CN104466154B - A kind of preparation method of lithium ion battery anode material nickel cobalt aluminium - Google Patents

A kind of preparation method of lithium ion battery anode material nickel cobalt aluminium Download PDF

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CN104466154B
CN104466154B CN201410750308.8A CN201410750308A CN104466154B CN 104466154 B CN104466154 B CN 104466154B CN 201410750308 A CN201410750308 A CN 201410750308A CN 104466154 B CN104466154 B CN 104466154B
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nickel cobalt
ion battery
lithium ion
battery anode
cobalt aluminium
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CN201410750308.8A
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Chinese (zh)
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CN104466154A (en
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朱永明
胡会利
阮泽文
滕祥国
于元春
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哈尔滨工业大学(威海)
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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/485Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of or comprising active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/48Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525Selection 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
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

The invention discloses a kind of preparation method of lithium ion battery anode material nickel cobalt aluminium, comprises the following steps:Nickel, cobalt and aluminum salt solution are mixed, coprecipitation reaction is carried out again in mixed solution cocurrent addition reactor by precipitating reagent, complexing agent with above-mentioned nickel cobalt aluminium, regulation system pH value is 10 ~ 11, temperature is 40 ~ 60 DEG C, and mixing speed is 500 ~ 1500 revs/min, after 10 ~ 30 h of reaction, filtered, washing, dries, obtains hydroxide precursor;Presoma high temperature pre-sintering is obtained nickel cobalt aluminum oxide, then is mixed with lithium source, high temperature sintering under oxygen atmosphere obtains nickel cobalt aluminium powder after broken and screening.The burn tinctuer pre-sintered by calculating presoma, and with Ni in nickel cobalt aluminum oxide under the different pre-sintering temperatures of XPS analysis2+And Ni3+Content, obtain Ni3+Content highest nickel cobalt aluminum oxide, is converted into Ni with more nickel ions during promoting double sintering3+, reduce Li+With Ni2+Mixing, improve material chemical property.

Description

A kind of preparation method of lithium ion battery anode material nickel cobalt aluminium

Technical field

The present invention relates to energy storage material and electrochemical field, especially a kind of system of lithium ion battery anode material nickel cobalt aluminium Preparation Method.

Background technology

Since Japanese Sony Corporation in 1991 successfully develops first and realizes the commercialization of lithium ion battery, lithium ion Battery is increasingly paid close attention to by people, due to its light weight, small volume, specific energy height, little self discharge, good cycle, dirt The features such as contaminating little and memory-less effect, becomes one of green secondary cell of 21 century most application prospect.With electrode The development of material, occurs the cell positive material for differing from one another, such as cobalt acid lithium, lithium nickelate, LiMn2O4, LiFePO4 and nickel in succession Cobalt-manganese ternary material etc..Lithium ion battery is more in national defense industry, space technology, portable electric appts and electric automobile etc. at present Individual field is used widely, and therefore requirement of the people to lithium ion battery also more and more higher, such as has a safety feature, specific capacity Height, cycle performance are excellent, light weight small volume etc., but battery material ripe at present is difficult to while meeting above items Performance.LiNi1-x-yCoxA1yO2(NCA) be at present industrial applications specific capacity highest positive electrode, with cyclicity The good, abundant raw materials of energy and the more low advantage of cost, are a kind of lithium ion power battery cathode materials of great application prospect.

Current ternary material LiNi1-x-yCoxA1yO2Synthetic method mainly have coprecipitation, high temperature solid-state method, colloidal sol-solidifying Glue method, molte-salt synthesis, spray drying process, microwave method, hydro-thermal method and combustion method etc., but LiNi prepared by every kind of method1-x- yCoxA1yO2Material still has several drawbacks part, is further improved.Wherein, coprecipitation process is simple to operate, synthesis Material property preferably, be a kind of method of most industrial applications prospect.

