CN104466154A - Preparation method of lithium ion battery positive material nickel cobalt aluminum - Google Patents
Preparation method of lithium ion battery positive material nickel cobalt aluminum Download PDFInfo
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- CN104466154A CN104466154A CN201410750308.8A CN201410750308A CN104466154A CN 104466154 A CN104466154 A CN 104466154A CN 201410750308 A CN201410750308 A CN 201410750308A CN 104466154 A CN104466154 A CN 104466154A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of lithium ion battery positive material nickel cobalt aluminum. The preparation method comprises the following steps: mixing nickel, cobalt and aluminum salt solutions, mixing a precipitator, a complexing agent and the mixed solution of the nickel cobalt aluminum to obtain a mixed solution, adding the mixed solution into a reaction kettle to carry out co-precipitation reaction, adjusting the pH value of the system to 10 to 11 at the temperature of 40 to 60 DEG C, stirring at the speed of 500 to 1500 turns/minute, carrying out reaction for 10 to 30 hours, filtering, washing and drying to obtain a hydroxide precursor; pre-sintering the precursor at high temperature to obtain a nickel cobalt aluminum oxide, mixing the nickel cobalt aluminum oxide with a lithium source to obtain a mixture, sintering the mixture at high temperature under an oxygen atmosphere, and crushing and sieving to obtain the nickel cobalt aluminum powder. By calculating the pre-sintering loss rate of the precursor, the content of Ni<2+> and the content of Ni<3+> in the nickel cobalt aluminum oxide at different temperatures are analyzed by utilizing XPS, so that the nickel cobalt aluminum oxide with the highest content of Ni<3+> can be obtained, more nickel ions in the secondary sintering process can be promoted to be converted into Ni<3+>, the mixed arrangement of the Li<+> and the Ni<2+> can be reduced, and the electrochemical performance of the material can be improved.
Description
Technical field
The present invention relates to energy storage material and electrochemical field, especially a kind of preparation method of lithium ion battery anode material nickel cobalt aluminium.
Background technology
Since Japanese Sony Corporation in 1991 first successfully develops and realizes the commercialization of lithium ion battery, lithium ion battery more and more receives the concern of people, because its quality is light, volume is little, specific energy is high, self discharge is little, the feature such as the little and memory-less effect of good cycle, pollution, become one of 21 century green secondary cell most with application prospect.Along with the development of electrode material, in succession there is the cell positive material differed from one another, as cobalt acid lithium, lithium nickelate, LiMn2O4, LiFePO4 and nickel-cobalt-manganese ternary material etc.Current lithium ion battery is used widely in multiple fields such as national defense industry, space technology, portable electric appts and electric automobiles, therefore the requirement of people to lithium ion battery is also more and more higher, as security performance is good, specific capacity is high, cycle performance is excellent, the light volume of quality is little, but battery material ripe is at present difficult to meet above properties simultaneously.LiNi
1-x-yco
xa1
yo
2(NCA) be the positive electrode that the specific capacity of at present industrial applications is the highest, having the advantages such as good cycle, abundant raw materials and cost are lower, is a kind of lithium ion power battery cathode material having application prospect.
Current ternary material LiNi
1-x-yco
xa1
yo
2synthetic method mainly contain coprecipitation, high temperature solid-state method, sol-gel process, molte-salt synthesis, spray drying process, microwave method, hydro thermal method and combustion method etc., but LiNi prepared by often kind of method
1-x-yco
xa1
yo
2material also comes with some shortcomings part, is further improved.Wherein, coprecipitation process is simple to operate, and the material property of synthesis is best, is a kind of method most with industrial applications prospect.
When prior art prepares lithium ion battery anode material nickel cobalt aluminium, nickel cobalt aluminium hydroxide presoma is prepared by co-precipitation, directly to mix with lithium source or High Temperature Pre sinters and mixes with lithium source afterwards, then obtain nickel cobalt aluminium positive electrode through high temperature sintering and follow-up break process.Nickel cobalt aluminium oxyhydroxide, mainly nickel hydroxide decomposes more than 230 DEG C, generates NiO, and when temperature reaches 400 DEG C, part NiO absorbs air and is oxidized to Ni
2o
3, finally when temperature is higher than more than 600 DEG C, Ni
2o
3be reduced SA NiO; In addition, if nickelous too high levels in nickel cobalt aluminum oxide, follow-up sintering process can not be oxidized to nickelic completely, and nickelous and lithium ion radius closely, easily produce mixing phenomenon, affect material electrochemical performance.Therefore, different temperatures presintering obtains different Ni
2+and Ni
3+the presoma of content, final material electrochemical performance is different.
