CN115852468B - Monocrystalline power lithium manganate and preparation method and application thereof - Google Patents
Monocrystalline power lithium manganate and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of lithium ion batteries, and discloses a preparation method of monocrystal power lithium manganate, which comprises the following steps: step 1: mixing the lithium compound and the manganese compound according to the molar ratio of 2 xLi/Mn of 0.8-1.0, and uniformly mixing; step 2: the mixture of the lithium compound and the manganese metal compound prepared in the step 1 is burned for the first time, and the lithium manganese compound is obtained after the burning; step 3: crushing the lithium manganese compound obtained in the step 2 to obtain a powdery lithium manganese compound; step 4: and (3) adding a certain amount of lithium compound into the powdery lithium manganese compound obtained in the step (3), wherein the adding amount is 3-8% of the mass of the lithium manganese compound, and mixing and then performing secondary burning. The lithium deficiency ignition during primary ignition is utilized, so that the minimum temperature required by single crystallization of the lithium manganese compound is reduced, and the dissolution of manganese is reduced; in addition, the invention also discloses the monocrystal power type lithium manganate prepared by the method and application thereof.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to monocrystalline power lithium manganate, and a preparation method and application thereof.
Background
At present, the lithium ion battery is in an important position in the industry chain in the vigorous era of new energy automobile industry, and the most critical component in the lithium ion battery is the lithium ion positive electrode material. A nickel cobalt lithium manganate ternary material, a nickel cobalt lithium aluminate ternary material, lithium cobaltate, lithium iron phosphate and spinel lithium manganate. The spinel lithium manganate is one of the main current positive electrode materials with the lowest comprehensive cost, and the phenomenon that the surface manganese of the lithium manganate is dissolved easily in a battery system causes serious voltage and capacity attenuation.
To eliminate or mitigate the phenomenon of manganese dissolution present in lithium ion battery cathode materials, the skilled artisan generally addresses this by two aspects: coating and adding complexing agent into the battery. Wherein CN201610250000.6 discloses a lithium battery anode material which is spinel lithium nickel manganese oxide coated with a coating layer on the surface, wherein the coating layer contains Li a B b O c And LiMnBO 3 The method comprises the steps of carrying out a first treatment on the surface of the The structural formula of the spinel lithium nickel manganese oxide is LiM x+y Ni 0 .5-x Mn 1 .5-y O 4 Wherein M is selected from at least one of Co, al, cr, fe, mg, zr or Ti, 0.ltoreq.x<0 .2、0≤y<0.2; the Li is a B b O c In particular LiBO 2 、LiB 3 O 5 、LiB 5 O 8 、LiB 7 O 11 、Li 2 B 4 O 7 、Li 3 BO 3 、Li 3 B 5 O 9 、Li 3 B 7 O 12 、Li 4 B 2 O 5 Or Li (lithium) 4 B 6 O 11 At least one of them.
The proposal is that Li is coated outside spinel lithium nickel manganese oxide a B b O c And LiMnBO 3 Thereby inhibiting the dissolution of manganese in the electrolyte and improving the high-temperature stability of the spinel lithium nickel manganese oxide.
CN201110048750.2 discloses a positive electrode material for a lithium secondary battery, and a secondary battery module using the lithium secondary battery, wherein the surface of a lithium-manganese composite oxide has a coating layer containing an oxide or fluoride containing M (M is one or more elements selected from Mg, al, and Cu) and a phosphorus compound, and the atomic concentration of the lithium-manganese composite oxide side is higher in the coating layer than in the electrolyte side on the surface layer side of the coating layer.
According to the scheme, the surface of the lithium-manganese composite oxide is coated with an oxide or fluoride and a coating layer of a phosphorus compound, so that the manganese dissolution of the lithium secondary battery at high temperature and high voltage is inhibited.