When prior art prepares lithium ion battery anode material nickel cobalt aluminium, prepared before nickel cobalt aluminium hydroxide by being co-precipitated Body is driven, directly mix with lithium source or is mixed with lithium source after high temperature is pre-sintered, then obtain through high temperature sintering and follow-up break process Arrive nickel cobalt aluminium positive electrode.Nickel cobalt aluminium oxyhydroxide, mainly nickel hydroxide are decomposed more than 230 DEG C, generate NiO, When temperature reaches 400 DEG C, part NiO absorption airs are simultaneously oxidized to Ni2O3, finally when temperature is higher than more than 600 DEG C, Ni2O3 It is reduced SA NiO;In addition, if nickelous too high levels in nickel cobalt aluminum oxide, follow-up sintering process can not be complete Nickelic is oxidized to, nickelous with lithium ion radius closely, easily produces mixing phenomenon, affects material electrochemical Energy.Therefore, different temperatures pre-sintering obtains different Ni2+And Ni3+The presoma of content, final material chemical property are different.

Content of the invention

The problem solved required for of the invention is to improve a kind of preparation method of lithium ion battery anode material nickel cobalt aluminium, should Method is preparation nickel cobalt aluminium positive electrode under different pre-sintering temperature parts, and the burning for calculating the nickel cobalt aluminum oxide after pre-sintering is lost Rate, and use x-ray photoelectron power spectrum(XPS)Analysis wherein Ni2+And Ni3+Content, obtains Ni3+Content highest nickel cobalt aluminum oxidation Thing, during promoting double sintering, more nickel ions are converted into Ni3+, reduce Li+With Ni2+Mixing, prepare electrochemistry The good nickel cobalt aluminium positive electrode of energy.

For solving above-mentioned technical problem, the technical scheme is that:A kind of lithium ion battery anode material nickel cobalt aluminium Preparation method, comprises the following steps:

(1)The preparation of nickel cobalt aluminium presoma:Nickel salt solution, cobalt salt solution and aluminum salt solution are mixed, after mixing in solution Concentration of metal ions be 0.5mol/L ~ 2.0mol/L, then will precipitant solution, enveloping agent solution and above-mentioned nickel cobalt aluminium mixed Closing in reactor of the solution by the addition of constant flow pump together cocurrent equipped with bottom liquid carries out coprecipitation reaction, and control ph, temperature are stirred After mixing 10 ~ 30h, filtered, repeatedly washed, dried, obtain lithium ion battery anode material nickel cobalt aluminium hydroxide presoma;

(2)The preparation of nickel cobalt aluminium positive electrode:The nickel cobalt aluminum oxide that will be obtained after the pre-sintering of presoma high temperature, calculates high Burn tinctuer after warm pre-sintering with XPS analysis wherein Ni2+And Ni3+Content, then mix with lithium source, high under oxygen atmosphere Temperature sintering, obtains lithium ion battery anode material nickel cobalt aluminium powder after broken and screening.

The present invention burn tinctuer pre-sintered by calculating presoma, and different pre-sintered with X-ray photoelectron spectroscopic analysis At a temperature of obtain Ni in nickel cobalt aluminum oxide2+And Ni3+Content, obtain Ni3+The most nickel cobalt aluminum oxide of content, can promote During entering double sintering, more nickel ions are converted into Ni3+, reduce Li+With Ni2+Mixing, improve material electrochemistry Energy.

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described nickel salt, cobalt salt and aluminium salt are preferably Nitrate, according to Ni: Co: Al mol ratio 0.80: 0.15: 0.05;

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described precipitating reagent be preferably 1mol/L ~ The sodium hydroxide solution of 5mol/L;

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described complexing agent is preferably 4 ~ 10mol/L Ammonia spirit;

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described bottom liquid is preferably 4 ~ 10mol/L's Ammonia spirit;

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described step(1)In pH value be preferably 10~11;

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described step(1)In temperature be preferably 40~60℃;

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described step(1)In mixing speed excellent Elect 500 ~ 1500 revs/min as;

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described step(2)In pre-sintering preferably For 500 ~ 750 DEG C of 2 ~ 8h of insulation, programming rate is 1 ~ 6 DEG C/min;

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described step(2)In sintering be preferably 750 ~ 850 DEG C of 10 ~ 20h of insulation, programming rate is 1 ~ 6 DEG C/min;

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described step(2)In nickel cobalt aluminum oxidation The mol ratio of thing and lithium source is preferably 1:(1~1.05);

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described step(2)In lithium source be preferably Lithium hydroxide, lithium carbonate, lithium nitrate, lithium sulfate, lithium oxalate, lithium acetate, one or more in lithium chloride;

In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described step(2)In Ni2+And Ni3+Contain The analysis method of amount is preferably burn tinctuer and X-ray photoelectron spectroscopic analysis method.

