CN105591092A - Ni-Co-Mn composite oxide lithium ion battery anode material, preparation method and application thereof - Google Patents
Ni-Co-Mn composite oxide lithium ion battery anode material, preparation method and application thereof Download PDFInfo
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a Ni-Co-Mn composite oxide lithium ion battery anode material which is a Ni-Co-Mn composite oxide or a carbon-coated Ni-Co-Mn composite oxide. The molecular formula of the Ni-Co-Mn composite oxide is Ni<x>Mn<y>Co<z>O<4+/-[delta]>, wherein the mole numbers of the Ni, Co, Mn are: 0.025 <= x <= 0.95, 0.025 <= y <= 0.95, 0.025 <= z <= 1.2, and 0 <= [delta] <= 1. The material is good in rate capability and is high in safety. The invention also discloses a preparation method and an application of the Ni-Co-Mn composite oxide lithium ion battery anode material.
Description
Technical field
The present invention relates toOnePlant cobalt-nickel-manganese oxide compound lithium ion battery cathode material and its preparation method and application.
Background technology
Along with the miniaturization of portable electric appts and the fast development of electric automobile, people also improve day by day for the requirement of capacity of lithium ion battery. The measure such as nucleocapsid structure material, surface are coated, doping vario-property still can not meet the requirement of extensive high power capacity, small size lithium ion battery by preparing for current business-like material with carbon element, silicon, tin metal and metal alloy etc., and there is Volume Changes in above-mentioned material in removal lithium embedded cyclic process, cause between charge and discharge cycles rear electrode material particle and and collector between loose contact, form " isolated island " effect. " isolated island " effect can cause the destroyed and resistance of the conductive network between electrode material, conductive agent carbon black and collector to increase, the cycle performance of battery declines, carbon material surface can produce Li dendrite simultaneously, can puncture barrier film and cause both positive and negative polarity short circuit, causes battery explosion, on fire when serious.
Summary of the invention
The object of the present invention is to provideOneKind of good rate capability, safe cobalt-nickel-manganese oxide compound lithium ion battery negative material.
The molecular formula of cobalt-nickel-manganese oxide compound lithium ion battery negative material is NixMnyCozO4±δ, wherein, nickel: cobalt: manganese molal quantity is 0.025≤x≤0.95,0.025≤y≤0.95,0.025≤z≤1.2,0≤δ≤1, and the preparation method of this material is as follows:
Taking the mixture of two or more compounds in mixture, nickel cobalt manganese composite hydroxide, the compound oxyhydroxide of nickel cobalt manganese, the compound carbonyls of nickel cobalt manganese, nickel cobalt manganese compound carbonate and nickel cobalt manganese composite hydroxide, the compound oxyhydroxide of nickel cobalt manganese, nickel cobalt manganese compound carbonate and the compound carbonyls of nickel cobalt manganese of nickel salt, cobalt salt, manganese salt as raw material, under argon gas, nitrogen or air atmosphere, after two-section calcining, cooling with stove, obtain the cobalt-nickel-manganese oxide compound powder of smoky gray.
Cobalt-nickel-manganese oxide compound lithium ion battery negative material is the cobalt-nickel-manganese oxide compound of carbon coated, and the molecular formula of described cobalt-nickel-manganese oxide compound is NixMnyCozO4±δ, wherein, nickel: cobalt: manganese molal quantity is 0.025≤x≤0.95,0.025≤y≤0.95,0.025≤z≤1.2,0≤δ≤1, and the preparation method of this material is as follows:
1) taking the mixture of two or more compounds in mixture, nickel cobalt manganese composite hydroxide, the compound oxyhydroxide of nickel cobalt manganese, nickel cobalt manganese compound carbonate, the compound carbonyls of nickel cobalt manganese and nickel cobalt manganese composite hydroxide, nickel cobalt manganese compound carbonate, the compound oxyhydroxide of nickel cobalt manganese and the compound carbonyls of nickel cobalt manganese of nickel salt, cobalt salt, manganese salt as raw material, under argon gas, nitrogen or air atmosphere, after two-section calcining, cooling with stove, obtain the cobalt-nickel-manganese oxide compound powder of smoky gray;
2) after cobalt-nickel-manganese oxide compound powder is mixed with the dressing agent of positively charged, pour in absolute ethyl alcohol, stirring and refluxing 8~20h at 60~80 DEG C, filters, and high purity water washs after 6~8 times, and 60~100 DEG C of oven dry, obtain black powder;
3) by step 2) to pour quality into be in its water of 10~20 times to gained black powder, adds after material with carbon element, stirs 0.5~4h, filters, dries, and obtains the cobalt-nickel-manganese oxide compound of black carbon coated.
