CN108899502A - A kind of high capacity nickle cobalt lithium manganate base composite positive pole and preparation method thereof - Google Patents
A kind of high capacity nickle cobalt lithium manganate base composite positive pole and preparation method thereof Download PDFInfo
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- CN108899502A CN108899502A CN201810693943.5A CN201810693943A CN108899502A CN 108899502 A CN108899502 A CN 108899502A CN 201810693943 A CN201810693943 A CN 201810693943A CN 108899502 A CN108899502 A CN 108899502A
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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Abstract
The present invention is suitable for field of lithium ion battery anode, the present invention provides a kind of high capacity nickle cobalt lithium manganate base composite positive pole and preparation method thereof, by the positive electrode for obtaining high capacity in the ternary system of high nickel content, adulterate strontium and iridium, so that material has preferable multiplying power and cycle performance, add washing process together between double sintering once sintered, pass through washing, the modification of boron element surface and twice sintering process, material surface structure can be improved, surface residual alkali content is reduced to improve interface stability, to promote the capacity and circulation safe performance of positive electrode.
Description
Technical field
The invention belongs to field of lithium ion battery anode more particularly to a kind of high capacity nickle cobalt lithium manganate base are compound just
Pole material and preparation method thereof.
Background technique
Nickel-cobalt-manganternary ternary anode material is widely used in 3C due to energy density with higher and lower cost
Product and new-energy automobile field.The nickelic low cobalt of tertiary cathode material promoted battery energy density, reduce material at
This etc. has a clear superiority, but safety and stability problem is more prominent.Due to the skill of nickelic tertiary cathode material
Art barrier is higher, preparation process and equipment and in terms of requirement be all significantly larger than common ternary material, it is high
Nickel ternary material moves to maturity to produce and to do there are many more R&D work, breakthrough of difficulties.
Nowadays, with the increase of battery material cost, and raising of the country to high Energy Density Materials subsidy, Ge great Zheng
Pole material factory commercial city is actively being laid out nickelic product development, production, and the market for nickelic battery material below gains the initiative.
Simple high-nickel material is easy to taking off due to Li ion since structural stability is not good enough in charge and discharge process
Embedding and Ni, Co, Mn ionic valence condition variation causes collapsing for material structure, causes pole to the cycle life and safety of material
Big harm.The residual alkali of high-nickel material is high, will lead to the transmission path blocking of lithium ion, capacity is relatively low, and to further battery
Size mixing technology has an impact.
For these problems, we can add washing process together once sintered between double sintering, so as to
Residual alkali is reduced, the capacity and circulation safe performance of material are promoted.
Summary of the invention
In view of the above problems, the purpose of the present invention is to provide a kind of high capacity nickle cobalt lithium manganate base composite positive pole and
Preparation method, it is intended to reach reduction residual alkali by improving preparation process, promote the capacity and circulation safe performance of material
Purpose.
A kind of preparation method preparing high capacity nickle cobalt lithium manganate base composite positive pole, the method includes following steps
Suddenly：
Step S1, certain molar ratio under room temperature, is pressed into lithium source, nickelic ternary precursor, barium source and iridium source, together
It is added in high speed mixer and is sufficiently mixed uniformly, obtain mixed-powder, mixed-powder carry out under the atmosphere of oxygen
High temperature sintering, up to LiNi after cooling after the completion of sintering0.8Co0.1Mn0.1-x-ySrxIryO2Composite positive pole；
Step 2, by the LiNi in step S10.8Co0.1Mn0.1-x-ySrxIryO2Composite positive pole is pulverized and sieved, so
After washed, in water-washing process, a certain amount of boric acid is added or boron oxide is reacted with lithium source, by the solution washed into
Row ageing be evaporated, will ageing be evaporated after material be placed in rake type vacuum dryer carry out rotation be evaporated, obtain dry mixed powder；
Dry mixed powder obtained in step S2 will be carried out low-temperature sintering by step 3 under the atmosphere of oxygen, obtain boron
The composite positive pole of cladding；
The composite positive pole that boron coats is crossed sieve by step 4, obtains final LiNi0.8Co0.1Mn0.1-x- ySrxIryO2/ B composite positive pole.