Compared with prior art, the lithium ion battery anode material nickel cobalt aluminium that prepared by the inventive method has following beneficial effect Really:

(1)When optimum temperature is pre-sintered, presoma thoroughly can decompose, low activity in the nickel cobalt aluminum oxide for obtaining Ni2+Content is few, improves the chemical property of material;

(2)After optimum temperature pre-sintering, Ni is obtained3+Content highest oxidation of precursor thing, material when reducing double sintering Li in material+And Ni2+Mixing phenomenon, improve material chemical property;

(3)Synthetic material has high reversible specific capacity, and cyclical stability is good, in the range of 2.5 ~ 4.3V, electric discharge ratio Capacity is more than 170mAh/g.

Description of the drawings

Fig. 1 be embodiment 1 pre-sintering after nickel cobalt aluminum oxide XRD spectrum;

Fig. 2 be embodiment 1 pre-sintering after nickel cobalt aluminum oxide XPS collection of illustrative plates;

Fig. 3 is the first charge-discharge curve of the product of embodiment 1;

Fig. 4 is the cycle performance figure of the product of embodiment 1;

Fig. 5 be embodiment 2 pre-sintering after nickel cobalt aluminum oxide XRD spectrum;

Fig. 6 be embodiment 2 pre-sintering after nickel cobalt aluminum oxide XPS collection of illustrative plates;

Fig. 7 is the first charge-discharge curve of the product of embodiment 2;

Fig. 8 is the cycle performance figure of the product of embodiment 2;

Fig. 9 be embodiment 3 pre-sintering after nickel cobalt aluminum oxide XRD spectrum;

Figure 10 be embodiment 3 pre-sintering after nickel cobalt aluminum oxide XPS collection of illustrative plates;

Figure 11 is the first charge-discharge curve of the product of embodiment 3;

Figure 12 is the cycle performance figure of the product of embodiment 3.

Specific embodiment

Below in conjunction with Figure of description and specific embodiment, the invention will be further described.

Embodiment 1

With nickel nitrate, cobalt nitrate and aluminum nitrate as raw material, according to Ni: Co: Al mol ratio 0.8: 0.15: 0.05, it is configured to Ammonia spirit of the mixed solution with the sodium hydroxide solution and 6mol/L of 2mol/L is passed through constant flow pump by the mixed solution of 1mol/L Cocurrent is added in the reactor of 2L, and it is ammonia spirit that 10.5, temperature is 50 DEG C the bottom of as to fill 600mL, pH value in reactor Liquid, mixing speed are 600 revs/min, carry out precipitation reaction, and control ph fluctuation during being somebody's turn to do is less than ± 0.4, temperature fluctuation Less than ± 1 DEG C, after precipitation reaction is complete, filtered, for several times, until filtrate pH value is close to 7, in filtrate, nitrate anion contains for washing Amount is less than 1 × 10-5Mol/L, is vacuum dried at 120 DEG C, obtains graminaceous nickel cobalt aluminium hydroxide presoma;

By the nickel cobalt aluminium presoma prepared in above-mentioned steps in tube type resistance furnace 750 DEG C of pre-burning 2h, programming rate is 5 DEG C/min, nickel cobalt aluminum oxide is obtained, then with lithium hydroxide according to mol ratio 1:1.05 are well mixed, and are placed in the pipe of oxygen atmosphere 800 DEG C of sintering 12h in formula resistance furnace, programming rate is 5 DEG C/min, is just obtaining lithium ion battery through broken and screening after cooling Pole material nickel cobalt aluminium powder.

After testing, in the present embodiment the pre-sintered burn tinctuer of presoma high temperature is 8.88%, and the X of oxidation of precursor thing is penetrated Respectively as shown in Figure 1 and Figure 2, the first discharge specific capacity for being prepared into button cell is for ray diffraction diagram spectrum and x-ray photoelectron power spectrum 161mAh/g, as shown in figure 3, the capability retention after 50 circulations is 92.75%, as shown in Figure 4.

