CN106571455B - A kind of silver-colored mesopore silicon oxide cladding tertiary cathode material of load and preparation method and application - Google Patents
A kind of silver-colored mesopore silicon oxide cladding tertiary cathode material of load and preparation method and application Download PDFInfo
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- 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
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- 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
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Abstract
The present invention relates to a kind of silver-colored mesopore silicon oxide cladding tertiary cathode material of load and preparation method and application, lithium salts, nickel salt, cobalt salt, manganese salt are dissolved in uniform dielectric, and ammonium hydroxide is added in double chelating agent wettings, double chelating agent solutions are added in inorganic salts uniform dielectric, are heated with stirring to form xerogel;It clays into power, calcining obtains ternary material;Tetraethyl orthosilicate, ethyl alcohol and surfactant cetyl trimethylammonium bromide is added in ternary nano material aqueous solution, and precipitating centrifuge washing drying and calcining obtains silica-ternary core-shell positive electrode;Silver oxide solution A soluble in water;PVP solution B soluble in water;Solution B, which is added drop-wise in solution A, obtains solution C;Silica-ternary core-shell positive electrode is added in solution C and obtains solution D;Will reducing agent be added dropwise solution D in, washing filtering and drying to obtain arrive final product.Preparation method is simple, and process conditions are easy to accomplish, and energy consumption is low, and prepares pollution-free.
Description
Technical field
The present invention relates to a kind of preparation methods of lithium electricity positive electrode, more particularly to a kind of silver-colored mesopore silicon oxide cladding of load
Tertiary cathode material and preparation method and application.
Background technique
With the rapid development of smaller, lighter and higher performance electronics and communication apparatus, people mention to for these equipment
The battery performance of power supply source especially proposes increasingly higher demands to specific energy.But the lithium-ion electric being commercialized at present
The specific capacity of pond and MH/Ni battery has been difficult to continue to improve.Therefore, there is an urgent need to develop the higher batteries of specific energy.Lithium from
Sub- secondary cell has been widely used for mobile communication, laptop, video camera, photograph as high-energy-density electrochmical power source
The fields such as machine, portable instrument, rapidly developing becomes one of currently the most important ones secondary cell.Lithium ion battery is as most
The green high-capacity battery of a new generation, develops rapidly in early 1990s, and lithium ion battery is because its voltage is high, energy
Density is high, have extended cycle life, the advantages that environmental pollution is small gains great popularity.
Due to ternary material LiNi1-x-yCoxMnyO2(0 < x < 1,0 < y < 1) have better than LiFePO 4 and cobalt acid lithium
Characteristic, and according to the ratio for adjusting nickel, cobalt, manganese, the ternary electrode material of different performance can be prepared.With new energy vapour
The rise and development of vehicle, ternary material are the hot spots of research.
Summary of the invention
In order to overcome the deficiencies of the prior art, the present invention provides a kind of system for carrying silver-colored mesopore silicon oxide cladding tertiary cathode material
Preparation Method.
