℃
0.2co
0.5mn
0.3o
2positive electrode.
Embodiment seven:
A kind of LiNi
0.6co
0.2mn
0.2o
2the method of lithium ion battery tri compound positive electrode: respectively 0.02mol tetra-water acetic acid manganese, 0.02mol Cobalt diacetate tetrahydrate, 0.06mol tetra-water acetic acid nickel are dissolved in the aqueous solution successively, stir and form the homogeneous aqueous solution, under constantly stirring, add 0.2mol hydrazine, stir and after 5 minutes, form the lilac solution of transparent and homogeneous, then slowly in solution, drip concentrated ammonia liquor, regulator solution PH=7, forms the deep purple solution of homogeneous by solution stirring after one hour; Solution is transferred to evaporating dish and be placed on electric furnace, along with heating by electric cooker solution evaporation is boiled to spontaneous combustion rapidly after critical point, produce dark-coloured bulk powder, the time is about 30 minutes; By the heat treatment 8 hours at 500 ℃ of gained powder, obtain ternary Ni
0.2co
0.5mn
0.3o
2oxidation predecessor; Take 0.05mol (4.4994g) Ni
0.2co
0.5mn
0.3o
2oxidation predecessor and 0.0525mol (2.2029g) LiOHH
2o stirs 1h, heat treatment 8 hours at 600 ℃ after fully mixing, and heat treatment obtains ternary LiNi after 12 hours at 800 ℃
0.6co
0.2mn
0.2o
2positive electrode.
Embodiment eight:
A kind of LiNi
0.2co
0.2mn
0.6o
2the method of lithium ion battery tri compound positive electrode: respectively 0.02mol tetra-water acetic acid manganese, 0.02mol Cobalt diacetate tetrahydrate, 0.06mol tetra-water acetic acid nickel are dissolved in the aqueous solution successively, stir and form the homogeneous aqueous solution, under constantly stirring, add 0.1mol ammonium acetate, stir and after 5 minutes, form the lilac solution of transparent and homogeneous, then slowly in solution, drip concentrated ammonia liquor, regulator solution PH=8, forms the deep purple solution of homogeneous by solution stirring after one hour; Solution is transferred to evaporating dish and be placed on electric furnace, along with heating by electric cooker solution evaporation is boiled to spontaneous combustion rapidly after critical point, produce dark-coloured bulk powder, the time is about 30 minutes; By the heat treatment 10 hours at 400 ℃ of gained powder, obtain ternary Ni
0.2co
0.2mn
0.6o
2oxidation predecessor; Take 0.05mol (4.4247g) Ni
0.2co
0.2mn
0.6o
2oxidation predecessor and 0.0525mol (5.3545g) CH3COOLi2H
2o stirs 1h, heat treatment 8 hours at 600 ℃ after fully mixing, and heat treatment obtains ternary LiNi after 8 hours at 950 ℃
0.2co
0.2mn
0.6o
2positive electrode.
Claims (4)
1. a preparation method for lithium ion battery tri compound positive electrode, is characterized in that, its step is as follows:
(1) by soluble nickel salt, solubility cobalt salt, soluble manganese salt, by nickel, cobalt, manganese mol ratio, be x:y:(1-x-y) be dissolved in water, be stirred to and form homogeneous transparent solution; 0.1≤x≤0.8 wherein, 0.1≤y≤0.6,0.2≤x+y≤0.9;
(2) in homogeneous transparent solution, add organic acid as metal ion chelation agent; Organic acid amount of substance is 0.5 ~ 2.0:1 with the ratio of the total amount of substance of metal ion;
(3) add ammonia spirit, regulator solution PH to 5.5 ~ 11, are constantly stirred to formation uniform solution;
(4) described uniform solution is moved into evaporating dish and be placed on electric furnace, along with heating by electric cooker to uniform solution evaporation is boiled to spontaneous combustion rapidly after critical point; Then heat treatment 4 ~ 10 hours at 400 ~ 600 ℃, finally obtains ternary Ni
xco
ymn
1-x-yo
2oxidized metal predecessor;
(5) by described ternary Ni
xco
ymn
1-x-yo
2oxidized metal predecessor and lithium-containing compound in the total amount of substance of transition metal and elemental lithium amount of substance be 1:1.05 ratio stir mix after heat treatment 6 ~ 10 hours at 400 ~ 600 ℃, heat treatment obtains ternary LiNi after 6 ~ 14 hours at 600 ~ 950 ℃
xco
ymn
1-x-yo
2positive electrode.
2. the preparation method of lithium ion battery tri compound positive electrode as claimed in claim 1, is characterized in that: described soluble nickel salt is nickel nitrate or nickel acetate; Described solubility cobalt salt is cobalt nitrate or cobalt acetate; Described soluble manganese salt is manganese nitrate or manganese acetate.
3. the preparation method of lithium ion battery tri compound positive electrode as claimed in claim 1, is characterized in that: described organic acid is citric acid, urea, ammonium acetate or hydrazine.
4. the preparation method of lithium ion battery tri compound positive electrode as claimed in claim 1, is characterized in that: described lithium-containing compound is lithium hydroxide or lithium acetate.
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| CN104051724A (en) * | 2014-06-06 | 2014-09-17 | 奇瑞汽车股份有限公司 | Carbon-coated nickel-cobalt lithium manganate positive electrode material and preparation method thereof |
| CN104103825A (en) * | 2014-08-06 | 2014-10-15 | 于英超 | Rich lithium ternary lithium ion battery cathode materials and production method thereof |
| CN106904668A (en) * | 2017-04-14 | 2017-06-30 | 郑州科技学院 | A kind of preparation method of tetrakaidecahedron shape nanometer nickel-cobalt LiMn2O4 |
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