CN101510600A - Method for preparing positive electrode material of Li-ion battery using impact-flow equipment - Google Patents
Method for preparing positive electrode material of Li-ion battery using impact-flow equipment Download PDFInfo
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Abstract
The invention discloses a method which utilizes impinging stream equipment to prepare lithium ion battery anode materials. The method comprises the following steps: hydroxides or soluble salts of Li and soluble salts of transition metals are respectively dissolved into deionized water to form solutions, then the two solutions are impinged with each other in the impinging stream equipment at a speed of 2 m/s-30 m/s and react with each other, a sediment produced by the reaction is moved into a high temperature furnace after being washed and dried, calcined for 3h-15h at 300 DEG C-700 DEG C and then cooled down, finally a Li-ion battery anode material is obtained. The method provided by the invention has simple process, the reaction time can be effectively shortened and the production efficiency can be improved; the Li-ion battery anode material obtained by adopting the method has even grains, small grain size and high electrochemistry capacity.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, be specifically related to a kind of method of utilizing impact-flow equipment to prepare anode material for lithium-ion batteries.
Background technology
Lithium ion battery is released at first by Sony Corporation in 1991, till now, lithium ion battery provides power supply for a lot of electric equipments, uses lithium ion battery to do power supply mostly comprising mobile phone, notebook computer and some other portable electric equipment.And its demand is also more and more wider, and lithium ion battery has entered into the field of electric motor car and hybrid vehicle at present.
At present, the preparation method of anode material for lithium-ion batteries mainly contains solid-phase synthesis and liquid phase synthesizing method.In liquid phase synthesizing method, what be most widely used is coprecipitation.The advantage for preparing positive electrode with coprecipitation is that raw material mixes more even, need not repeat repeatedly roasting and grinding, and its anode material for lithium-ion batteries particle of producing is less.But also there are some shortcomings in this method:
(1) reaction efficiency is low, and reaction time is long
In coprecipitation, the preparation presoma all is to mix with paddle usually, and reaction efficiency is low, generally all needs to stir 5～15h and does not wait, and reaction time is longer.
(2) the product electrochemistry capacitance is low
The product that general coprecipitation is prepared is than the electrochemistry capacitance height of the product of conventional solid-state method preparation, and is still still not ideal enough, with the big in addition gap of theoretical capacity of positive electrode.
The notion of percussion flow (Impinging Streams, note by abridging be IS) is at first proposed in 1961 by Elperin.Its principle is two strands of two phase flows flow at high speed bumps in opposite directions, and the result causes the impingement region of height turbulence between two accelerating tubes.With the gas-solid percussion flow is example, and its principle is that air-flow axial velocity on striking face is tending towards 0 and transfer Radial Flow to, but particle mat inertia infiltrate reverse flow and the moment that begins to infiltrate alternate relative velocity reach maximum; Slowing down under the frictional resistance effect subsequently decays to 0 up to axial velocity, is reversed acceleration subsequently again and moves to striking face, and may infiltrate original air-flow once more.Till now, percussion flow has been applied to a lot of fields, comprises gas-solid, gas-liquid, liquid liquid etc.Verified, percussion flow is to transmit one of effective method of the transmittance process of especially outdiffusion control between hardening constituent, and the comparable conventional method of carry-over factor improves several times to tens times, and this characteristic is subjected to common concern.Another result that bump causes greatly promotes to mix, and especially microcosmic mixes.In recent years, people begin this characteristic is used for producing superfine powder by chemical reaction, as application number is that 200410072307.9 patent application discloses a kind of method of percussion flow of utilizing and prepares high purity magnesium hydrate, publication number is that the Chinese patent of CN1757597 discloses a kind of percussion flow prepared in reaction porous calcium carbonate superfine powder that utilizes, product product lover, the production efficiency height, but percussion flow be reflected at the preparation of anode material for lithium-ion batteries and produce in also do not use.