Summary of the invention
The problem that will solve required for the present invention improves a kind of preparation method of lithium ion battery anode material nickel cobalt aluminium, the method is under different pre-sintering temperature part, prepare nickel cobalt aluminium positive electrode, calculate the burn tinctuer of the nickel cobalt aluminum oxide after presintering, and analyze wherein Ni by x-ray photoelectron power spectrum (XPS)
2+and Ni
3+content, obtains Ni
3+the nickel cobalt aluminum oxide that content is the highest, promotes that in double sintering process, more nickel ion is converted into Ni
3+, reduce Li
+with Ni
2+mixing, prepare the nickel cobalt aluminium positive electrode that chemical property is good.
For solving the problems of the technologies described above, technical scheme of the present invention is: 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, concentration of metal ions after mixing in solution is 0.5mol/L ~ 2.0mol/L, again by the mixed solution of precipitant solution, enveloping agent solution and above-mentioned nickel cobalt aluminium by together with constant flow pump and stream add in the reactor that end liquid is housed and carry out coprecipitation reaction, control ph, temperature, after stirring 10 ~ 30h, filter, repeatedly wash, dry, obtain lithium ion battery anode material nickel cobalt aluminium hydroxide presoma;
(2) preparation of nickel cobalt aluminium positive electrode: the nickel cobalt aluminum oxide that obtains after being sintered by presoma High Temperature Pre, calculates the burn tinctuer after High Temperature Pre sintering and with XPS analysis wherein Ni
2+and Ni
3+content, then to mix with lithium source, high temperature sintering under oxygen atmosphere, after broken and screening, obtain lithium ion battery anode material nickel cobalt aluminium powder.
The present invention by calculating the burn tinctuer of presoma presintering, and obtains Ni in nickel cobalt aluminum oxide with under the different pre-sintering temperature of X-ray photoelectron spectroscopic analysis
2+and Ni
3+content, obtain Ni
3+the nickel cobalt aluminum oxide that content is maximum, can promote that in double sintering process, more nickel ion is converted into Ni
3+, reduce Li
+with Ni
2+mixing, improve the chemical property of material.
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 precipitation reagent is preferably the sodium hydroxide solution of 1mol/L ~ 5mol/L;
In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described complexing agent is preferably the ammonia spirit of 4 ~ 10mol/L;
In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described end liquid is preferably the ammonia spirit of 4 ~ 10mol/L;
In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, the pH value in described step (1) is preferably 10 ~ 11;
In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, the temperature in described step (1) is preferably 40 ~ 60 DEG C;
In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, the mixing speed in described step (1) is preferably 500 ~ 1500 revs/min;
In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, the presintering in described step (2) is preferably 500 ~ 750 DEG C of insulation 2 ~ 8h, and programming rate is 1 ~ 6 DEG C/min;
In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, the sintering in described step (2) is preferably 750 ~ 850 DEG C of insulation 10 ~ 20h, and programming rate is 1 ~ 6 DEG C/min;
In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, the nickel cobalt aluminum oxide in described step (2) and the mol ratio in lithium source are preferably 1: (1 ~ 1.05);
In the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, the lithium source in described step (2) is preferably lithium hydroxide, lithium carbonate, lithium nitrate, lithium sulfate, lithium oxalate, lithium acetate, one or more in lithium chloride;
In the preparation method of [0019] above-mentioned lithium ion battery anode material nickel cobalt aluminium, the Ni in described step (2)
2+and Ni
3+the analytical method of content is preferably burn tinctuer and X-ray photoelectron spectroscopic analysis method.
[0020] compared with prior art, the lithium ion battery anode material nickel cobalt aluminium that prepared by the inventive method has following beneficial effect:
(1) when optimum temperature presintering, presoma can thoroughly decompose, low activity Ni in the nickel cobalt aluminum oxide obtained
2+content is few, improves the chemical property of material;
[0020] (2) are after optimum temperature presintering, obtain Ni
3+the oxidation of precursor thing that content is the highest, Li during minimizing double sintering in material
+and Ni
2+mixing phenomenon, improve the chemical property of material;
(3) synthetic material has high reversible specific capacity, and cyclical stability is good, and within the scope of 2.5 ~ 4.3V, specific discharge capacity is greater than 170mAh/g.
Accompanying drawing explanation
Fig. 1 is the XRD collection of illustrative plates of nickel cobalt aluminum oxide after the presintering of embodiment 1;
Fig. 2 is the XPS collection of illustrative plates of nickel cobalt aluminum oxide after the presintering of embodiment 1;
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 is the XRD collection of illustrative plates of nickel cobalt aluminum oxide after the presintering of embodiment 2;
Fig. 6 is the XPS collection of illustrative plates of nickel cobalt aluminum oxide after the presintering of embodiment 2;
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 is the XRD collection of illustrative plates of nickel cobalt aluminum oxide after the presintering of embodiment 3;
Figure 10 is the XPS collection of illustrative plates of nickel cobalt aluminum oxide after the presintering of embodiment 3;
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.