Cn201710629068.X discloses a positive electrode active material, a preparation method thereof, a positive electrode and a lithium ion battery, wherein the positive electrode active material comprises a core formed by a material containing lithium manganese iron phosphate, a first shell positioned on the surface of the core, and a second shell positioned on the surface of the first shell; the material of the first shell is carbon material, and the material of the second shell is Mo 2 N。
The scheme is that a first shell of carbon material and Mo are coated on the outer surface of a positive electrode active material 2 N, thereby inhibiting elution of manganese from the electrode material.
It is not difficult to see that all of the above 3 schemes reduce manganese dissolution from the standpoint of surface coating of the electrode material.
CN 201911099470.7 discloses a layered-spinel phase composite positive electrode material and a preparation method thereof, wherein the layered-spinel phase composite positive electrode material is composed of layered structure LiNi x Co y Mn z O 2 LiM with spinel phase 2 O 4 Composite aLiM 2 O 4 ·(1-a)LiNi x Co y Mn z O 2 The method comprises the steps of carrying out a first treatment on the surface of the Wherein x is more than or equal to 0.5 and less than or equal to 0.8,0.02, y is more than or equal to 0.2,0.02 and z is more than or equal to 0.4,0<a is less than or equal to 0.05, M is one or more of Ni, co and Mn; the preparation method of the layered-spinel phase composite positive electrode material comprises the following steps:
1) Preparing a nickel cobalt manganese precursor by adopting a coprecipitation method;
2) Mixing the nickel cobalt manganese precursor with part of lithium source and additive, wherein the molar ratio of Li of part of lithium source to Me in the nickel cobalt manganese precursor is 0.85-1,performing primary sintering to obtain lithium-deficient positive electrode material Li δ Ni x Co y Mn z O 2 ；
3) Crushing a lithium-deficient cathode material, mixing the crushed cathode material with an additive and a residual lithium source, wherein the molar ratio of Li in the total lithium source to Me in the lithium-deficient cathode material is 1.02-1.10, and then performing secondary sintering, crushing and sieving to obtain a layered-spinel phase composite cathode material;
step 2) wherein 0.5 is less than or equal to delta <1, and Me is transition metal in the nickel cobalt manganese precursor;
step 3) Me is a transition metal in the lithium-deficient cathode material;
step 2), after the first sintering is finished, a section of heat preservation procedure is further included, namely the sintering temperature is reduced to 250-550 ℃, and the heat preservation is carried out for 1-4 hours;
step 2), the temperature of the first sintering is 800-1050 ℃, and the sintering time is 10-14h;
the temperature of the second sintering in the step 3) is 300-800 ℃, and the sintering time is 5-8h.
The beneficial effects of the scheme are recorded as follows:
according to the invention, the lithium-deficient cathode material is formed by adopting the first sintering, and the partial layered structure is promoted to be converted into the spinel phase by a special cooling process, so that the layered-spinel phase composite cathode material is obtained, the rate performance of the cathode material is improved, and the thermal stability of the material is further improved. On the basis, the layered structure of the lithium-deficient cathode material is repaired by a secondary sintering lithium supplementing process, so that a lattice structure with good layered structure and easy lithium ion deintercalation can be obtained. In addition, metal ions corresponding to the doped metal oxide in the sintering process are usually +2/+3/+4 valence, and enter a crystal lattice of the nickel cobalt lithium manganate to form vacancies in the material, so that the diffusion migration rate of lithium ions in the charge and discharge process is improved, and the rate capability of the positive electrode material is improved.
It can be seen that the lithium supplementing process of this document is mainly for repairing the layered structure, and the document does not describe whether the lithium supplementing process contributes to the spinel structure, and neither the examples nor the comparative examples can support the prominent contribution of the lithium supplementing process to the spinel structure.
The problem that this scheme needs to solve: how to propose a new solution to reduce manganese dissolution.
Disclosure of Invention
The invention aims to provide single crystal power type lithium manganate, a preparation method and application thereof, wherein each unit cell of a normal spinel lithium manganate structure has 8 LiMn 2 O 4 Wherein 8 Li fills tetrahedral voids, 1/8 of 64 tetrahedral sites 8a, 32O rows are stacked in cubes, 16 Mn fills in the octahedral voids, wherein lithium deficiency is sintered, the stacking mode of O is changed, and the unit cell volume is increased. And further, the minimum temperature required by single crystallization is reduced, the dissolution of manganese is reduced, and the cycle life of the anode material is prolonged.