Summary of the invention
The objective of the invention is to overcome the shortcoming of prior art, a kind of method of utilizing impact-flow equipment to prepare anode material for lithium-ion batteries is provided.The inventive method has promoted the mixing of reactant microcosmic greatly, reaction time is short, the production efficiency height, reacted presoma can obtain the anode material for lithium-ion batteries that pattern is good, electrochemistry capacitance is high through low furnace temperature, the sintering of short period, has good application prospects.
The object of the invention is achieved through the following technical solutions:
A kind of method of utilizing impact-flow equipment to prepare anode material for lithium-ion batteries:
The hydroxide of lithium or soluble-salt be dissolved in make solution in the deionized water, the soluble-salt of transition metal is dissolved in makes solution in the deionized water, then these two kinds of solution are clashed in impact-flow equipment mutually with the speed of 2～30m/s and react, the precipitation that obtains moves in the high temperature furnace after washing drying, calcine 3～15h down at 300～700 ℃, promptly get anode material for lithium-ion batteries after the cooling.
Described transition metal is selected from one or more in nickel, cobalt, manganese, iron, the vanadium.
The soluble-salt of described transition metal is selected from one or more in nitrate, sulfate, the acetate.
The soluble-salt of described transition metal is dissolved in deionized water make solution before, mix the hydroxide of boron, magnesium, aluminium, cobalt, nickel, manganese, vanadium, chromium, calcium, yttrium, thulium, gadolinium, holmium, lanthanum, neodymium, fluorine, phosphorus or in the soluble-salt one or more.
The soluble-salt of described transition metal is dissolved in deionized water make solution before, mix the hydroxide of carbon source and boron, magnesium, aluminium, cobalt, nickel, manganese, vanadium, chromium, calcium, yttrium, thulium, gadolinium, holmium, lanthanum, neodymium, fluorine, phosphorus or in the soluble-salt one or more; Described carbon source comprises glucose or sucrose, and carbon source accounts for target end-product 5～20% quality.
The soluble-salt of the hydroxide of described lithium or soluble-salt and transition metal, and the boron that mixes, magnesium, aluminium, cobalt, nickel, manganese, vanadium, chromium, calcium, yttrium, thulium, gadolinium, holmium, lanthanum, neodymium, fluorine, the hydroxide of phosphorus or the mol ratio of soluble-salt are: molar fraction * (1～1.1) of lithium in target end-product chemical formula: the molar fraction of transition metal in target end-product chemical formula: the molar fraction of doping element in target end-product chemical formula; That is:
If target end-product chemical formula is Li
pA
yM
xB
zO
nIn, described M is cobalt, nickel, manganese, iron or vanadium; A, B are respectively boron, magnesium, aluminium, cobalt, nickel, manganese, vanadium, chromium, calcium, yttrium, thulium, gadolinium, holmium, lanthanum, neodymium, fluorine, phosphorus; P, x, y, z, n are respectively Li, M, A, B, the molal quantity of O element in target end-product chemical formula, then
The soluble-salt of the hydroxide of described lithium or soluble-salt and transition metal, and the boron that mixes, magnesium, aluminium, cobalt, nickel, manganese, vanadium, chromium, calcium, yttrium, thulium, gadolinium, holmium, lanthanum, neodymium, fluorine, the hydroxide of phosphorus or the mol ratio of soluble-salt are: 1～1.1 * p:x:y:z.
Feed gas in the described high temperature furnace, described gas is one or more in nitrogen, argon gas, air, hydrogen, the oxygen.
Impact-flow equipment among the present invention is free impact-flow equipment (as Fig. 1), compares with the submergence impact-flow equipment, and microcosmic in the free impact-flow equipment mixes obviously stronger than submergence percussion flow because two strands in opposite directions fluid can adopt very high service speed.At two strands of high-pressure fluids of two nozzle ejections of its upper side, the turbulence impingement region that collision jet produces is on the stable state liquid level of impact-flow equipment, and the speed that reaction mass enters the import of impact-flow equipment impingement region is 2～30m/s.