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 are raw material, according to Ni: Co: Al mol ratio 0.8: 0.15: 0.05, be mixed with the mixed solution of 1mol/L, by mixed solution and the sodium hydroxide solution of 2mol/L and the ammonia spirit of 6mol/L by constant flow pump and stream adds in the reactor of 2L, 600mL is filled in reactor, pH value is 10.5, temperature is that the ammonia spirit of 50 DEG C is as end liquid, mixing speed is 600 revs/min, carry out precipitation reaction, in this process control ph fluctuation be no more than ± 0.4, temperature fluctuation is no more than ± and 1 DEG C, after precipitation reaction completely, filter, washing for several times, until filtrate pH value is close to 7, in filtrate, nitrate radical content is less than 1 × 10
-5mol/L, 120 DEG C of vacuumizes, obtains graminaceous nickel cobalt aluminium hydroxide presoma,
By the nickel cobalt aluminium presoma 750 DEG C of pre-burning 2h in tube type resistance furnace prepared in above-mentioned steps, programming rate is 5 DEG C/min, obtain nickel cobalt aluminum oxide, mix according to mol ratio 1:1.05 with lithium hydroxide again, be placed in the tube type resistance furnace 800 DEG C sintering 12h of oxygen atmosphere, programming rate is 5 DEG C/min, obtains lithium ion battery anode material nickel cobalt aluminium powder after cooling through broken and screening.
After testing, the burn tinctuer of the presoma High Temperature Pre sintering in the present embodiment is 8.88%, the X ray diffracting spectrum of oxidation of precursor thing and x-ray photoelectron power spectrum are respectively as shown in Figure 1 and Figure 2, the first discharge specific capacity being prepared into button cell is 161mAh/g, as shown in Figure 3, capability retention after 50 circulations is 92.75%, as shown in Figure 4.
Embodiment 2
With nickel nitrate, cobalt nitrate and aluminum nitrate are raw material, according to Ni: Co: Al mol ratio 0.8: 0.15: 0.05, be mixed with the mixed solution of 2mol/L, by mixed solution and the sodium hydroxide solution of 5mol/L and the ammonia spirit of 10mol/L by constant flow pump and stream adds in the reactor of 2L, 600mL is filled in reactor, pH value is 11.0, temperature is that the ammonia spirit of 60 DEG C is as end liquid, mixing speed is 1000 revs/min, carry out precipitation reaction, in this process control ph fluctuation be no more than ± 0.4, temperature fluctuation is no more than ± and 1 DEG C, after precipitation reaction completely, filter, washing for several times, until filtrate pH value is close to 7, in filtrate, nitrate radical content is less than 1 × 10
-5mol/L, 120 DEG C of vacuumizes, obtains graminaceous nickel cobalt aluminium hydroxide presoma,
By the nickel cobalt aluminium presoma 650 DEG C of pre-burning 4h in tube type resistance furnace prepared in above-mentioned steps, programming rate is 5 DEG C/min, obtain nickel cobalt aluminum oxide, mix according to mol ratio 1:1.05 with lithium hydroxide again, be placed in the tube type resistance furnace 800 DEG C sintering 12h of oxygen atmosphere, programming rate is 5 DEG C/min, obtains lithium ion battery anode material nickel cobalt aluminium powder after cooling through broken and screening.
After testing, the burn tinctuer of the presoma High Temperature Pre sintering in the present embodiment is 5.97%%, the X ray diffracting spectrum of oxidation of precursor thing and x-ray photoelectron power spectrum are respectively as shown in Figure 5, Figure 6, the first discharge specific capacity being prepared into button cell is 174mAh/g, as shown in Figure 7, capability retention after 50 circulations is 94.04%, as shown in Figure 8.
[0043] case study on implementation 3
With nickel nitrate, cobalt nitrate and aluminum nitrate are raw material, according to Ni: Co: Al mol ratio 0.8: 0.15: 0.05, be mixed with the mixed solution of 1mol/L, by mixed solution and the sodium hydroxide solution of 2mol/L and the ammonia spirit of 6mol/L by constant flow pump and stream adds in the reactor of 2L, 600mL is filled in reactor, pH value is 10.5, temperature is that the ammonia spirit of 60 DEG C is as end liquid, mixing speed is 750 revs/min, carry out precipitation reaction, in this process control ph fluctuation be no more than ± 0.4, temperature fluctuation is no more than ± and 1 DEG C, after precipitation reaction completely, filter, washing for several times, until filtrate pH value is close to 7, in filtrate, nitrate radical content is less than 1 × 10
-5mol/L, 120 DEG C of vacuumizes, obtains graminaceous nickel cobalt aluminium hydroxide presoma,
By the nickel cobalt aluminium presoma 500 DEG C of pre-burning 6h in tube type resistance furnace prepared in above-mentioned steps, programming rate is 5 DEG C/min, obtain nickel cobalt aluminum oxide, mix according to mol ratio 1:1.05 with lithium hydroxide again, be placed in the tube type resistance furnace 800 DEG C sintering 12h of oxygen atmosphere, programming rate is 5 DEG C/min, obtains lithium ion battery anode material nickel cobalt aluminium powder after cooling through broken and screening.
