CN109802123A - A kind of preparation method of nickelic positive electrode - Google Patents
A kind of preparation method of nickelic positive electrode Download PDFInfo
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- CN109802123A CN109802123A CN201910094882.5A CN201910094882A CN109802123A CN 109802123 A CN109802123 A CN 109802123A CN 201910094882 A CN201910094882 A CN 201910094882A CN 109802123 A CN109802123 A CN 109802123A
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Abstract
The invention discloses a kind of preparation methods of nickelic positive electrode, comprising the following steps: uniformly mixes by the hydroxide containing Ni, the compound containing lithium and containing doped chemical, calcining obtains the substrate A after mixing；Substrate A is added in washing solution, and controls the temperature of washing solution, surface residual lithium carbonate and lithium hydroxide are washed off, the compound containing lithium is added in cleaning solvent, is dried after the substrate washed, obtains mixture B；After evenly mixing by mixture B, cladding element and lithium-containing compound, it calcines, crushes, the nickelic positive electrode being finally modified.The present invention improves the high-temperature stability of nickel material by doping, the lithium carbonate and lithium hydroxide of surface residual are reduced by washing, improve the water suction and processing performance of material, the destruction of material surface when can not only repair washing by coating, positive electrode can also be reduced to contact with the direct of electrolyte, so as to improve the hot properties and long circulating performance of battery core.
Description
Technical field
The present invention relates to lithium battery material technical field, especially a kind of preparation side for being modified nickelic tertiary cathode material
Method.
Background technique
High capacity, low cost nickelic ternary anode material for lithium-ion batteries LiNi x Co y Mn 1-x-y O 2 (x >=
0.8) become at present the lithium ion power battery cathode material of most application prospect, capacity the mentioning with nickel content of ternary material
It is high and increase, but the free lithium content of corresponding material surface also increases, and causes material residual alkali degree higher, surface texture exists
Deintercalation can be destroyed lithium ion in the process repeatedly, and be reacted with electrolyte, and poor circulation is caused.Therefore it is reduced by washing
Material surface residual alkali, while material surface is coated to improve stability of material, promote first effect, capacity and the circulation of material
Performance.
In tertiary cathode material, the main function of nickel is for promoting energy density, and higher nickel also means that material
With higher energy density and lower cobalt, the small amount of cobalt can bring declining to a great extent for material cost again.
And high-nickel material is while have high-energy density, disadvantage is also more obvious, and structural stability and high temperature are steady
Fixed poor, the particle on surface is easy to happen phase transformation: layer structure → spinel structure → rock salt structure (irreversible), the phase on surface
Change can be to particle internal stretch, so as to cause material failure cracking.In order to solve this problem, it is mentioned by doping and surface cladding
The destruction of high lattice stability and isolation electrolyte to anode.
Higher nickel, sintering when be easier in air CO2 and H2O react, formation Li2CO3 and LiOH.
In this case material is more hygroscopic, PH higher, poor processability；And excessive Li2CO3 will lead to it is swollen
Gas influences high temperature circulation and high temperature storage.In this case surface washing is essential.
Summary of the invention
It is an object of the invention to based on the deficiencies of the prior art, provide a kind of preparation method of nickelic positive electrode, lead to
Overdoping improves the high-temperature stability of nickel material, improves the hot properties and long circulating performance of battery core.
To achieve the above object, the invention adopts the following technical scheme:
A kind of preparation method of nickelic positive electrode, comprising the following steps:
(1) preparation of substrate: being 1:1 by the hydroxide containing Ni, the compound containing lithium and containing doped chemical in molar ratio
~1.30:0~0.1 is uniformly mixed, and the temperature lower calcination after mixing at 650~900 DEG C obtains the substrate A；
(2) substrate A is added in washing solution, and controls the temperature of washing solution, surface residual lithium carbonate and hydrogen
Lithia is washed off, in order to prevent the precipitation of excessive structure lithium, and the compound containing lithium, the substrate washed are added in cleaning solvent
It is dried afterwards in certain temperature, obtains mixture B；
(3) mixture B, cladding element and lithium-containing compound is equal for 1:0.005~0.01:0.01~0.05 with molar ratio
It after even mixing, calcines, crushes, the nickelic positive electrode being finally modified, wherein the cladding element is at a certain temperature
For the one of which of Ti, Al, Mg, Si, B, Ce.
As a further improvement of the present invention: the chemical general formula of the hydroxide containing Ni is Ni1-x-yM1xM2y
(OH)2, wherein M1For one of Co or Mn, M2For one of Mn, Al, Mg, Zr, Ba, 0≤x≤0.20,0≤y≤
0.20。
As a further improvement of the present invention: the compound containing lithium is lithium carbonate, lithium hydroxide, lithia, acetic acid
One of which in lithium.