Described nickel salt is one or more mixtures in nickelous carbonate, carbonyl nickel, nickel oxalate, nickel acetate, nickel nitrate, nickel chloride, nickel acetate, nickelous sulfate, nickel phosphate, nickelous bromide, nickel iodide.
Described cobalt salt is one or more mixtures in cobalt carbonate, carbonyl cobalt, cobalt oxalate, cobalt acetate, cobalt nitrate, cobalt chloride, cobalt acetate, cobaltous sulfate, cobalt phosphate, cobaltous bromide, cobaltous iodide.
Described manganese salt is one or more mixtures in manganese carbonate, manganese carbonyl, manganese oxalate, manganese acetate, manganese nitrate, manganese chloride, manganese sulfate, manganese phosphate, manganous bromide, manganese iodide.
The molecular formula of described nickel cobalt manganese composite hydroxide, the compound oxyhydroxide of nickel cobalt manganese, nickel cobalt manganese compound carbonate, the compound carbonyls of nickel cobalt manganese is respectively NixMnyCoz(OH)2、NixMnyCozO(OH)、NixMnyCozCO3、NixMnyCoz(CO)8, wherein, nickel: cobalt: manganese molal quantity is 0.025≤x≤0.95,0.025≤y≤0.95,0.025≤z≤1.2.
The heating rate of the first paragraph calcining of described two-section calcining is 1~10 DEG C/min, is warmed up to 300~500 DEG C, insulation 4~12h; The heating rate of second segment is 1~8 DEG C, is warmed up to 500~900 DEG C, insulation 1h~5h.
The dressing agent of described positively charged is polyaniline, PDDA (PDDA), 3-aminopropyl triethoxysilane (APTES).
Described material with carbon element is active carbon, acetylene black, carbonaceous mesophase spherules, conductive black, carbon fiber, CNT, Graphene, and its quality is 1~15% of cobalt-nickel-manganese oxide compound quality.
The cobalt-nickel-manganese oxide compound of described cobalt-nickel-manganese oxide compound and carbon coated is applied in lithium ion battery as the negative pole of lithium ion battery.
Adopt X-ray diffraction instrument (XRD) and field emission scanning electron microscope (SEM) to characterize crystalline structure, granule size, shape etc., determined that cobalt-nickel-manganese oxide compound has Fd3m space group structure.
The present invention compared with prior art, has the following advantages:
1, the present invention makes using the cobalt-nickel-manganese oxide compound of cobalt-nickel-manganese oxide compound and carbon coated as the negative pole of lithium ion battery that lithium ion battery specific discharge capacity is large, good rate capability.
2, the present invention can effectively avoid the generation of Li dendrite, makes lithium ion battery have higher security.
The abundant raw materials of the cobalt-nickel-manganese oxide compound that 3, prepared by the present invention, preparation process is simple, easy operating, possesses homogeneous grain diameter, productive rate is high, cost is low, constant product quality, cost performance advantages of higher simultaneously; Prepared cobalt-nickel-manganese oxide compound can be widely used in the fields such as lithium ion battery, lithium-air battery, lithium-sulfur cell, thermal sensitive ceramics, catalysis.
Brief description of the drawings
Fig. 1 is the XRD spectra of prepared cobalt-nickel-manganese oxide compound in embodiment 1-9.
Fig. 2 is field emission electron ESEM (SEM) figure of prepared cobalt-nickel-manganese oxide compound in embodiment 4.
Fig. 3 is the charging and discharging curve figure that in embodiment 5, prepared cobalt-nickel-manganese oxide compound is assembled into button cell.
Fig. 4 is the cycle performance curve map that in embodiment 5, prepared cobalt-nickel-manganese oxide compound is assembled into button cell.
Detailed description of the invention
Embodiment 1:
By 5gNi1/3Co1/3Mn1/3(OH)2Raw material is put into corundum material boat, is then positioned in calcining furnace. In air, be raised to 500 DEG C and be incubated 10h with the heating rate of 5 DEG C/min, be then raised to 600 DEG C and be incubated 8h with the heating rate of 1 DEG C/min, obtain smoky gray Ni1/3Co1/3Mn1/3O4±δ(0≤δ≤1) powder.