The invention is not specifically described: nM represents nanomole/liter, μM represents micromoles/liter, mM represents millimoles/liter, and M represents moles/liter;
the preparation method of the monocrystal power lithium manganate comprises the following steps:
step 1: mixing the lithium compound and the manganese compound according to the molar ratio of 2 xLi/Mn of 0.8-1.0, and uniformly mixing;
step 2: the mixture of the lithium compound and the manganese metal compound prepared in the step 1 is burned for the first time, and the lithium manganese compound is obtained after the burning;
step 3: crushing the lithium manganese compound obtained in the step 2 to obtain a crushed lithium manganese compound;
step 4: and (3) adding a certain amount of lithium compound into the crushed lithium manganese compound obtained in the step (3), wherein the adding amount is 3-8% of the mass of the lithium manganese compound, and mixing and then performing secondary burning.
Wherein the compound is selected from one or more of crystal water compound or non-crystal water compound of lithium carbonate, lithium hydroxide and lithium nitrate;
the manganese compound is selected from one or more of manganous oxide, manganese carbonate and manganese dioxide.
Preferably, the temperature of the primary firing is 770-870 ℃ and the firing time is 4-12 hours.
More preferably, the temperature of the primary firing is 770-840 ℃ and the firing time is 6-10 hours;
more preferably, the temperature of the primary firing is 800-840 ℃ and the firing time is 7-9 hours;
in practical application, the primary firing temperature can be 770 deg.C, 780 deg.C, 790 deg.C, 800 deg.C, 810 deg.C, 820 deg.C, 830 deg.C, 840 deg.C, 850 deg.C, 860 deg.C, 870 deg.C.
Preferably, the temperature of the secondary firing is 550-750 ℃ and the firing time is 4-12 hours.
More preferably, the temperature of the secondary firing is 600-700 ℃ and the firing time is 6-10 hours.
In practical application, the secondary ignition temperature can be 550 ℃, 560 ℃, 570 ℃, 580 ℃, 590 ℃, 600 ℃, 610 ℃, 620 ℃, 630 ℃, 640 ℃, 650 ℃, 660 ℃, 670 ℃, 680 ℃, 690 ℃, 700 ℃, 710 ℃, 720 ℃, 730 ℃, 740 ℃, 750 ℃.
Preferably, in the step 1, the method further comprises a doping agent, wherein the doping agent is selected from one or more of an oxide, a hydroxide and a carbonic acid compound of Nb, mg, co, V, ti, al, zr, zn, la, and the doping agent accounts for 0.1-1.5% of the mass of the manganese compound.
Preferably, after the crushed lithium manganese compound is prepared in the step 3, a coating agent is added into the crushed lithium manganese compound and mixed, wherein the coating agent is one or more of oxides of aluminum, silicon, titanium, magnesium, lanthanum and vanadium.
Preferably, the lithium manganese compound prepared in the step 2 is crushed to obtain a crushed lithium manganese compound, and the crushed lithium manganese compound with the median particle size in the range of 4-7 um is selected for secondary burning.
Preferably, the coating method is a sol-gel method, and the coating agent is 1-10% of the mass of the crushed lithium manganese compound; the coating agent is one or more of aluminum, silicon, titanium, magnesium, lanthanum, vanadium, fluorine and other ion sol with mass fraction of 5-20%.
In addition, the lithium manganate also comprises single crystal power type lithium manganate, and is obtained by adopting the preparation method of the single crystal power type lithium manganate.
Preferably, the core-shell structure takes a lithium manganese compound as a core layer and one or more of oxides of aluminum, silicon, titanium, magnesium, lanthanum and vanadium as a coating layer.
In addition, the lithium ion secondary battery comprises a positive electrode, a negative electrode, a diaphragm and electrolyte, wherein the active material used in the positive electrode is single crystal power lithium manganate.