After testing, the burn tinctuer of the presoma High Temperature Pre sintering in the present embodiment is 7.33%, the X ray diffracting spectrum of oxidation of precursor thing and x-ray photoelectron power spectrum are respectively as shown in Figure 9, Figure 10, the first discharge specific capacity being prepared into button cell is 171mAh/g, as shown in figure 11, capability retention after 50 circulations is 93.54%, as shown in figure 12.
Claims (13)
1. a preparation method for 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, concentration of metal ions after mixing in solution is 0.5mol/L ~ 2.0 mol/L, again by the mixed solution of precipitant solution, enveloping agent solution and above-mentioned nickel cobalt aluminium by constant flow pump and stream add in the reactor that end liquid is housed and carry out coprecipitation reaction, control ph, temperature, after stirring 10 ~ 30h, filter, repeatedly wash, dry, obtain lithium ion battery anode material nickel cobalt aluminium hydroxide presoma;
(2) preparation of nickel cobalt aluminium positive electrode: by presoma at different temperatures presintering obtain nickel cobalt aluminum oxide, analyze Ni in nickel cobalt aluminum oxide
2+and Ni
3+content, with Ni
3+the nickel cobalt aluminum oxide that content is the highest mixes with lithium source, high temperature sintering under oxygen atmosphere, after fragmentation and screening, obtain lithium ion battery anode material nickel cobalt aluminium powder.
2. the preparation method of anode material for lithium-ion batteries according to claim 1, is characterized in that: the nickel salt in described step (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 anode material for lithium-ion batteries according to claim 1, is characterized in that: the precipitation reagent in described step (1) is the sodium hydroxide solution of 1 mol/L ~ 5 mol/L.
4. the preparation method of anode material for lithium-ion batteries according to claim 1, is characterized in that: the complexing agent in described step (1) is the ammonia spirit of 4 ~ 10 mol/L.
5. the preparation method of anode material for lithium-ion batteries according to claim 1, is characterized in that: the end liquid in described step (1) is the ammonia spirit of 4 ~ 10 mol/L.
6. the preparation method of anode material for lithium-ion batteries according to claim 1, is characterized in that: the pH in described step (1) is 10 ~ 11.
7. the preparation method of anode material for lithium-ion batteries according to claim 1, is characterized in that: the precipitation reaction temperature in described step (1) is 40 ~ 60 DEG C.
8. the preparation method of anode material for lithium-ion batteries according to claim 1, is characterized in that: in the precipitation reaction process of described step (1), mixing speed is 500 ~ 1500 revs/min.
9. according to the preparation method of the anode material for lithium-ion batteries in claim 1 ~ 8 described in any one, it is characterized in that: in described 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.
10. according to the preparation method of the anode material for lithium-ion batteries in claim 1 ~ 8 described in any one, it is characterized in that: in described step (2), sintering temperature is 750 ~ 850 DEG C, and programming rate is 1 ~ 6 DEG C/min, and temperature retention time is 10 ~ 20h.
11., according to the preparation method of the anode material for lithium-ion batteries in claim 1 ~ 8 described in any one, is characterized in that: in described step (2), the mol ratio in nickel cobalt aluminum oxide and lithium source is 1: (1 ~ 1.05).
12., according to the preparation method of the anode material for lithium-ion batteries in claim 1 ~ 8 described in any one, is characterized in that: in described step (2), lithium source is lithium hydroxide, lithium carbonate, lithium nitrate, lithium sulfate, lithium oxalate, lithium acetate, one or more in lithium chloride.
13., according to the preparation method of the anode material for lithium-ion batteries in claim 1 ~ 8 described in any one, is characterized in that: Ni in described step (2)
2+and Ni
3+detection method of content for calculating burn tinctuer and X-ray photoelectron spectroscopic analysis method.
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| CN104966819A (en) * | 2015-05-06 | 2015-10-07 | 合肥国轩高科动力能源股份公司 | High energy density lithium-ion battery positive electrode material and preparation method thereof |
| CN104993127A (en) * | 2015-06-05 | 2015-10-21 | 苏州珍展科技材料有限公司 | Preparation method for titanium-oxide-coated anode material for lithium ion cell |
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| CN105406058A (en) * | 2015-12-28 | 2016-03-16 | 浙江华友钴业股份有限公司 | Preparation method for nickel-cobalt-aluminium oxide having super-large particle diameter |
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