Embodiment 2

With nickel nitrate, cobalt nitrate and aluminum nitrate as raw material, according to Ni: Co: Al mol ratio 0.8: 0.15: 0.05, it is configured to Ammonia spirit of the mixed solution with the sodium hydroxide solution and 10mol/L of 5mol/L is passed through constant current by the mixed solution of 2mol/L Pump cocurrent is added in the reactor of 2L, fills the ammonia spirit conduct that 600mL, pH value are that 11.0, temperature is 60 DEG C in reactor Bottom liquid, mixing speed are 1000 revs/min, carry out precipitation reaction, and control ph fluctuation during being somebody's turn to do is less than ± 0.4, temperature Fluctuation, is filtered after precipitation reaction is complete less than ± 1 DEG C, and washing for several times, is close to 7 up to filtrate pH value, nitric acid in filtrate Radical content is less than 1 × 10-5Mol/L, is vacuum dried at 120 DEG C, obtains graminaceous nickel cobalt aluminium hydroxide presoma;

By the nickel cobalt aluminium presoma prepared in above-mentioned steps in tube type resistance furnace 650 DEG C of pre-burning 4h, programming rate is 5 DEG C/min, nickel cobalt aluminum oxide is obtained, then with lithium hydroxide according to mol ratio 1:1.05 are well mixed, and are placed in the pipe of oxygen atmosphere 800 DEG C of sintering 12h in formula resistance furnace, programming rate is 5 DEG C/min, is just obtaining lithium ion battery through broken and screening after cooling Pole material nickel cobalt aluminium powder.

After testing, in the present embodiment the pre-sintered burn tinctuer of presoma high temperature is 5.97%%, and the X of oxidation of precursor thing is penetrated Respectively as shown in Figure 5, Figure 6, the first discharge specific capacity for being prepared into button cell is for ray diffraction diagram spectrum and x-ray photoelectron power spectrum 174mAh/g, as shown in fig. 7, the capability retention after 50 circulations is 94.04%, as shown in Figure 8.

Case study on implementation 3

With nickel nitrate, cobalt nitrate and aluminum nitrate as raw material, according to Ni: Co: Al mol ratio 0.8: 0.15: 0.05, it is configured to Ammonia spirit of the mixed solution with the sodium hydroxide solution and 6mol/L of 2mol/L is passed through constant flow pump by the mixed solution of 1mol/L Cocurrent is added in the reactor of 2L, and it is ammonia spirit that 10.5, temperature is 60 DEG C the bottom of as to fill 600mL, pH value in reactor Liquid, mixing speed are 750 revs/min, carry out precipitation reaction, and control ph fluctuation during being somebody's turn to do is less than ± 0.4, temperature fluctuation Less than ± 1 DEG C, after precipitation reaction is complete, filtered, for several times, until filtrate pH value is close to 7, in filtrate, nitrate anion contains for washing Amount is less than 1 × 10-5Mol/L, is vacuum dried at 120 DEG C, obtains graminaceous nickel cobalt aluminium hydroxide presoma;

By the nickel cobalt aluminium presoma prepared in above-mentioned steps in tube type resistance furnace 500 DEG C of pre-burning 6h, programming rate is 5 DEG C/min, nickel cobalt aluminum oxide is obtained, then with lithium hydroxide according to mol ratio 1:1.05 are well mixed, and are placed in the pipe of oxygen atmosphere 800 DEG C of sintering 12h in formula resistance furnace, programming rate is 5 DEG C/min, is just obtaining lithium ion battery through broken and screening after cooling Pole material nickel cobalt aluminium powder.

After testing, in the present embodiment the pre-sintered burn tinctuer of presoma high temperature is 7.33%, and the X of oxidation of precursor thing is penetrated Ray diffraction diagram spectrum and x-ray photoelectron power spectrum respectively as shown in Figure 9, Figure 10, are prepared into the first discharge specific capacity of button cell For 171mAh/g, as shown in figure 11, the capability retention after 50 circulations is 93.54%, as shown in figure 12.