The beneficial effects of the invention are as follows:
the invention provides monocrystalline power lithium manganate, a preparation method and application thereof, wherein each unit cell of a normal spinel lithium manganate structure has 8 LiMn 2 O 4 Wherein 8 Li fills tetrahedral voids, 1/8 of 64 tetrahedral sites 8a, 32O rows are stacked in cubes, 16 Mn fills in the octahedral voids, wherein lithium deficiency is sintered, the stacking mode of O is changed, and the unit cell volume is increased. And further, the minimum temperature required by single crystallization is reduced, the dissolution of manganese is reduced, and the cycle life of the motor material is prolonged.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the description of the present invention, it is to be noted that the specific conditions are not specified in the examples, and the description is performed under the conventional conditions or the conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
Step 1: 8000g of spheroidal trimanganese tetroxide and 1712g of battery grade lithium carbonate, 2 XLi/Mn molar ratio 0.94, were mixed in a high-speed mixer.
Step 2: the mixed material is burned once in a roller hearth furnace in air atmosphere, the burning temperature is 840 ℃, and the burning time is 8 hours. And naturally cooling to room temperature after the firing is finished to obtain the lithium manganese compound.
Step 3: crushing and grading the lithium manganese compound. Controlling the median particle size d50=5-7 um to obtain the crushed lithium manganese compound.
Step 4: 8000g of crushed lithium manganese compound is baked for 2 hours in vacuum, and is put into a high-speed mixer after being baked, and the lithium carbonate with the additional mass of 361.6g is put into the high-speed mixer for even mixing; and (5) carrying out secondary firing on the obtained mixed material in a roller kiln. The firing temperature is 700 ℃, the firing time is 8 hours, the material is naturally cooled to room temperature, and the material is screened by a pair of rollers, so that the monocrystal power lithium manganate with high safety performance is finally obtained.
Example 2
Substantially the same as in example 1, except that the molar ratio of trimanganese tetroxide to lithium carbonate in step 1 was 0.8 in terms of 2×Li/Mn; and the lithium supplementing amount in the step 4 is 8 percent.
Example 3
Substantially the same as in example 1, except that the manganese tetraoxide and lithium carbonate in step 1 were formulated in a molar ratio of 2×li/Mn of 1.0; and 3% of lithium is supplemented in the step 4.
Example 4
Substantially the same as in example 1, except that the primary firing temperature was 770℃and the firing time was 8 hours.
Example 5
Substantially the same as in example 1, except that the primary firing temperature was 870℃and the firing time was 8 hours.
Example 6
Substantially the same as in example 1, except that the primary firing temperature was 840℃and the firing time was 4 hours.
Example 7
Substantially the same as in example 1, except that the primary firing temperature was 840℃and the firing time was 12 hours.
Example 8
Substantially the same as in example 1, except that the secondary firing temperature was 550℃and the firing time was 8 hours.
Example 9
Substantially the same as in example 1, except that the secondary firing temperature was 750℃and the firing time was 8 hours.
Example 10
Substantially the same as in example 1, except that the secondary firing temperature was 700℃and the firing time was 4 hours.
Example 11
Substantially the same as in example 1, except that the secondary firing temperature was 700℃and the firing time was 12 hours.
Example 12
Substantially the same as in example 1, except that a dopant was added in step 1, 8000g of spheroidal trimanganese tetraoxide and 1712g of battery grade lithium carbonate were added, the 2 XLI/Mn molar ratio being 0.94, 30g of nano Nb 2 O 5 Mixing in a high-speed mixer.