The present invention both can be used for preparing anode material for lithium-ion batteries such as LiMn2O4, lithium nickelate, LiFePO 4, cobalt acid lithium, lithium vanadate, the nickel cobalt manganese lithium of non-impurity-doped element, also can be used to prepare anode material for lithium-ion batteries such as the LiMn2O4 that covers carbon or contain doped chemical, lithium nickelate, LiFePO 4, cobalt acid lithium, lithium vanadate, nickel cobalt manganese lithium.
The present invention compared with prior art has following advantage and beneficial effect:
(1) reaction efficiency height, good product performance
When the head-on collision reaction takes place two strands of liquid materials, form a turbulent flow impingement region in impact-flow equipment, promoted the mixing of its microcosmic greatly, the reaction time is short, the production efficiency height.The presoma that the reaction back generates is through low furnace temperature, and the sintering of short period can obtain the anode material for lithium-ion batteries of pattern and better performances.
(2) product electrochemistry capacitance height
Utilize the synthetic anode material for lithium-ion batteries that obtains of percussion flow reaction, particle diameter is little, and uniform particles has significantly improved the electrochemistry capacitance of positive electrode, can be through mixing near its theoretical capacity, and product is stable, is fit to industrialization development.
Description of drawings
Fig. 1 is the structural representation of free impact-flow equipment.
The 1-material inlet, the 2-material outlet
Embodiment
Free impact-flow equipment such as Fig. 1, material 1 enters impact-flow equipment through entering the mouth, and drives two strands of materials with pump and at the equipment impingement region head-on collision reaction takes place with certain speed, and the precipitation that obtains derives from material outlet 2.Can add a paddle or magnetic stirring apparatus as required.
Embodiment 1
With lithium nitrate, manganese nitrate takes by weighing by Li:Mn=1:1, is dissolved in respectively making solution in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 2m/s and reacts, and it is an amount of to add sodium carbonate in impact-flow equipment, regulates pH=10.The precipitation that obtains is moved into after washing drying in the high temperature furnace, at 600 ℃ of calcining 12h, obtains LiMn after the cooling
2O
4Positive electrode.The product electrochemistry capacitance is 120mAh/g, and cycle performance is good.
With lithium nitrate, manganese nitrate is by Li:Mn=1.03: 1 takes by weighing, and is dissolved in respectively making solution in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 10m/s and reacts.It is an amount of to add sodium carbonate in impact-flow equipment, regulates pH=10.The precipitation that obtains is moved into after washing drying in the high temperature furnace, at 600 ℃ of calcining 10h, obtains LiMn
2O
4Positive electrode.The product electrochemistry capacitance is 122mAh/g, and cycle performance is good.
Embodiment 3
Lithium nitrate, nickel nitrate Li:Ni=1:1 in molar ratio take by weighing, and are dissolved in respectively making solution in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 7m/s and react.The precipitation that obtains is moved into after washing drying in the high temperature furnace, and at 700 ℃ of calcining 10h, cooling obtains LiNiO
2Positive electrode, product cut size is little, and electrochemistry capacitance reaches 170mAh/g and even, and cycle performance is good.
Embodiment 4
Lithium nitrate, nickel nitrate Li:Ni=1.02:1 in molar ratio take by weighing, and are dissolved in respectively making solution in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 8m/s and react.The precipitation that obtains is moved into after washing drying in the high temperature furnace, and at 650 ℃ of calcining 15h, cooling obtains LiNiO
2Positive electrode, product cut size is little, and electrochemistry capacitance reaches 175mAh/g and even, and cycle performance is good.
Embodiment 5
Nickel nitrate, cobalt nitrate 4:1 in molar ratio takes by weighing, be dissolved in and make solution 1 in the deionized water, get again with (Ni+Co) equimolar lithium hydroxide and be dissolved in the deionized water, add NaOH or ammoniacal liquor and regulate pH=7～8, make solution 2, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 10m/s and react.The precipitation that obtains is moved into after washing drying in the high temperature furnace, at 600 ℃ of calcining 15h, obtains LiNi after the cooling
0.8Co
0.2O
2Positive electrode.The product electrochemistry capacitance is 160mAh/g, and cycle performance is good.