A kind of preparation method carrying silver-colored mesopore silicon oxide cladding tertiary cathode material, which is characterized in that this method it is specific
Step are as follows:
(1) by mole ratio 1:1-x-y:x:y(0 < x < 1,0 < y < 1) lithium salts, nickel salt, cobalt salt, manganese salt are dissolved in uniformly
In medium, magnetic agitation is dissolved completely in inorganic salts in uniform dielectric;The double chelating agents of mixing that mole ratio is 1 ~ 2:1 are added
A small amount of deionized water wetting, is added ammonium hydroxide, shakes to formation colourless transparent solution, then nothings are added in colorless and transparent double chelating agent solutions
In machine salt uniform dielectric, the clear solution of bluish violet, 60 ~ 80 DEG C of heating stirrings to formation bluish violet colloidal sol are formed;By gel material
Expect to be heated to forming the porous xerogel of black for 180 ~ 240 DEG C in air dry oven;Obtained black xerogel is ground into
Powder calcines 5 ~ 10 h at 750 ~ 900 DEG C of Muffle furnace and obtains ternary material;
(2) positive silicic acid four is added in 60 ~ 80 DEG C of 15 ~ 30min of stirring in the ternary nano material aqueous solution in step (1)
Ethyl ester, ethyl alcohol and surfactant cetyl trimethylammonium bromide (CTAB), 60 ~ 80 DEG C are continued 1 ~ 2 h of stirring, make positive silicic acid
Tetra-ethyl ester is crosslinked with CTAB micella;In ternary core outer cladding silica shell, m (tetraethyl orthosilicate): m(CTAB): m
(ethyl alcohol)=0.25 ~ 0.5:0.05 ~ 0.1:1;Precipitating is centrifuged, uses deionized water and ethanol washing 2 ~ 3 times, convection oven respectively
50 ~ 80 DEG C of dry 5 ~ 8h are placed in 400 ~ 600 DEG C of 5 ~ 10 h of calcining in Muffle furnace, obtain silica-ternary core-shell anode material
Material;
(3) 0.005 ~ 0.01 mol silver oxide is dissolved in deionized water, 4 ~ 10 mL ammonia is added dropwise after stirring 10 ~ 20 min
Water obtains solution A;5 ~ 10 g PVP are dissolved in 100 mL deionized waters, stirring obtains solution B to transparent;Dropwise by solution B
It is added drop-wise in solution A, drips 5 ~ 10 h of stirring, obtain solution C;Step (2) products therefrom is added in solution C, solution is obtained
D;0.0016 ~ 0.0048 mol reducing agent is added dropwise in solution D and continues 2 ~ 4 h of stirring, by obtained sediment spend from
Sub- water and ethanol washing for several times after, filter, obtain final product after drying.
The lithium salts is lithium nitrate, lithium carbonate, lithium chloride, lithium acetate, lithium citrate, lithium oxalate, lithium formate, lithium lactate
Or one of isopropyl lithium alkoxide or combinations thereof.
The nickel salt is nickel nitrate, nickel chloride, nickel acetate, nickel sulfate or one kind of nickel oxalate or combinations thereof.
The cobalt salt is cobalt nitrate, cobalt chloride, cobalt acetate, cobaltous sulfate or one kind of cobalt oxalate or combinations thereof.
The manganese salt is manganese nitrate, manganese chloride, manganese carbonate, manganese acetate or one kind of manganese oxalate or combinations thereof.
The uniform dielectric is deionized water, ethyl alcohol, acetone.
The chelating agent be citric acid (CA), ethylenediamine tetra-acetic acid (EDTA), acetylacetone,2,4-pentanedione, in polyacrylic acid (PPA)
Any two kinds.
The reducing agent is sodium borohydride, ascorbic acid.
A kind of silver-colored mesopore silicon oxide cladding tertiary cathode material of load, which is characterized in that according to any of the above-described the method system
It is standby to obtain.
A kind of application carrying silver-colored mesopore silicon oxide cladding tertiary cathode material as lithium electricity positive electrode.
The present invention provides a kind of ternary-load silver meso-porous silica core-shell structure positive electrode (LiNi1-x-yCoxMnyO2@
Ag/meso-SiO2(0 < x < 1,0 < y < 1)) preparation method, the present invention using ternary nano particle as core, with mesoporous SiO2For shell,
Using in-situ reducing growth method in mesoporous SiO2Nano silver grain is loaded in duct.Wherein, mesoporous silicon oxide not only mitigates electricity
Corrosion of the liquid to tertiary cathode material is solved, and provides channel for the transmission of electronics;And in mesoporous SiO2The silver loaded in duct
Nanoparticle further improves the electric conductivity of material.First discharge specific capacity reaches 180 mAh/g under 1 C multiplying power, has
Higher theoretical capacity is recycled by 50 times, and specific discharge capacity is 162 mAh/g, has more stable circulation.Preparation method letter
Single, process conditions are easy to accomplish, and energy consumption is low, and prepare pollution-free.
Detailed description of the invention
Fig. 1 is embodiment 1LiNi1/3Co1/3Mn1/3O2@Ag/meso-SiO2The cycle life figure of material.
Specific embodiment
The present invention is described in detail by following specific example, but protection scope of the present invention is not only restricted to these
Examples of implementation.