Specifically, in step S1, lithium source is lithium hydroxide, and high temperature sintering temperature is 700~900 DEG C, sintering time is 8~
15h, oxygen atmosphere flow are 0.2~1.2m3/h。
Specifically, in step S2, water control is 1~1.5 in the mass ratio of water and positive electrode to be washed when washing：1
In range, washing time is 5~30min, and the revolving speed of vacuum drier is 300~600r/min, and the amount of boron is in step S1
LiNi0.8Co0.1Mn0.1-x-ySrxIryO2The 0.5%~2% of composite positive pole gross mass.
Specifically, low-temperature sintering temperature is 180~350 DEG C in step S3, the sintered heat insulating time is 5~10h, oxygen gas
The flow of atmosphere is 0.2~1.2m3/h。
Specifically, the sieve mesh of sieve is 325 in step S4.
The present invention also provides a kind of high capacity nickle cobalt lithium manganate base composite positive pole, the high capacity nickle cobalt lithium manganate bases
Composite positive pole is prepared by a kind of preparation method of high capacity nickle cobalt lithium manganate base composite positive pole.
The beneficial effects of the invention are as follows：By obtaining the positive electrode of high capacity, doping in the ternary system of high nickel content
Strontium and iridium wash between double sintering plus together work once sintered so that material has preferable multiplying power and cycle performance
Skill can improve material surface structure, reduce surface residual alkali content by washing, the modification of boron element surface and twice sintering process
Interface stability is improved, to promote the capacity and circulation safe performance of positive electrode.
Detailed description of the invention
Fig. 1 is the circulation volume conservation rate curve comparison figure after embodiment 1 and the electric discharge of comparative example 1.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right
The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and
It is not used in the restriction present invention.
A kind of preparation method of high capacity nickle cobalt lithium manganate base composite positive pole, includes the following steps：
Step S1, certain molar ratio under room temperature, is pressed into lithium source, nickelic ternary precursor, barium source and iridium source, together
It is added in high speed mixer and is sufficiently mixed uniformly, obtain mixed-powder, mixed-powder carry out under the atmosphere of oxygen
High temperature sintering, up to LiNi after cooling after the completion of sintering0.8Co0.1Mn0.1-x-ySrxIryO2Composite positive pole；
In this step, lithium source is lithium hydroxide, and high temperature sintering temperature is 700~900 DEG C, and sintering time is 8~15h, oxygen
Gas atmosphere flow is 0.2~1.2m3/h。
Step 2, by the LiNi in step S10.8Co0.1Mn0.1-x-ySrxIryO2Composite positive pole is pulverized and sieved, so
After washed, in water-washing process, a certain amount of boric acid is added or boron oxide is reacted with lithium source, by the solution washed into
Row ageing be evaporated, will ageing be evaporated after material be placed in rake type vacuum dryer carry out rotation be evaporated, obtain dry mixed powder；
In this step, water control is 1~1.5 in the mass ratio of water and positive electrode to be washed when washing：In 1 range,
Washing time is 5~30min, and the revolving speed of vacuum drier is 300~600r/min, and the amount of boron is in step S1
LiNi0.8Co0.1Mn0.1-x-ySrxIryO2The 0.5%~2% of composite positive pole gross mass.
Dry mixed powder obtained in step S2 will be carried out low-temperature sintering by step 3 under the atmosphere of oxygen, obtain boron
The composite positive pole of cladding；
In this step, low-temperature sintering temperature is 180~350 DEG C, and the sintered heat insulating time is 5~10h, the flow of oxygen atmosphere
For 0.2~1.2m3/h。
The composite positive pole that boron coats is crossed sieve by step 4, obtains final LiNi0.8Co0.1Mn0.1-x- ySrxIryO2/ B composite positive pole.