Embodiment 6
With Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide takes by weighing by the mol ratio of Fe:P:Li=1:1:1, with Fe (NO
3)
2, NH
4H
2PO
4Be dissolved in and make solution 1 in the deionized water, lithium hydroxide is dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 7m/s and reacts.The precipitation that obtains is moved into after washing drying in the tube type high-temperature furnace, and under the Ar protection, 300 ℃ of calcining 3h promptly get LiFePO
4Positive electrode.The product electrochemistry capacitance is 126mAh/g, and cycle performance is good.
Embodiment 7
With FeSO
4, NH
4H
2PO
4, lithium hydroxide takes by weighing by the mol ratio of Fe:P:Li=1:1:1.02, with FeSO
4, NH
4H
2PO
4Be dissolved in and make solution 1 in the deionized water, lithium hydroxide is dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 8m/s and reacts.The precipitation that obtains is moved into after washing drying in the tube type high-temperature furnace, and under the Ar protection, 600 ℃ of calcining 6h promptly get LiFePO
4Positive electrode.The product electrochemistry capacitance is 130mAh/g, and cycle performance is good.
Embodiment 8
With Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide takes by weighing by the mol ratio of Fe:P:Li=1:1:1.05, with Fe (NO
3)
2, NH
4H
2PO
4Be dissolved in and make solution 1 in the deionized water, lithium hydroxide is dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 7m/s and reacts.The precipitation that obtains is moved into after washing drying in the tube type high-temperature furnace, at N
2Protection is calcined 10h, is promptly got LiFePO for 600 ℃ down
4Positive electrode.The product electrochemistry capacitance is 128mAh/g, and cycle performance is good.
Embodiment 9
With FeSO
4, NH
4H
2PO
4, lithium hydroxide takes by weighing by the mol ratio of Fe:P:Li=1:1:1.02, with FeSO
4, NH
4H
2PO
4Be dissolved in and make solution 1 in the deionized water, lithium hydroxide is dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 8m/s and reacts.The precipitation that obtains is moved into after washing drying in the tube type high-temperature furnace, and under nitrogen protection, 700 ℃ of calcining 6h promptly get LiFePO
4Positive electrode.The product electrochemistry capacitance is 130mAh/g, and cycle performance is good.
Embodiment 10
With Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide takes by weighing by the mol ratio of Fe:P:Li=1:1:1.03, takes by weighing to account for target end-product mass fraction 15% (with product LiFePO again
4The quality of/C positive electrode is calculated) sucrose, with Fe (NO
3)
2, NH
4H
2PO
4, sucrose is dissolved in and makes solution 1 in the deionized water, lithium hydroxide is dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 15m/s and react.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 5h, is promptly got LiFePO for 550 ℃ down
4/ C positive electrode.The product electrochemistry capacitance is 150mAh/g, and cycle performance is good.
Embodiment 11
With Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide takes by weighing by the mol ratio of Fe:P:Li=1:1:1.02, takes by weighing to account for target end-product mass fraction 5% (with product LiFePO again
4The quality of/C positive electrode is calculated) glucose, with Fe (NO
3)
2, NH
4H
2PO
4, glucose is dissolved in and makes solution 1 in the deionized water, lithium hydroxide is dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 30m/s and react.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 9h, is promptly got LiFePO for 550 ℃ down
4/ C positive electrode.The product electrochemistry capacitance is 155mAh/g, and cycle performance is good.
Embodiment 12
With Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide takes by weighing by the mol ratio of Fe:P:Li=1:1:1.02, takes by weighing to account for target end-product mass fraction 5% (with product LiFePO again
4The quality of/C positive electrode is calculated) glucose, with Fe (NO
3)
2, NH
4H
2PO
4, glucose is dissolved in and makes solution 1 in the deionized water, lithium hydroxide is dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 8m/s and react.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 8h, is promptly got LiFePO for 600 ℃ down
4/ C positive electrode.The product electrochemistry capacitance is 152mAh/g, and cycle performance is good.