Example 13
Substantially the same as in example 12, except that the dopant in step 1 was selected as ZrO 2 。
Example 14
Substantially the same as in example 1, except that 8000g of crushed single crystal lithium manganate and 20L of ethanol were dissolved in step 4, stirred to 1h, 200ml of 5% by mass of alumina sol was added in a stirred state, stirred for 4h, evaporated in a water bath, and vacuum-baked at 110℃for 2h. Drying, putting into a high-speed mixer, adding 361.6g of lithium carbonate into the high-speed mixer, and uniformly mixing; and (5) carrying out secondary firing on the obtained mixed material in a roller kiln. The firing temperature is 700 ℃, the firing time is 8 hours, the material is naturally cooled to room temperature, and the material is screened by a pair of rollers, so that the monocrystal power lithium manganate with high safety performance is finally obtained.
Example 15
Substantially the same as in example 14, except that the aluminum sol in step 4 was replaced with a silica sol.
Example 16
Substantially the same as in example 15, except that the aluminum sol in step 4 was replaced with a titanium sol.
Comparative example 1
Essentially the same as in example 1, except that the manganese tetraoxide and lithium carbonate were dosed at a molar ratio of 2×li/Mn of 1, no further lithium carbonate was added in step 4.
Comparative example 2
Essentially the same as in example 1, except that the manganese tetraoxide and lithium carbonate were dosed at a molar ratio of 2×li/Mn of 1.10, no further lithium carbonate was added in step 4.
Comparative example 3
Substantially the same as in example 1, except that the manganese tetraoxide and lithium carbonate were compounded in a molar ratio of 2×li/Mn of 1, 10% of lithium carbonate was added in step 4.
Full cell performance test:
the obtained monocrystal power lithium manganate is uniformly mixed according to the mass ratio of 97%, 1.5% PVDF and 1.5% carbon nano tube to prepare coating slurry. The method comprises the following steps:
1. and dissolving PVDF in NMP to prepare a glue solution with the solid content of 8%, adding carbon nano tube slurry, mixing and dispersing at a high speed for 1.5h, adding the product, kneading and stirring for 6h, and adding an appropriate amount of NMP to adjust the viscosity of the slurry to 4500-7500mPa.s. And obtaining the positive electrode slurry for the lithium battery.
2. And preparing the negative electrode slurry by adopting a similar method and a similar formula to obtain the negative electrode slurry for the lithium battery.
3. The positive electrode slurry was coated on the aluminum foil, and the negative electrode slurry was coated on the copper foil. The soft package battery is prepared through the procedures of drying, rolling, vermicelli, welding electrode lugs, winding, liquid injection, sealing and the like, and the battery capacity, circulation and short circuit experiments (the highest temperature of the short circuit surface is 90 ℃) are tested.
4. And after the circulation is finished, disassembling the battery to take the diaphragm, and measuring the manganese content in the diaphragm to confirm the manganese leaching amount.
Table 1: full cell performance test results:
analysis:
1. it is apparent from examples 1 to 3 that in the present invention, in the case where the molar ratio of Li/Mn is 0.94 in step 1, the effect of promoting the development of the capacity and the elution amount of manganese of the battery is promoted.
2. It can be seen from examples 1 and examples 4 to 7 that in the present invention, the primary firing temperature was 840℃and the time was 8 hours as the optimum conditions; and it can be seen from example 5 that the manganese dissolution rate of the material is increased when the primary firing temperature is 870 c compared with other examples, and therefore, in practical application, it is recommended that the primary firing temperature is set to 870 c or less.
3. It can be seen from examples 1 and examples 8 to 11 that in the present invention, the secondary firing temperature was 700℃and the time was 8 hours as the optimum conditions.
4. It can be seen from examples 1 and examples 12 to 13 that in the present invention, the addition of the dopant while the trimanganese tetroxide and lithium carbonate are mixed contributes to the improvement of the cycle life of the electrode material.
5. It can be seen from examples 1 and examples 14 to 16 that in the present invention, the lithium manganate material having a core-shell structure, which is coated with the coating layer on the outer surface, has a better capacity and better stability, and the elution of manganese is also alleviated.
6. It is apparent from example 1 and comparative example 1 that in the present invention, the secondary ignition of lithium supplement after the primary ignition of lithium deficiency has an obvious promoting effect on controlling manganese dissolution, battery capacity and cycle life compared with the primary ignition of lithium.