Embodiment 2:
By 5gNi1/3Co1/3Mn1/3(OH)2Raw material is put into corundum material boat, is then positioned in calcining furnace. In air, be raised to 450 DEG C and be incubated 10h with the heating rate of 3 DEG C/min, be then raised to 600 DEG C and be incubated 10h with the heating rate of 2 DEG C/min, obtain smoky gray Ni1/3Co1/3Mn1/3O4±δ(0≤δ≤1) powder.
Embodiment 3:
By 5gNi1/3Co1/3Mn1/3(OH)2Raw material is put into corundum material boat, is then positioned in calcining furnace. In air, be raised to 600 DEG C and be incubated 10h with the heating rate of 5 DEG C/min, be then raised to 700 DEG C and be incubated 3h with the heating rate of 3 DEG C/min, obtain smoky gray Ni1/3Co1/3Mn1/3O4±δ(0≤δ≤1) powder.
Embodiment 4:
By 5gNi1/3Co1/3Mn1/3O(OH) raw material is put into corundum material boat, is then positioned in calcining furnace. In air, be raised to 600 DEG C and be incubated 10h with the heating rate of 3 DEG C/min, be then raised to 700 DEG C and be incubated 1h with the heating rate of 2 DEG C/min, obtain smoky gray Ni1/3Co1/3Mn1/3O4±δ(0≤δ≤1) powder.
As shown in Figure 2, the Ni making1/3Co1/3Mn1/3O4±δThe particle of (0≤δ≤1) dusty material is spherical uniformly, and particle diameter is distributed in 300~600nm.
Embodiment 5:
By 5gNi1/3Co1/3Mn1/3(OH)2Raw material is put into corundum material boat, is then positioned in calcining furnace. In air, be raised to 600 DEG C and be incubated 10h with the heating rate of 2 DEG C/min, be then raised to 700 DEG C and be incubated 1h with the heating rate of 2 DEG C/min, obtain smoky gray Ni1/3Co1/3Mn1/3O4±δ(0≤δ≤1) powder.
As shown in Figure 3, prepared cobalt-nickel-manganese oxide compound and metal lithium sheet are assembled into after button cell, its specific discharge capacity is 1140mAh/g, is 3 times of specific discharge capacity (372mAh/g) of current business-like graphite.
As shown in Figure 4, prepared cobalt-nickel-manganese oxide compound and metal lithium sheet are assembled into after button cell, circulate after 350 circles under 0.2A/g current density, its specific discharge capacity is still 1.88 times of the specific discharge capacities of graphite.
Embodiment 6:
By 5gNi1/3Co1/3Mn1/3(OH)2Raw material is put into corundum material boat, is then positioned in calcining furnace. In air, be raised to 600 DEG C and be incubated 12h with the heating rate of 2 DEG C/min, be then raised to 800 DEG C and be incubated 1h with the heating rate of 2 DEG C/min, obtain smoky gray Ni1/3Co1/3Mn1/3O4±δ(0≤δ≤1) powder.
Embodiment 7:
By 5gNi1/3Co1/3Mn1/3(OH)2Raw material is put into corundum material boat, is then positioned in calcining furnace. In nitrogen protection gas, be raised to 600 DEG C and be incubated 12h with the heating rate of 5 DEG C/min, be then raised to 900 DEG C and be incubated 1h with the heating rate of 2 DEG C/min, obtain smoky gray Ni1/3Co1/3Mn1/3O4±δ(0≤δ≤1) powder.
Embodiment 8:
By 5gNi1/3Co1/3Mn1/3CO3Raw material is put into corundum material boat, is then positioned in calcining furnace. In argon shield gas, be raised to 600 DEG C and be incubated 12h with the heating rate of 2 DEG C/min, be then raised to 700 DEG C and be incubated 1h with the heating rate of 2 DEG C/min, obtain smoky gray Ni1/3Co1/3Mn1/3O4±δ(0≤δ≤1) powder.
Embodiment 9:
The nickel that is 8:1:1 by 5g mol ratio, cobalt, manganese subcarbonate raw material ball milling mix after, put into corundum material boat, be then positioned in calcining furnace. In air, be raised to 600 DEG C and be incubated 10h with the heating rate of 2 DEG C/min, be then raised to 700 DEG C and be incubated 3h with the heating rate of 2 DEG C/min, obtain smoky gray Ni0.8Co0.1Mn0.1O4±δ(0≤δ≤1) powder.