As a further improvement of the present invention: the doped chemical is Al, B, Ba, Mg, Ce, Cr, F, Mo, Ti, Sr, P, Zr
In one of which or any combination.
As a further improvement of the present invention: the chemical general formula of the substrate A is Li1+aNi1-x-yM1xM2yM3zO2,
In 0≤a≤0.3,0≤x≤0.2,0≤y≤0.2,0≤z≤0.1, the one of which of M1 Co, Mn, M2For Mn, Al, Mg,
The one of which of Zr, Ba, M3For the one of which or any combination of Al, B, Ba, Mg, Ce, Cr, F, Mo, Ti, Sr, P, Zr.
As a further improvement of the present invention: the washing solution be deionized water, boric acid aqueous solution, phosphate aqueous solution,
The solid and liquid weight ratio of the one of which of ethyl alcohol, propyl alcohol, the substrate A and washing solution is 2~0.5, the temperature of the washing solution
At 0~65 DEG C, having washed drying temperature is 100~200 DEG C for degree control.
As a further improvement of the present invention: the calcination temperature in the step (3) is 650~900 DEG C.
Beneficial effects of the present invention are as follows:
1) present invention improves the high-temperature stability of nickel material by doping.
2) present invention reduces the lithium carbonate and lithium hydroxide of surface residual by washing, improves the water suction and processability of material
Can, certain additive is added when washing, prevents the transition of structure lithium from deviating to influence capacity performance.
3) destruction of material surface, can also reduce positive electrode when the present invention can not only repair washing by cladding
Direct with electrolyte contacts, so as to improve the hot properties and long circulating performance of battery core；It is added centainly while cladding
Lithium compound is mended, so that capacity boost.
4) the nickelic positive electrode being prepared of the invention, residual alkali is lower, and PH is lower, not hygroscopic, processing performance
Good, the battery core head effect and capacity being prepared by it are higher, and normal temperature circulation, high temperature circulation and high temperature storage are more excellent, and
Its thermal stability is largely improved by adulterating and coating
Detailed description of the invention
Fig. 1 embodiment and comparative example pH value, remaining lithium, water suction and processing compare.
Fig. 2 embodiment and comparative example gram volume, head effect comparison diagram.
Fig. 3 embodiment and comparative example normal temperature circulation comparison diagram are from top to bottom followed successively by embodiment 3, reality with lines right endpoint
Apply example 1, comparative example 1, embodiment 2, comparative example 2.
Fig. 4 embodiment and comparative example high temperature circulation comparison diagram are from top to bottom followed successively by embodiment 3, reality with lines right endpoint
Apply example 1, embodiment 2, comparative example 1, comparative example 2.
Fig. 5 embodiment and comparative example high temperature storage comparison diagram, every group of histogram are followed successively by comparative example 1, comparison from left to right
Example 2, embodiment 1, embodiment 2, embodiment 3.
Fig. 6 embodiment and comparative example DSC comparison diagram.
Specific embodiment
The present invention will be further described With reference to embodiment:
A kind of preparation method of nickelic positive electrode, comprising the following steps:
(1) preparation of substrate: being 1:1 by the hydroxide containing Ni, the compound containing lithium and containing doped chemical in molar ratio
~1.30:0~0.1 is uniformly mixed, and the temperature lower calcination after mixing at 650~900 DEG C obtains the substrate A；
(2) substrate A being added in washing solution, the solid and liquid weight ratio of the substrate A and washing solution is 2~0.5, and
The temperature of control washing solution is washed off surface residual lithium carbonate and lithium hydroxide, in order to prevent excessive structure lithium at 0~65 DEG C
Precipitation, the compound containing lithium is added in cleaning solvent, the temperature after the substrate washed at 100~200 DEG C is dried, and is obtained
Mixture B；
(3) mixture B, cladding element and lithium-containing compound is equal for 1:0.005~0.01:0.01~0.05 with molar ratio
After even mixing, in 650~900 DEG C of temperature lower calcinations, crush, the nickelic positive electrode being finally modified, wherein the cladding
Element is the one of which of Ti, Al, Mg, Si, B, Ce.
Nickeliferous hydroxide is all made of Ni in case of the present invention0.94Co0.045Al0.015(OH)2.015, the compound containing lithium
It is all made of lithium hydroxide, is sintered under oxygen-enriched atmosphere, drying is under vacuum conditions.