7. As can be seen from example 3 and comparative example 1, in the present invention, after the primary burning of lithium deficiency, the capacity of the battery without secondary lithium supplementation or with insufficient secondary lithium supplementation is improved to some extent, but in general, the cycle life and high temperature stability of the battery are significantly reduced.
8. It is apparent from example 3 and comparative example 2 that in the present invention, after a sufficient amount of lithium is given at the time of one firing, the battery exhibits a remarkable decrease in the stability at high temperature, cycle life, and elution of manganese.
9. It can be seen from example 3 and comparative example 3 that in the present invention, after the primary firing of lithium deficiency and the secondary addition of excess lithium, the capacity and high temperature stability of the battery are significantly reduced.
10. As can be seen from comparative examples 1 to 3, when the excessive lithium is used for sintering, the retention rate of comparative examples 2 and 3 after 1500 cycles is significantly improved compared with comparative example 1, and we speculate that the reason for this phenomenon is that the excessive lithium forms a lithium-rich phase material, the content of 4-valent manganese in the material is more, and the stability of 4-valent manganese is stronger than that of 3-valent manganese, so that the retention rate of comparative example after 1500 cycles is significantly improved compared with comparative example 1, and the effect of inhibiting the dissolution of manganese is more obvious.
Claims (6)
1. The preparation method of the monocrystal power lithium manganate is characterized by comprising the following steps of:
step 1: lithium compound and manganese compound are mixed according to the molar ratio of 2 xLi/Mn of 0.8-1.0 for lithium deficiency, and the mixture is uniformly mixed;
step 2: the mixture of the lithium compound and the manganese compound prepared in the step 1 is burned for the first time, and the lithium manganese compound is obtained after the burning;
step 3: crushing the lithium manganese compound obtained in the step 2 to obtain a crushed lithium manganese compound, and adding a coating agent into the crushed lithium manganese compound and mixing, wherein the coating agent is selected from cation sol containing any one of aluminum, silicon, titanium, magnesium, lanthanum and vanadium;
step 4: adding a certain amount of lithium compound into the product obtained in the step 3, wherein the adding amount is 3-8% of the mass of the lithium manganese compound, and mixing and then performing secondary burning;
wherein the lithium compound is selected from one or more of crystal water compound or non-crystal water compound of lithium carbonate, lithium hydroxide and lithium nitrate;
the manganese compound is selected from one or more of manganous oxide, manganese carbonate and manganese dioxide;
the primary firing temperature is 770-840 ℃ and the firing time is 6-10 hours; the temperature of the secondary firing is 600-700 ℃ and the firing time is 6-10 hours;
in the step 1, the method further comprises a doping agent, wherein the doping agent is selected from one or more of an oxide, a hydroxide and a carbonic acid compound of Nb, mg, co, V, ti, al, zr, zn, la, and the doping agent accounts for 0.1-1.5% of the mass of the manganese compound.
2. The method for preparing single crystal power type lithium manganate according to claim 1, wherein the lithium manganese compound prepared in the step 2 is crushed to obtain a crushed lithium manganese compound, and the crushed lithium manganese compound with the median particle size in the range of 4-7 um is selected for secondary burning.
3. The method for preparing single crystal power type lithium manganate according to claim 1, wherein the coating method is a sol-gel method, and the coating agent is 1-10% of the mass of the crushed lithium manganese compound.
4. A single crystal power lithium manganate, characterized in that it is obtained by the method for preparing a single crystal power lithium manganate according to any one of claims 1 to 3.
5. The single crystal power lithium manganate according to claim 4, wherein the single crystal power lithium manganate has a core-shell structure in which a lithium manganese compound is used as a core layer and one or more of oxides of aluminum, silicon, titanium, magnesium, lanthanum and vanadium are used as cladding layers.
6. A lithium ion secondary battery comprising a positive electrode, a negative electrode, a separator, and an electrolyte, wherein the active material used in the positive electrode is the single crystal kinetic lithium manganate according to claim 4 or 5.
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