Embodiment 13
Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide, magnesium acetate takes by weighing by the mol ratio of Fe:P:Li:Mg=1:1:0.98:0.02, takes by weighing to account for target end-product mass fraction 15% (with product Li again
0.98Mg
0.02FePO
4The quality of/C positive electrode is calculated) sucrose, with Fe (NO
3)
2, NH
4H
2PO
4Be dissolved in sucrose and make solution 1 in the deionized water, lithium hydroxide, magnesium acetate are dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 12m/s and reacts.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 5h, is promptly got Li for 600 ℃ down
0.98Mg
0.02FePO
4/ C positive electrode.The product electrochemistry capacitance is 159mAh/g, and cycle performance is good.
Embodiment 14
Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide, magnesium acetate takes by weighing by the mol ratio of Fe:P:Li:Mg=1:1:0.99:0.01, takes by weighing to account for target end-product mass fraction 10% (with product Li again
0.99Mg
0.01FePO
4The quality of/C is calculated) sucrose, with Fe (NO
3)
2, NH
4H
2PO
4, sucrose is dissolved in and makes solution 1 in the deionized water, lithium hydroxide, magnesium acetate are dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 8m/s and react.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 5h, is promptly got Li for 600 ℃ down
0.99Mg
0.01FePO
4/ C positive electrode.The product electrochemistry capacitance is 156mAh/g, and cycle performance is good.
Embodiment 15
Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide, chromium chloride takes by weighing by the mol ratio of Fe:P:Li:Cr=1:1:0.99:0.01, takes by weighing to account for target end-product mass fraction 5% (with product Li again
0.99Cr
0.01FePO
4The quality of/C positive electrode is calculated) sucrose, with Fe (NO
3)
2, NH
4H
2PO
4, sucrose is dissolved in and makes solution 1 in the deionized water, lithium hydroxide, chromium chloride are dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 10m/s and react.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 6h, is promptly got Li for 600 ℃ down
0.99Cr
0.01FePO
4/ C positive electrode.The product electrochemistry capacitance is 160mAh/g, and cycle performance is good.
Embodiment 16
Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide, chromium chloride takes by weighing by the mol ratio of Fe:P:Li:Cr=1:1:0.98:0.02, takes by weighing to account for target end-product mass fraction 5% (with product Li again
0.98Cr
0.02FePO
4The quality of/C positive electrode is calculated) glucose, with Fe (NO
3)
2, NH
4H
2PO
4, glucose is dissolved in and makes solution 1 in the deionized water, lithium hydroxide, chromium chloride are dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 15m/s and react.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 10h, is promptly got Li for 650 ℃ down
0.98Cr
0.02FePO
4/ C positive electrode.The product electrochemistry capacitance is 162mAh/g, and cycle performance is good.
Embodiment 17
FeSO
4, NH
4H
2PO
4, lithium hydroxide, manganese sulfate takes by weighing by the mol ratio of Li:P:Fe:Mn=1:1:0.9:0.1.With FeSO
4, NH
4H
2PO
4Be dissolved in and make solution 1 in the deionized water, lithium hydroxide, manganese sulfate are dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 6m/s and reacts.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 10h, is promptly got LiFe for 600 ℃ down
0.9Mn
0.1PO
4Positive electrode.The product electrochemistry capacitance is 155mAh/g, and cycle performance is good.
Embodiment 18
FeSO
4, NH
4H
2PO
4, lithium hydroxide, manganese sulfate takes by weighing by the mol ratio of Li:P:Fe:Mn=1:1:0.9:0.1, takes by weighing mass fraction 20% again (with product LiFe
0.9Mn
0.1PO
4The quality of/C positive electrode is calculated) sucrose, with FeSO
4, NH
4H
2PO
4, sucrose is dissolved in and makes solution 1 in the deionized water, lithium hydroxide, manganese sulfate are dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 9m/s and react.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 12h, is promptly got LiFe for 600 ℃ down
0.9Mn
0.1PO
4/ C positive electrode.The product electrochemistry capacitance is 165mAh/g, and cycle performance is good.