Prepared in case of the present invention to positive electrode pH value to obtain test method as follows: weigh 5.00 ± 0.05g powder
Last sample is scattered in 50.00 ± 0.10g deionized water, and 10min is stirred, and obtains clear liquid, uses good acid after debugging
Degree meter is put into clear liquid, and the bead of pH note has to not cross clear liquid when test, and reading at this time is the pH value of sample.
The test method for the residual lithium in positive electrode surface being prepared in case of the present invention is as follows: weigh 10.000 ±
The powder of 0.050g mass is scattered in 100g deionized water, 10min is sufficiently stirred, and dissolution is obtained by filtration using filter paper
There are LiOH and Li2CO3Clear aqueous solution；Use the HCl solution of concentrated hydrochloric acid configuration 0.1M.Use 0.1M HCl as titrant,
MR and BTB is titrated on potentiometric titrimeter as indicator, finds the HCl of consumption accurately according to indicator or potential change
Dosage, and write down corresponding volume.According to the HCl volume of consumption, LiOH and Li is calculated2CO3Content.
The positive electrode being prepared in case of the present invention is tested using cylindrical electrical core 18650, the anode formula of battery core
Are as follows: the positive electrode of preparation: conductive agent SP: bonding agent (VM750)=100:2:1.4, cathode formula are as follows: S360-L1: conductive agent
SP: dispersing agent C MC: bonding agent SBR=100:1.2:1.4:1.8, diaphragm use Celgard 12+4, electrolyte using
TC-2823 (nickelic ternary is recommended to use electrolyte), the temperature of normal temperature circulation are 25 DEG C, and the temperature of high temperature circulation is 45 DEG C, high
Warm storage condition is to save 7 days at 60 DEG C.
It is as follows that positive electrode DSC test method is prepared in case of the present invention: the full electric state anode pole piece of dismantling impregnates
It is cleaned into DMC solution, soaking time needs to confirm；Pole piece is placed in glove box transitional storehouse after cleaning and vacuumizes standing, it is quiet
Setting the time needs to confirm；Pole piece is scraped into powder with Stupalox in glove box after the completion of standing.Sky quality is accurately weighed, by 2mg
Left and right powder is added, and the electrolyte of 2 μ L or so is added with micropipettor, covers sealing gold plaque and assembles high pressure crucible,
It weighs crucible gross weight and records.Empty reference crucible is chosen completely as far as possible, and sample quality calculates accurate；Temperature range: 25~
450 DEG C, 5 DEG C/min of heating rate.To guarantee that test is accurate, the heating rate that whether can use 2 DEG C/min need to be discussed.
Comparative example 1
(1) Ni first0.94Co0.045Al0.015(OH)2.015It is uniformly mixed with lithium hydroxide, metal molar ratio is M (Ni+
Co+Al): M (Li)=1:1.05；
(2) mixture is under conditions of oxygen-enriched, 725 DEG C of calcining 13h, is then crushed sieving processing to sintered product, obtains
Positive electrode.
(3) testing its PH is 12.08, and the weight ratio that the lithium carbonate and lithium hydroxide of surface residual account for positive electrode respectively is
0.7531% and 0.3098%.
(4) 18650 cylindrical electrical core evaluation tests are made into resulting positive electrode: its head effect and 0.2C gram volume difference
For 87% and 218mAh/g；25 DEG C of room temperature circulations, 300 weeks capacity retention ratios are 93%；45 DEG C of high temperature circulations, after 300 weeks
Capacity retention ratio is 89%；After 60 DEG C of high temperature storages, capacity retention ratio 92%, capacity restoration rate is 95%.
(5) DSC has tested peak temperature at 205 DEG C, and maximum temperature is at 230 DEG C.
Comparative example 2
(1) Ni0.94Co0.045Al0.015 first (OH) 2.015 and lithium hydroxide uniformly mix, and metal molar ratio is
M (Ni+Co+Al): M (Li)=1:1.05；
(2) mixture is under conditions of oxygen-enriched, 725 DEG C of calcining 13h, is then crushed sieving processing to sintered product.
(3) to the above-mentioned product and deionized water for obtaining being crushed after being sieved, after weight ratio 1:1 mixing, control is gone from water
Temperature be 45 DEG C, after agitator treating 20min, after centrifuge dripping, vacuum drying 10h, obtains positive electrode at 150 DEG C.
(4) testing its PH is 11.38, and the weight ratio that the lithium carbonate and lithium hydroxide of surface residual account for positive electrode respectively is
0.1521% and 0.1112%.