Embodiment 10:
The carbonyl nickel that is 5:2:3 by the mol ratio of 5g nickel, cobalt, manganese, manganese carbonyl, the mixed raw material of carbonyl cobalt ball milling, put into corundum material boat, is then positioned in calcining furnace. In air, be raised to 600 DEG C and be incubated 8h with the heating rate of 2 DEG C/min, be then raised to 700 DEG C and be incubated 1h with the heating rate of 2 DEG C/min, obtain smoky gray Ni0.5Co0.2Mn0.3O4±δ(0≤δ≤1) powder.
Embodiment 11:
The hydroxy nickel oxide that is 1:1:1 by the mol ratio of 5g nickel, cobalt, manganese, hydroxyl oxidize manganese, the mixed raw material of hydroxy cobalt oxide ball milling, put into corundum material boat, is then positioned in calcining furnace. In air, be raised to 600 DEG C and be incubated 10h with the heating rate of 2 DEG C/min, be then raised to 700 DEG C and be incubated 5h with the heating rate of 2 DEG C/min, obtain smoky gray Ni1/3Mn1/3Co1/3O4±δ(0≤δ≤1) powder.
Embodiment 12:
The nickel oxalate that is 1:1:8 by the mol ratio of 5g nickel, cobalt, manganese, manganese oxalate, the mixed raw material of cobalt oxalate ball milling, put into corundum material boat, is then positioned in calcining furnace. In air, be raised to 600 DEG C and be incubated 10h with the heating rate of 3 DEG C/min, be then raised to 700 DEG C and be incubated 3h with the heating rate of 2 DEG C/min, obtain smoky gray Ni0.1Co0.1Mn0.8O4±δ(0≤δ≤1) powder.
Embodiment 13:
To in embodiment 1, obtain 5g smoky gray powder, after mixing with 3-aminopropyl triethoxysilane (APTES) positively charged dressing agent, pour in absolute ethyl alcohol, at 70 DEG C after stirring and refluxing 20h, filtration, high purity water wash after 6 times, and 80 DEG C of oven dry, obtain black powder. This black powder is poured in 50g water, added after the carbon dust of 0.25g, stir 0.5h, filter, dry, obtain the cobalt-nickel-manganese oxide compound dusty material of the coated activated carbon of black.
Embodiment 14:
To in embodiment 5, obtain 5g smoky gray powder, after mixing, pour in absolute ethyl alcohol with polyaniline positive electricity dressing agent, at 60 DEG C, after stirring and refluxing 10h, filtration, high purity water wash after 6 times, and 60 DEG C of oven dry, obtain black powder. This black powder is poured in 100g water, added after the Graphene of 0.5g, stir 2h, filter, dry, obtain the cobalt-nickel-manganese oxide compound dusty material of black carbon coated.
Embodiment 15:
To in embodiment 3, obtain 100g smoky gray powder, after mixing with 3-aminopropyl triethoxysilane (APTES) positively charged dressing agent, pour in absolute ethyl alcohol, at 80 DEG C after stirring and refluxing 12h, filtration, high purity water wash after 8 times, and 80 DEG C of oven dry, obtain black powder. This black powder is poured in 1000g water, added after the CNT of 2.5g, stir 3h, filter, dry, obtain the cobalt-nickel-manganese oxide compound dusty material of black enveloped carbon nanometer tube.
Claims (10)
1. cobalt-nickel-manganese oxide compound lithium ion battery negative material, is characterized in that this material is the cobalt-nickel-manganese oxide compound of cobalt-nickel-manganese oxide compound or carbon coated, and the molecular formula of described cobalt-nickel-manganese oxide compound is NixMnyCozO4±δ, wherein, nickel: cobalt: manganese molal quantity is 0.025≤x≤0.95,0.025≤y≤0.95,0.025≤z≤1.2,0≤δ≤1.
2. the preparation method of cobalt-nickel-manganese oxide compound lithium ion battery negative material as claimed in claim 1, is characterized in that the preparation method of described cobalt-nickel-manganese oxide compound is as follows:
Taking the mixture of two or more compounds in mixture, nickel cobalt manganese composite hydroxide, the compound oxyhydroxide of nickel cobalt manganese, the compound carbonyls of nickel cobalt manganese, nickel cobalt manganese compound carbonate and nickel cobalt manganese composite hydroxide, the compound oxyhydroxide of nickel cobalt manganese, nickel cobalt manganese compound carbonate and the compound carbonyls of nickel cobalt manganese of nickel salt, cobalt salt, manganese salt as raw material, under argon gas, nitrogen or air atmosphere, after two-section calcining, cooling with stove, obtain the cobalt-nickel-manganese oxide compound powder of smoky gray.