Embodiment one:
(1) mol: 0.0033 mol: 0.0033 mol of 0.01 mol:0.0033 of mole ratio is pressed by lithium acetate, vinegar
Sour nickel, cobalt acetate and manganese acetate are added stirring in deionized water and all dissolve to metal salt;By the mixing pair that mole ratio is 2:1
Chelating agent EDTA-CA adds a small amount of deionized water to soak, and ammonium hydroxide is added, and shakes to formation colourless transparent solution, then will be colorless and transparent double
Chelating agent solution is added in inorganic salts uniform dielectric, forms the clear solution of bluish violet, and 70 DEG C of heating stirrings are to forming bluish violet
Colloidal sol;80 DEG C of heating stirrings extremely form bluish violet colloidal sol;By gel rubber material in air dry oven 240 DEG C be heated to being formed it is black
The porous xerogel of color;The black xerogel grind into powder that will be obtained, calcines 5 h at 850 DEG C of Muffle furnace and obtains LiNi1/ 3Co1/3Mn1/3O2。
(2) by the LiNi in step (1)1/3Co1/3Mn1/3O2Positive silicic acid tetrem is added in 80 DEG C of 15 min of stirring in aqueous solution
Ester, ethyl alcohol and Surfactant CTAB, 80 DEG C are continued to stir 1 h, are crosslinked tetraethyl orthosilicate with CTAB micella.?
Ternary core outer cladding silica shell, m (tetraethyl orthosilicate): m(CTAB): m(ethyl alcohol)=0.25:0.05:1;To precipitate from
The heart, uses deionized water and ethanol washing 3 times respectively, and 80 DEG C of 5 h of drying of convection oven are placed in 600 DEG C of calcinings 5 in Muffle furnace
H obtains silica-ternary core-shell positive electrode (LiNi1/3Co1/3Mn1/3O2@meso-SiO2).
(3) 0.005 mol silver oxide is dissolved in deionized water, 4 mL ammonium hydroxide is added dropwise after stirring 20 min, obtain solution
A;5 g PVP are dissolved in 100 mL deionized waters, stirring obtains solution B to transparent;Solution B is added drop-wise in solution A dropwise,
10 h of stirring are dripped, solution C is obtained;Step (2) products therefrom is added in solution C, solution D is obtained;By 0.0016 mol boron
Sodium hydride be added dropwise in solution D continues stir 2 h, by obtained sediment deionized water and ethanol washing for several times after, take out
Final product LiNi is obtained after filter, drying1/3Co1/3Mn1/3O2@Ag/meso-SiO2.Fig. 1 is LiNi1/3Co1/3Mn1/3O2@Ag/
meso-SiO2The cycle life figure of material, 180 mAh/g of its first discharge specific capacity under 1 C multiplying power, after 50 circulations,
Its specific discharge capacity is about 162 mAh/g.Mesoporous SiO2Not only mitigate corrosion of the electrolyte to tertiary cathode material, but also is electricity
The transmission of son provides channel;And in mesoporous SiO2The Nano silver grain loaded in duct further improves the conduction of material
Property, and then obtain the battery material of superior performance.
Embodiment two:
(1) by 0.01 mol:0.005 mol:0.003 mol:0.002 mol of mole ratio by lithium nitrate, nickel nitrate,
Cobalt nitrate and manganese nitrate are added stirring in deionized water and all dissolve to metal salt;By the double chelatings of mixing that mole ratio is 1:1
Agent EDTA-PPA adds a small amount of deionized water to soak, and ammonium hydroxide is added, and shakes to formation colourless transparent solution, then colorless and transparent pair is chelated
Agent solution is added in inorganic salts uniform dielectric, forms the clear solution of bluish violet, 80 DEG C of heating stirrings to formation bluish violet colloidal sol;
80 DEG C of heating stirrings extremely form bluish violet colloidal sol;By gel rubber material in air dry oven 240 DEG C be heated to forming black it is more
The xerogel in hole;The black xerogel grind into powder that will be obtained, calcines 5 h at 850 DEG C of Muffle furnace and obtains
LiNi0.5Co0.3Mn0.2O2。
(2) by the LiNi in step (1)0.5Co0.3Mn0.2O2Positive silicic acid four is added in 80 DEG C of 15 min of stirring in aqueous solution
Ethyl ester, ethyl alcohol and Surfactant CTAB, 80 DEG C are continued to stir 1 h, are crosslinked tetraethyl orthosilicate with CTAB micella.