(5) 18650 cylindrical electrical core evaluation tests are made into resulting positive electrode: its head effect and 0.2C gram volume difference
For 85.3% and 212.6mAh/g；25 DEG C of room temperature circulations, 300 weeks capacity retention ratios are 82.7%；45 DEG C of high temperature circulations, 300
Capacity retention ratio after week is 89%；After 60 DEG C of high temperature storages, capacity retention ratio 89%, capacity restoration rate is 92%.
(6) DSC has tested 207 DEG C of peak temperature, 232 DEG C of maximum temperature.
Embodiment 1
(1) Ni first0.94Co0.045Al0.015(OH)2.015, lithium hydroxide and adulterant oxidation strontium uniformly mix, metal
Molar ratio is M (Ni+Co+Al): M (Li): M (Sr)=1:1.05:0.01.
(2) mixture is under conditions of oxygen-enriched, 725 DEG C of calcining 13h, is then crushed sieving processing to sintered product, obtains
Positive electrode.
(3) testing its PH is 12.03, and the weight ratio that the lithium carbonate and lithium hydroxide of surface residual account for positive electrode respectively is
0.7038% and 0.3211%.
(4) 18650 cylindrical electrical core evaluation tests are made into resulting positive electrode: its head effect and 0.2C gram volume difference
For 87.5% and 218.2mAh/g；25 DEG C of room temperature circulations, 300 weeks capacity retention ratios are 92.7%；45 DEG C of high temperature circulations, 300
Capacity retention ratio after week is 94%；After 60 DEG C of high temperature storages, capacity retention ratio 94%, capacity restoration rate is 97%.
(5) DSC has tested 211 DEG C of peak temperature, 240 DEG C of maximum temperature.
Embodiment 2
(1) Ni first0.94Co0.045Al0.015(OH)2.015, lithium hydroxide and adulterant oxidation strontium uniformly mix, metal
Molar ratio is M (Ni+Co+Al): M (Li): M (Sr)=1:1.05:0.01.
(2) mixture is under conditions of oxygen-enriched, 725 DEG C of calcining 13h, is then crushed sieving processing to sintered product.
(3) to the above-mentioned product and deionized water for obtaining being crushed after being sieved, after weight ratio 1:1 mixing, control is gone from water
Temperature be 45 DEG C and (be added account for lithium hydroxide from water weight 0.0048% in deionized water, prevent the transition of structure lithium
Abjection), after agitator treating 20min, after centrifuge dripping, vacuum drying 10h, obtains positive electrode at 150 DEG C.
(4) it is 11.33 that test, which obtains PH, and the lithium carbonate and lithium hydroxide of surface residual account for the weight ratio of positive electrode respectively
For 0.1356% and 0.1181%.
(5) 18650 cylindrical electrical core evaluation tests are made into resulting positive electrode: its head effect and 0.2C gram volume difference
For 87.2% and 217.9mAh/g；25 DEG C of room temperature circulations, 300 weeks capacity retention ratios are 88%；45 DEG C of high temperature circulations, 300 weeks
Capacity retention ratio afterwards is 90%；After 60 DEG C of high temperature storages, capacity retention ratio 90%, capacity restoration rate is 93%.
(6) DSC has tested 211 DEG C of peak temperature, 243 DEG C of maximum temperature.
Embodiment 3
(1) Ni first0.94Co0.045Al0.015(OH)2.015, lithium hydroxide and adulterant oxidation strontium uniformly mix, metal
Molar ratio is M (Ni+Co+Al): M (Li): M (Sr)=1:1.05:0.01.
(2) mixture is under conditions of oxygen-enriched, 725 DEG C of calcining 13h, is then crushed sieving processing to sintered product.
(3) to the above-mentioned product and deionized water for obtaining being crushed after being sieved, after weight ratio 1:1 mixing, control is gone from water
Temperature be 45 DEG C and (be added account for lithium hydroxide from water weight 0.0048% in deionized water, prevent the transition of structure lithium
Abjection), after agitator treating 20min, after centrifuge dripping, the vacuum drying 10h at 150 DEG C.
(4) drying obtains product and uniformly mixes with covering titanium dioxide and a small amount of lithium hydroxide, metal molar ratio
For M (Ni+Co+Al): M (Ti): M (Li)=1:0.005:0.0047.
(5) mixture is under conditions of oxygen-enriched, 550 DEG C of calcining 10h, then handles sintered product sieving, obtains anode
Material.
(6) it is 11.31 that test, which obtains PH, and the lithium carbonate and lithium hydroxide of surface residual account for the weight ratio of positive electrode respectively
For 0.1366% and 0.1081%.