Embodiment 19
Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide, aluminum sulfate takes by weighing by the mol ratio of Fe:P:Li:Al=1:1:0.97:0.03, with Fe (NO
3)
2, NH
4H
2PO
4Be dissolved in and make solution 1 in the deionized water, lithium hydroxide, aluminum sulfate are dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 6m/s and reacts.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 5h, is promptly got Li for 600 ℃ down
0.97Al
0.03FePO
4Positive electrode.The product electrochemistry capacitance is 150mAh/g, and cycle performance is good.
Embodiment 20
Fe (NO
3)
2, NH
4H
2PO
4, lithium hydroxide, aluminum sulfate takes by weighing by the mol ratio of Fe:P:Li:Al=1:1:0.97:0.03, takes by weighing mass fraction 15% again (with product Li
0.97Al
0.03FePO
4The quality of/C positive electrode is calculated) sucrose, with Fe (NO
3)
2, NH
4H
2PO
4, sucrose is dissolved in and makes solution 1 in the deionized water, lithium hydroxide, aluminum sulfate are dissolved in makes solution 2 in the deionized water, these two kinds of solution are clashed into mutually in impact-flow equipment with the speed of 10m/s and react.The precipitation that obtains is moved in the tube type high-temperature furnace, at N after washing drying
2Protection is calcined 12h, is promptly got Li for 650 ℃ down
0.97Al
0.03FePO
4/ C positive electrode.The product electrochemistry capacitance is 158mAh/g, and cycle performance is good.
Claims (8)
1, a kind of method of utilizing impact-flow equipment to prepare anode material for lithium-ion batteries is characterized in that:
The hydroxide of lithium or soluble-salt be dissolved in make solution in the deionized water, the soluble-salt of transition metal is dissolved in makes solution in the deionized water, then these two kinds of solution are clashed in impact-flow equipment mutually with the speed of 2～30m/s and react, the precipitation that obtains moves in the high temperature furnace after washing drying, calcine 3～15h down at 300～700 ℃, promptly get anode material for lithium-ion batteries after the cooling.
2, method according to claim 1 is characterized in that described transition metal is selected from one or more in nickel, cobalt, manganese, iron, the vanadium.
3, method according to claim 1, the soluble-salt that it is characterized in that described transition metal is selected from one or more in nitrate, sulfate, the acetate.
4, method according to claim 1, before it is characterized in that soluble-salt at described transition metal is dissolved in deionized water and makes solution, mix the hydroxide of boron, magnesium, aluminium, cobalt, nickel, manganese, vanadium, chromium, calcium, yttrium, thulium, gadolinium, holmium, lanthanum, neodymium, fluorine, phosphorus or in the soluble-salt one or more.
5, method according to claim 1, before it is characterized in that soluble-salt at described transition metal is dissolved in deionized water and makes solution, mix the hydroxide of carbon source and boron, magnesium, aluminium, cobalt, nickel, manganese, vanadium, chromium, calcium, yttrium, thulium, gadolinium, holmium, lanthanum, neodymium, fluorine, phosphorus or in the soluble-salt one or more; Described carbon source comprises glucose or sucrose, and carbon source accounts for target end-product 5～20% quality.
6, method according to claim 4, it is characterized in that the hydroxide of described lithium or the soluble-salt of soluble-salt and transition metal, and the boron that mixes, magnesium, aluminium, cobalt, nickel, manganese, vanadium, chromium, calcium, yttrium, thulium, gadolinium, holmium, lanthanum, neodymium, fluorine, the hydroxide of phosphorus or the mol ratio of soluble-salt are: molar fraction * (1～1.1) of lithium in target end-product chemical formula: the molar fraction of transition metal in target end-product chemical formula: the molar fraction of doping element in target end-product chemical formula.
7, method according to claim 5 is characterized in that feeding in the described high temperature furnace gas.