In this step, the sieve mesh of sieve is 325.
A kind of preparation method of high capacity nickle cobalt lithium manganate base composite positive pole passes through in the ternary system of high nickel content
Obtain the positive electrode of high capacity, adulterate strontium and iridium so that material has preferable multiplying power and cycle performance, once sintered and
Add one of washing process between double sintering, by washing, the modification of boron element surface and twice sintering process, material table can be improved
Face structure reduces surface residual alkali content to improve interface stability, to promote the capacity and circulation safe of positive electrode
Energy.
A kind of high capacity nickle cobalt lithium manganate base composite positive pole, it is compound just by a kind of above-mentioned high capacity nickle cobalt lithium manganate base
The preparation method of pole material is prepared.
In order to illustrate technical solutions according to the invention, the following is a description of specific embodiments.
Embodiment 1：
1) under room temperature, by lithium hydroxide, nickelic ternary precursor, barium source and iridium source in molar ratio 1.03：0.98：
0.01：0.01, it is added in high speed mixer and is sufficiently mixed uniformly together, obtain mixed-powder, mixed-powder is subjected to high temperature
Sintering, sintering temperature are 800 DEG C, and the sintered heat insulating time is 10h, blast oxygen, oxygen flow 0.4m in sintering process3/ h,
It keeps oxygen concentration to reach 99.9%, obtains LiNi after cooling0.8Co0.1Mn0.1-x-ySrxIryO2Composite positive pole.
2) LiNi for obtaining step 10.8Co0.1Mn0.1-x-ySrxIryO2Composite positive pole is pulverized and sieved, according to
Ratio of water to material 1：1 is washed, and in water-washing process, 1500ppm boric acid, washing time 10min, revolving speed 350r/ is added
Min, by the solution washed carry out ageing be evaporated, by the material after being evaporated be placed in rake type vacuum dryer carry out rotation be evaporated.
3) material after being evaporated step 2 carries out low-temperature sintering, and sintering temperature is 300 DEG C, and the sintered heat insulating time is 8h, burns
Oxygen, oxygen flow 0.3m are blasted during knot3/ h keeps oxygen concentration to reach 99.9%, obtains the anode composite of boron cladding
Material.
4) composite positive pole that the boron of step 3 coats is crossed into 325 mesh screens, obtains final washed
LiNi0.8Co0.1Mn0.1-x-ySrxIryO2/ B composite positive pole.
Comparative example 1：
1) under room temperature, by lithium hydroxide, nickelic ternary precursor, barium source and iridium source in molar ratio 1.03：0.98：
0.01：0.01, it is added in high speed mixer and is sufficiently mixed uniformly together, obtain mixed-powder, mixed-powder is subjected to high temperature
Sintering, sintering temperature are 800 DEG C, and the sintered heat insulating time is 10h, blast oxygen, oxygen flow 0.4m in sintering process3/ h,
Oxygen concentration is kept to reach 99.9%, up to LiNi after cooling0.8Co0.1Mn0.1-x-ySrxIryO2Composite positive pole.
2) by LiNi0.8Co0.1Mn0.1-x-ySrxIryO2Composite positive pole and 1500ppm boric acid are added in high mixer together
Mixed at high speed is carried out, low-temperature sintering is then carried out, sintering temperature is 300 DEG C, and the sintered heat insulating time is 8h, is blasted in sintering process
Oxygen, oxygen flow 0.3m3/ h keeps oxygen concentration to reach 99.9%, obtains the composite positive pole of boron cladding.
3) composite positive pole of boron that step 2 obtains cladding is crossed into 325 mesh screens, obtained final without washing
LiNi0.8Co0.1Mn0.1-x-ySrxIryO2/ B composite positive pole.