In ternary core outer cladding silica shell, m (tetraethyl orthosilicate): m(CTAB): m(ethyl alcohol)=0.5:0.1:1;To precipitate from
The heart, uses deionized water and ethanol washing 3 times respectively, and 80 DEG C of 5 h of drying of convection oven are placed in 600 DEG C of calcinings 5 in Muffle furnace
H obtains silica-ternary core-shell positive electrode (LiNi0.5Co0.3Mn0.2O2@meso-SiO2).
(3) 0.0075 mol silver oxide is dissolved in deionized water, 4 mL ammonium hydroxide is added dropwise after stirring 20 min, obtain solution
A;7.5 g PVP are dissolved in 100 mL deionized waters, stirring obtains solution B to transparent;Solution B is added drop-wise to solution A dropwise
In, 10 h of stirring are dripped, solution C is obtained;Step (2) products therefrom is added in solution C, solution D is obtained;By 0.0024 mol
Sodium borohydride be added dropwise in solution D continues stir 2 h, by obtained sediment deionized water and ethanol washing for several times after,
It filters, obtain final product LiNi after drying0.5Co0.3Mn0.2O2@Ag/meso-SiO2。
Embodiment three:
(1) by 0.01 mol:0.008 mol:0.001 mol:0.001 mol of mole ratio by lithium nitrate, nickel nitrate,
Cobalt nitrate and manganese nitrate are added stirring in deionized water and all dissolve to metal salt;By the double chelatings of mixing that mole ratio is 1:1
Agent EDTA-PPA adds a small amount of deionized water to soak, and ammonium hydroxide is added, and shakes to formation colourless transparent solution, then colorless and transparent pair is chelated
Agent solution is added in inorganic salts uniform dielectric, forms the clear solution of bluish violet, and 80 DEG C of heating stirrings are molten to bluish violet is formed
Glue;80 DEG C of heating stirrings extremely form bluish violet colloidal sol;Gel rubber material is heated to forming black for 240 DEG C in air dry oven
Porous xerogel;The black xerogel grind into powder that will be obtained, calcines 5 h at 850 DEG C of Muffle furnace and obtains
LiNi0.8Co0.1Mn0.1O2。
(2) by the LiNi in step (1)0.8Co0.1Mn0.1O2Positive silicic acid four is added in 80 DEG C of 15 min of stirring in aqueous solution
Ethyl ester, ethyl alcohol and Surfactant CTAB, 80 DEG C are continued to stir 1 h, are crosslinked tetraethyl orthosilicate with CTAB micella.
In ternary core outer cladding silica shell, m (tetraethyl orthosilicate): m(CTAB): m(ethyl alcohol)=0.5:0.1:1;To precipitate from
The heart, uses deionized water and ethanol washing 3 times respectively, and 80 DEG C of 5 h of drying of convection oven are placed in 600 DEG C of calcinings 5 in Muffle furnace
H obtains silica-ternary core-shell positive electrode (LiNi0.8Co0.1Mn0.1O2@meso-SiO2).