(7) 18650 cylindrical electrical core evaluation tests are made into resulting positive electrode: its head effect and 0.2C gram volume difference
For 89.5% and 221.8mAh/g；25 DEG C of room temperature circulations, 300 weeks capacity retention ratios are 94%；45 DEG C of high temperature circulations, 300 weeks
Capacity retention ratio afterwards is 94%；After 60 DEG C of high temperature storages, capacity retention ratio 95%, capacity restoration rate is 98%.
(8) DSC has tested 218 DEG C of peak temperature, 248 DEG C of maximum temperature.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all be fallen into the protection scope that claims of the present invention determines.
Claims (7)
1. a kind of preparation method of nickelic positive electrode, it is characterised in that the following steps are included:
(1) preparation of substrate: by the hydroxide containing Ni, the compound containing lithium and containing doped chemical be in molar ratio 1:1~
1.30:0~0.1 is uniformly mixed, and the temperature lower calcination after mixing at 650~900 DEG C obtains the substrate A；
(2) substrate A is added in washing solution, and controls the temperature of washing solution, surface residual lithium carbonate and hydroxide
Lithium is washed off, and the compound containing lithium is added in cleaning solvent, dries after the substrate washed, obtains mixture B；
(3) mixture B, cladding element and lithium-containing compound is uniformly mixed for 1:0.005~0.01:0.01~0.05 with molar ratio
After conjunction, calcine, crush, the nickelic positive electrode being finally modified, wherein the cladding element is Ti, Al, Mg, Si, B,
The one of which of Ce.
2. a kind of preparation method of nickelic positive electrode according to claim 1, it is characterised in that: the hydrogen-oxygen containing Ni
The chemical general formula of compound is Ni1-x-yM1xM2y(OH)2, wherein M1For one of Co or Mn, M2For in Mn, Al, Mg, Zr, Ba
One kind, 0≤x≤0.20,0≤y≤0.20.
3. a kind of preparation method of nickelic positive electrode according to claim 1, it is characterised in that: the chemical combination containing lithium
Object is lithium carbonate, lithium hydroxide, lithia, the one of which in lithium acetate.
4. a kind of preparation method of nickelic positive electrode according to claim 1, it is characterised in that: the doped chemical is
One of which or any combination in Al, B, Ba, Mg, Ce, Cr, F, Mo, Ti, Sr, P, Zr.
5. a kind of preparation method of nickelic positive electrode according to claim 1, it is characterised in that: the change of the substrate A
General formula is Li1+aNi1-x-yM1xM2yM3zO2, wherein 0≤a≤0.3,0≤x≤0.2,0≤y≤0.2,0≤z≤0.1, M1
For the one of which of Co, Mn, M2For the one of which of Mn, Al, Mg, Zr, Ba, M3For Al, B, Ba, Mg, Ce, Cr, F, Mo, Ti,
The one of which or any combination of Sr, P, Zr.
6. a kind of preparation method of nickelic positive electrode according to claim 1, it is characterised in that: the washing solution is
The one of which of deionized water, boric acid aqueous solution, phosphate aqueous solution, ethyl alcohol, propyl alcohol, the solid-liquid of the substrate A and washing solution
Weight ratio is 2~0.5, and the temperature of the washing solution is controlled at 0~65 DEG C, and having washed drying temperature is 100~200 DEG C.
7. a kind of preparation method of nickelic positive electrode according to claim 1, it is characterised in that: in the step (3)
Calcination temperature be 650~900 DEG C.
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| CN112635756A (en) * | 2020-12-21 | 2021-04-09 | 国联汽车动力电池研究院有限责任公司 | High-nickel positive electrode material and preparation method and application thereof |
| CN112635756B (en) * | 2020-12-21 | 2022-09-27 | 国联汽车动力电池研究院有限责任公司 | High-nickel positive electrode material and preparation method and application thereof |
| CN113060774A (en) * | 2021-03-26 | 2021-07-02 | 蜂巢能源科技有限公司 | Cobalt-free cathode material and preparation method and application thereof |
| CN113526570A (en) * | 2021-06-29 | 2021-10-22 | 格林美（无锡）能源材料有限公司 | Preparation method of high-nickel cathode material |
| CN113889618A (en) * | 2021-09-30 | 2022-01-04 | 中国电子科技集团公司第十八研究所 | Hydrophobic anode material modified by organic silicide and preparation method thereof |
| CN114142037A (en) * | 2021-11-19 | 2022-03-04 | 天津巴莫科技有限责任公司 | Method for preparing ultra-high nickel anode material by adopting gradient lithium supplement and prepared ultra-high nickel anode material |
| CN114229917A (en) * | 2021-12-09 | 2022-03-25 | 宜宾锂宝新材料有限公司 | Surface modification method of high-nickel anode material and modified high-nickel anode material |
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Application publication date: 20190524 |