8, method according to claim 6 is characterized in that described gas is one or more in nitrogen, argon gas, air, hydrogen, the oxygen.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100380692A CN101510600B (en) | 2009-03-20 | 2009-03-20 | Method for preparing positive electrode material of Li-ion battery using impact-flow equipment |
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|---|---|---|---|
| CN2009100380692A CN101510600B (en) | 2009-03-20 | 2009-03-20 | Method for preparing positive electrode material of Li-ion battery using impact-flow equipment |
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| CN101510600A true CN101510600A (en) | 2009-08-19 |
| CN101510600B CN101510600B (en) | 2011-07-20 |
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| CN2009100380692A Expired - Fee Related CN101510600B (en) | 2009-03-20 | 2009-03-20 | Method for preparing positive electrode material of Li-ion battery using impact-flow equipment |
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Cited By (5)
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| CN102234511A (en) * | 2011-08-17 | 2011-11-09 | 中南大学 | Method for preparing yellow fluorescent powder for white light-emitting diode (LED) |
| US20130252109A1 (en) * | 2010-09-08 | 2013-09-26 | Sk Innovation Co., Ltd. | Positive Electrode Active Material for Lithium Secondary Battery and Method for Preparing the Same |
| CN106848321A (en) * | 2017-02-23 | 2017-06-13 | 深圳市贝特瑞纳米科技有限公司 | A kind of metal oxide coats the preparation method of cell positive material |
| CN109921013A (en) * | 2017-12-13 | 2019-06-21 | 微宏动力系统（湖州）有限公司 | A kind of positive electrode material precursor of modification, preparation method, modification positive electrode and lithium battery |
| CN115430432A (en) * | 2022-08-24 | 2022-12-06 | 重庆理工大学 | Oxidation catalyst Li 2 Mn 0.9 Co 0.1 O 3 And method for preparing the same |
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| DE10223567A1 (en) * | 2002-05-27 | 2003-12-11 | Bernd Penth | Production of micro- and nano-particles, e.g. metal oxide or titanate for making electroceramic product, involves precipitation by impinging streams of hot aqueous metal salt and alkali hydroxide solutions in microjet reactor |
| CN2696710Y (en) * | 2004-02-24 | 2005-05-04 | 武汉化工学院 | Impact stream gas and liquid reactor |
| CN100364656C (en) * | 2005-02-05 | 2008-01-30 | 中国石油化工股份有限公司 | Impact flow reactor for liquid-phase reaction |
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2009
- 2009-03-20 CN CN2009100380692A patent/CN101510600B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130252109A1 (en) * | 2010-09-08 | 2013-09-26 | Sk Innovation Co., Ltd. | Positive Electrode Active Material for Lithium Secondary Battery and Method for Preparing the Same |
| US9825294B2 (en) * | 2010-09-08 | 2017-11-21 | Sk Innovation Co., Ltd. | Positive electrode active material for lithium secondary battery and method for preparing the same |
| CN102234511A (en) * | 2011-08-17 | 2011-11-09 | 中南大学 | Method for preparing yellow fluorescent powder for white light-emitting diode (LED) |
| CN106848321A (en) * | 2017-02-23 | 2017-06-13 | 深圳市贝特瑞纳米科技有限公司 | A kind of metal oxide coats the preparation method of cell positive material |
| CN109921013A (en) * | 2017-12-13 | 2019-06-21 | 微宏动力系统（湖州）有限公司 | A kind of positive electrode material precursor of modification, preparation method, modification positive electrode and lithium battery |
| CN109921013B (en) * | 2017-12-13 | 2022-06-24 | 微宏动力系统（湖州）有限公司 | Modified positive electrode material precursor, preparation method thereof, modified positive electrode material and lithium battery |
| CN115430432A (en) * | 2022-08-24 | 2022-12-06 | 重庆理工大学 | Oxidation catalyst Li 2 Mn 0.9 Co 0.1 O 3 And method for preparing the same |
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| CN101510600B (en) | 2011-07-20 |
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