(3) 0.01 mol silver oxide is dissolved in deionized water, 4 mL ammonium hydroxide is added dropwise after stirring 20 min, obtain solution A;
10 g PVP are dissolved in 100 mL deionized waters, stirring obtains solution B to transparent;Solution B is added drop-wise in solution A dropwise, is dripped
10 h of stirring are added, solution C is obtained;Step (2) products therefrom is added in solution C, solution D is obtained;0.0048 mol is anti-bad
Hematic acid be added dropwise in solution D continues stir 2 h, by obtained sediment deionized water and ethanol washing for several times after, filter,
Final product LiNi is obtained after drying0.8Co0.1Mn0.1O2@Ag/meso-SiO2。
Claims (3)
1. a kind of preparation method for carrying silver-colored mesopore silicon oxide cladding tertiary cathode material, which is characterized in that the specific step of this method
Suddenly are as follows:
(1) by mole ratio 1:1-x-y:x:y(0 < x < 1,0 < y < 1) lithium salts, nickel salt, cobalt salt, manganese salt be dissolved in uniform dielectric
In, magnetic agitation makes to be completely dissolved to form solution E;A small amount of deionized water is added to soak double chelating agents that mole ratio is 1 ~ 2:1,
Ammonium hydroxide is added, shakes to formation colourless transparent solution, then colorless and transparent double chelating agent solutions are added in solution Es, forms bluish violet
Clear solution, 60 ~ 80 DEG C of heating stirrings are to forming bluish violet colloidal sol;And it is put in air dry oven and is added for 180 ~ 240 DEG C
Heat extremely forms the porous xerogel of black;By the porous xerogel grind into powder of obtained black, at 750 ~ 900 DEG C of Muffle furnace
5 ~ 10 h of lower calcining obtain tertiary cathode material;
(2) aqueous solution is made in the tertiary cathode material in step (1) and in 60 ~ 80 DEG C of 15 ~ 30min of stirring, positive silicic acid is added
Tetra-ethyl ester, ethyl alcohol and surfactant cetyl trimethylammonium bromide (CTAB), 60 ~ 80 DEG C are continued 1 ~ 2 h of stirring, make positive silicon
Sour tetra-ethyl ester is crosslinked with CTAB micella;In tertiary cathode material outer cladding silica shell, m (tetraethyl orthosilicate): m
(CTAB): m(ethyl alcohol)=0.25 ~ 0.5:0.05 ~ 0.1:1;Precipitating is centrifuged, uses deionized water and ethanol washing 2 ~ 3 times respectively,
50 ~ 80 DEG C of convection oven dry 5 ~ 8h are placed in 400 ~ 600 DEG C of 5 ~ 10 h of calcining in Muffle furnace, obtain silica-tertiary cathode
Material;
(3) 0.005 ~ 0.01 mol silver oxide is dissolved in deionized water, 4 ~ 10 mL ammonium hydroxide is added dropwise after stirring 10 ~ 20 min, obtain
To solution A;5 ~ 10 g PVP are dissolved in 100 mL deionized waters, stirring obtains solution B to transparent;Solution B is added drop-wise to dropwise
In solution A, 5 ~ 10 h of stirring is dripped, solution C is obtained;Step (2) products therefrom is added in solution C, solution D is obtained;It will
0.0016 ~ 0.0048 mol reducing agent, which is added dropwise in solution D, continues 2 ~ 4 h of stirring, the sediment deionized water that will be obtained
With ethanol washing for several times after, filter, drying after obtain final product;
The lithium salts is lithium nitrate, lithium carbonate, lithium chloride, lithium acetate, lithium citrate, lithium oxalate, lithium formate, lithium lactate or different
One of lithium propoxide or combinations thereof;
The nickel salt is nickel nitrate, nickel chloride, nickel acetate, nickel sulfate or one kind of nickel oxalate or combinations thereof;
The cobalt salt is cobalt nitrate, cobalt chloride, cobalt acetate, cobaltous sulfate or one kind of cobalt oxalate or combinations thereof;
The manganese salt is manganese nitrate, manganese chloride, manganese carbonate, manganese acetate or one kind of manganese oxalate or combinations thereof;
The uniform dielectric is deionized water, ethyl alcohol, acetone;
Double chelating agents be citric acid (CA), ethylenediamine tetra-acetic acid (EDTA), acetylacetone,2,4-pentanedione, in polyacrylic acid (PPA)
Any two kinds;
The reducing agent is sodium borohydride, ascorbic acid.
2. a kind of silver-colored mesopore silicon oxide of load coats tertiary cathode material, which is characterized in that prepare method according to claim 1
It obtains.
3. carrying application of the silver-colored mesopore silicon oxide cladding tertiary cathode material as lithium electricity positive electrode according to claim 2.
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