Respectively with conductive agent acetylene carbon black, binder PVDF presses the composite positive pole that embodiment 1 and comparative example 1 are obtained
According to mass ratio 80：12：8 ratios are uniformly mixed, and suitable -2 pyrrolidones ball milling of 1- methyl is added is made into slurry within 1 hour and uniformly apply
On aluminium flake, positive plate is made in drying, tabletting.2032 button cells are assembled by cathode of metal lithium sheet, are tested using Siken
System carries out electric performance test (charging/discharging voltage is 2.75~4.3V, and temperature condition is 45 DEG C).Circulation after obtained electric discharge
Capacity retention ratio curve comparison figure washes work as shown in Figure 1, embodiment 1 passes through to add between double sintering once sintered together
The LiNi obtained after skill0.8Co0.1Mn0.1-x-ySrxIryO2/ B composite positive pole is than the positive electrode that does not coat than traditional
Comparative example 1 directly carries out the positive electrode for the surface cladding B that once sintered and double sintering obtains without washing, and circulation volume is protected
Holdup improves significantly, and reduces the residual alkali on high-nickel material surface, promotes the capacity and circulation safe performance of material.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (6)
1. a kind of preparation method of high capacity nickle cobalt lithium manganate base composite positive pole, which is characterized in that the method includes under
State step：
Step S1, certain molar ratio is pressed into lithium source, nickelic ternary precursor, barium source and iridium source, is added to high speed mixing together
It is sufficiently mixed in machine uniformly, obtains mixed-powder, mixed-powder progress is subjected to high temperature sintering under the atmosphere of oxygen, has been sintered
At after rear cooling up to LiNi0.8Co0.1Mn0.1-x-ySrxIryO2Composite positive pole；
Step 2, by the LiNi in step S10.8Co0.1Mn0.1-x-ySrxIryO2Composite positive pole is pulverized and sieved, then into
Row washing, in water-washing process, is added a certain amount of boric acid or boron oxide and LiNi0.8Co0.1Mn0.1-x-ySrxIryO2It is compound
The mixed solution washed is carried out ageing and is evaporated by the reaction of positive electrode surface residual alkali, and the material after ageing is evaporated is placed in rake
Formula vacuum drier carries out rotation and is evaporated, and obtains dry mixed powder；
Dry mixed powder obtained in step S2 will be carried out low-temperature sintering by step 3 under the atmosphere of oxygen, obtain boron cladding
Composite positive pole；
The composite positive pole that boron coats is crossed sieve by step 4, obtains final LiNi0.8Co0.1Mn0.1-x-ySrxIryO2/ B is multiple
Close positive electrode.
2. a kind of preparation method of high capacity nickle cobalt lithium manganate base composite positive pole as described in claim 1, feature exist
In in step S1, lithium source is lithium hydroxide, and high temperature sintering temperature is 700~900 DEG C, and sintering time is 8~15h, oxygen atmosphere
Flow is 0.2~1.2m3/h。
3. a kind of preparation method of high capacity nickle cobalt lithium manganate base composite positive pole as described in claim 1, feature exist
In in step S2, water control is 1~1.5 in the mass ratio of water and positive electrode to be washed when washing：In 1 range, when washing
Between be 5~30min, the revolving speed of vacuum drier is 300~600r/min, and the amount of boron is in step S1
LiNi0.8Co0.1Mn0.1-x-ySrxIryO2The 0.5%~2% of composite positive pole gross mass.
4. a kind of preparation method of high capacity nickle cobalt lithium manganate base composite positive pole as described in claim 1, feature exist
In in step S3, low-temperature sintering temperature is 180~350 DEG C, and the sintered heat insulating time is 5~10h, and the flow of oxygen atmosphere is 0.2
~1.2m3/h。
5. a kind of preparation method of high capacity nickle cobalt lithium manganate base composite positive pole as described in claim 1, feature exist
In in step S4, the sieve mesh of sieve is 325.
6. a kind of high capacity nickle cobalt lithium manganate base composite positive pole, which is characterized in that the high capacity nickle cobalt lithium manganate base is multiple
Positive electrode is closed to be prepared by any one of claim 1-5 the method.
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