3. the preparation method of cobalt-nickel-manganese oxide compound lithium ion battery negative material as claimed in claim 1, is characterized in that the preparation method of cobalt-nickel-manganese oxide compound of described carbon coated is as follows:
1) taking the mixture of two or more compounds in mixture, nickel cobalt manganese composite hydroxide, the compound oxyhydroxide of nickel cobalt manganese, nickel cobalt manganese compound carbonate, the compound carbonyls of nickel cobalt manganese and nickel cobalt manganese composite hydroxide, nickel cobalt manganese compound carbonate, the compound oxyhydroxide of nickel cobalt manganese and the compound carbonyls of nickel cobalt manganese of nickel salt, cobalt salt, manganese salt as raw material, under argon gas, nitrogen or air atmosphere, after two-section calcining, cooling with stove, obtain the cobalt-nickel-manganese oxide compound powder of smoky gray;
2) after cobalt-nickel-manganese oxide compound powder is mixed with the dressing agent of positively charged, pour in absolute ethyl alcohol, stirring and refluxing 8~20h at 60~80 DEG C, filters, and high purity water washs after 6~8 times, and 60~100 DEG C of oven dry, obtain black powder;
3) by step 2) to pour quality into be in its water of 10~20 times to gained black powder, adds after material with carbon element, stirs 0.5~4h, filters, dries, and obtains the cobalt-nickel-manganese oxide compound of black carbon coated.
4. preparation method as claimed in claim 2 or claim 3, is characterized in that described nickel salt is one or more mixtures in nickelous carbonate, carbonyl nickel, nickel oxalate, nickel acetate, nickel nitrate, nickel chloride, nickel acetate, nickelous sulfate, nickel phosphate, nickelous bromide, nickel iodide; Described cobalt salt is one or more mixtures in cobalt carbonate, carbonyl cobalt, cobalt oxalate, cobalt acetate, cobalt nitrate, cobalt chloride, cobalt acetate, cobaltous sulfate, cobalt phosphate, cobaltous bromide, cobaltous iodide; Described manganese salt is one or more mixtures in manganese carbonate, manganese carbonyl, manganese oxalate, manganese acetate, manganese nitrate, manganese chloride, manganese sulfate, manganese phosphate, manganous bromide, manganese iodide.
5. preparation method as claimed in claim 2 or claim 3, is characterized in that the molecular formula of described nickel cobalt manganese composite hydroxide, the compound oxyhydroxide of nickel cobalt manganese, nickel cobalt manganese compound carbonate, the compound carbonyls of nickel cobalt manganese is respectively NixMnyCoz(OH)2、NixMnyCozO(OH)、NixMnyCozCO3、NixMnyCoz(CO)8, wherein, nickel: cobalt: manganese molal quantity is 0.025≤x≤0.95,0.025≤y≤0.95,0.025≤z≤1.2.
6. preparation method as claimed in claim 2 or claim 3, is characterized in that the heating rate of the first paragraph calcining of described two-section calcining is 1~10 DEG C/min, is warmed up to 300~500 DEG C, insulation 4~12h; The heating rate of second segment is 1~8 DEG C, is warmed up to 500~900 DEG C, insulation 1h~5h.
7. preparation method as claimed in claim 3, the dressing agent that it is characterized in that described positively charged is polyaniline, PDDA (PDDA), 3-aminopropyl triethoxysilane (APTES).
8. preparation method as claimed in claim 3, is characterized in that described material with carbon element is active carbon, acetylene black, carbonaceous mesophase spherules, conductive black, carbon fiber, CNT, Graphene.
9. the preparation method as described in claim 3 or 8, the quality that it is characterized in that described material with carbon element is 1~15% of cobalt-nickel-manganese oxide compound quality.
10. the application of cobalt-nickel-manganese oxide compound lithium ion battery negative material as claimed in claim 1 in lithium ion battery.
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US10784501B2 (en) | 2017-12-12 | 2020-09-22 | Industrial Technology Research Institute | Positive electrode plate and method of forming slurry for positive electrode plate |
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