Claims (11)

1. a kind of preparation method of lithium ion battery anode material nickel cobalt aluminium, comprises the following steps:
(1) preparation of nickel cobalt aluminium presoma:Nickel salt solution, cobalt salt solution and aluminum salt solution are mixed, the gold after mixing in solution Category ion concentration is 0.5mol/L~2.0mol/L, then will be molten with the mixing of above-mentioned nickel cobalt aluminium to precipitant solution, enveloping agent solution Coprecipitation reaction is carried out in the reactor that liquid adds equipped with bottom liquid by constant flow pump cocurrent, control ph, temperature, stirring 10~ After 30h, filtered, repeatedly washed, dried, obtain lithium ion battery anode material nickel cobalt aluminium hydroxide presoma;
(2) preparation of nickel cobalt aluminium positive electrode:By presoma, pre-sintering obtains nickel cobalt aluminum oxide at different temperatures, analyzes nickel Ni in cobalt aluminum oxide2+And Ni3+Content, with Ni3+Content highest nickel cobalt aluminum oxide is mixed with lithium source, in oxygen atmosphere Lower high temperature sintering, obtains lithium ion battery anode material nickel cobalt aluminium powder after broken and screening;
Complexing agent in step (1) is the ammonia spirit of 4~10mol/L;
In step (2), pre-sintering temperature is 500~750 DEG C, and programming rate is 1~6 DEG C/min, and temperature retention time is 2~8h.
2. the preparation method of lithium ion battery anode material nickel cobalt aluminium according to claim 1, it is characterised in that:The step Suddenly nickel salt in (1), cobalt salt and aluminium salt are nitrate, according to Ni: Co: Al mol ratio 0.80: 0.15: 0.05.
3. the preparation method of lithium ion battery anode material nickel cobalt aluminium according to claim 1, it is characterised in that:The step Suddenly the precipitating reagent in (1) is the sodium hydroxide solution of 1mol/L~5mol/L.
4. the preparation method of lithium ion battery anode material nickel cobalt aluminium according to claim 1, it is characterised in that:The step Suddenly the bottom liquid in (1) is the ammonia spirit of 4~10mol/L.
5. the preparation method of lithium ion battery anode material nickel cobalt aluminium according to claim 1, it is characterised in that:The step Suddenly the pH in (1) is 10~11.
6. the preparation method of lithium ion battery anode material nickel cobalt aluminium according to claim 1, it is characterised in that:The step Suddenly the precipitation reaction temperature in (1) is 40~60 DEG C.
7. the preparation method of lithium ion battery anode material nickel cobalt aluminium according to claim 1, it is characterised in that:The step Suddenly during the precipitation reaction of (1), mixing speed is 500~1500 revs/min.
8. the preparation method of the lithium ion battery anode material nickel cobalt aluminium according to any one in claim 1~7, its are special Levy and be:In step (2) sintering temperature be 750~850 DEG C, programming rate be 1~6 DEG C/min, temperature retention time be 10~ 20h.
9. the preparation method of the lithium ion battery anode material nickel cobalt aluminium according to any one in claim 1~7, its are special Levy and be:In step (2), nickel cobalt aluminum oxide is 1 with the mol ratio of lithium source: (1~1.05).
10. the preparation method of the lithium ion battery anode material nickel cobalt aluminium according to any one in claim 1~7, its It is characterised by:In step (2) lithium source be lithium hydroxide, lithium carbonate, lithium nitrate, lithium sulfate, lithium oxalate, lithium acetate, chlorination One or more in lithium.
The preparation method of the 11. lithium ion battery anode material nickel cobalt aluminium according to any one in claim 1~7, its It is characterised by:Ni in step (2)2+And Ni3+Detection method of content for calculating burn tinctuer and x-ray photoelectron power spectrum point Analysis method.
CN201410750308.8A 2014-12-10 2014-12-10 A kind of preparation method of lithium ion battery anode material nickel cobalt aluminium CN104466154B (en)

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CN106159220B (en) * 2015-04-22 2018-10-02 南京理工大学 Two-step method prepares anode material for lithium-ion batteries LiNi0.80Co0.15Al0.05O2Method
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