CN102244239A - Method for preparing nickel cobalt aluminum serving as cathodic material of lithium ion battery - Google Patents
Method for preparing nickel cobalt aluminum serving as cathodic material of lithium ion battery Download PDFInfo
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Abstract
The invention discloses a method for preparing nickel cobalt aluminum serving as a cathodic material of a lithium ion battery, which comprises the following steps of: mixing nickel salt solution and cobalt salt solution uniformly, adding complexing agent solution, precipitant solution and the mixed solution into a reaction kettle with base solution in a parallel flow mode to perform precipitation reaction, performing solid-liquid separation after the reaction is performed fully, and washing; adding the washed solid material into the reaction kettle, dripping aluminum salt solution and the precipitant solution slowly to perform secondary precipitation reaction, so that an aluminum element is precipitated on the surface of the solid material gradually, stirring continuously in the integral process, performing solid-liquid separation after the reaction is finished, and washing and drying the solid material to a precursor of the cathodic material of the lithium ion battery; and mixing the precursor and a lithium source, performing two-section sintering under the condition of introducing oxygen, and crushing the calcined material which is subjected to the two-section sintering and performing subsequent processing to obtain the nickel cobalt aluminum serving as the cathodic material of the lithium ion battery. The method has the advantages of low requirement on equipment, high automation degree, environment friendliness, few wastes, high quality of products and the like and is easy to operate.
Description
Technical field
The present invention relates to a kind of preparation method of cell positive material, relate in particular to a kind of preparation method of anode material for lithium-ion batteries.
Background technology
From Sony in 1991 is made battery that positive electrode makes and is rendered to market with stratiform cobalt acid lithium since, lithium rechargeable battery demonstrates important function day by day in every field, battery material is constantly development also, the anode material for lithium-ion batteries that occurs each tool characteristic in succession is as LiMn2O4, lithium nickelate, LiFePO 4, nickel manganese cobalt ternary etc.Along with people are more and more higher to the requirement of lithium ion battery, people need the lithium rechargeable battery that service time is longer, size is littler, weight is lighter, this just requires its positive electrode should possess performances such as fail safe is good, specific capacity is high, cyclicity is stable simultaneously, but ripe at present cobalt acid lithium, LiMn2O4, LiFePO 4 and nickel-cobalt-manganese ternary material all are difficult to satisfy simultaneously aforesaid every requirement.And lithium nickelate has than the much higher characteristic of above-mentioned positive electrode capacity, by it is carried out suitable processing from aspects such as synthetic method, doping vario-properties, improve its cycle performance and security performance, be expected to make lithium nickelate to become the leading anode material for lithium-ion batteries in market.
Lithium nickelate has two kinds of structures, and the crystal structure with electro-chemical activity is α-NaFeO
2Type layer structure, stability of structure depend primarily on lithium ion and the nickelic ion order degree in the oxygen cubic closest packing.In reality is synthetic, because the 3d of nickelous
8The electron distributions characteristic, it is difficult to be oxidized to nickelic, the lithium nickelate that generates stoichiometric proportion is very difficult, usually all can there be a spot of nickelous to occupy niccolic lattice-site, simultaneously for replenishing charge balance, the nickelous of equivalent also can enter the lithium layer, causes cationic mixing, and capacitance is reduced.The method that solves this difficult problem has two kinds, and the one, make nickel be in trivalent as far as possible, the 2nd, mix the element (for example cobalt, magnesium, aluminium etc.) that can stablize its structure.Nonetheless can make the cycle performance and the security performance of lithium nickelate obtain bigger improvement, but still undesirable, and the lithium nickelate alkalescence of so producing is higher, can bring potential safety hazard for the battery of post-production.
The preparation method of existing lithium nickelate mainly contains solid phase synthesis and liquid phase is synthetic.Solid phase method is synthetic generally to carry out sintering after compound, lithium source and the doping element compound mixing with nickel, but this solid mixing method can not reach the even of atomic level, and performance is difficult to give full play to; Though liquid phase method can head it off, complex process, yield poorly.Consider that from the actual production angle solid phase method prepares lithium nickelate and is more suitable for large-scale production undoubtedly, but the working condition harshness, the control difficulty, particularly strict to sintering atmosphere, because under air atmosphere, can only obtain Li
2Ni
8-xM
xO
10In addition, the control of sintering temperature also is a great problem, and its domain of walker is narrower, and temperature is low then reacts insufficient, and the temperature height then can decompose, and is difficult to react completely.
Summary of the invention
The technical problem to be solved in the present invention is to overcome the deficiencies in the prior art, provides that a kind of equipment requirements is low, automaticity is high, simple to operate, environmental friendliness, waste of raw materials are few, the preparation method of the lithium ion battery anode material nickel cobalt aluminium of good product quality and suitable suitability for industrialized production.
For solving the problems of the technologies described above, the technical scheme that the present invention proposes is a kind of preparation method of lithium ion battery anode material nickel cobalt aluminium, may further comprise the steps:
(1) preparation of nickel cobalt aluminium presoma: nickel salt solution and cobalt salt solution are mixed, mixing back solution metal ion concentration is 0.5M～2.0M, again enveloping agent solution, precipitant solution are added with described mixing back solution and stream and be equipped with in the reactor of end liquid, add thermal agitation and carry out the primary sedimentation reaction, treat fully reaction back when being 7 μ m～14 μ m (for example the solid deposit seed of Sheng Chenging grow into average grain diameter), begin the slip that overflows is carried out Separation of Solid and Liquid, again the solid material after separating is washed; When the cleaning solution pH value after the washing reaches 8.5～11.5, stop to wash and the solid material is joined in the reactor that end liquid is housed, the aluminum salt solution and the precipitant solution that slowly drip 0.1M～1.0M again in reactor are carried out the secondary precipitation reaction, constantly stir, make aluminium element be deposited to this solid material surface gradually, fully after the reaction, the slip that overflows is carried out Separation of Solid and Liquid, solid product after the separation through the washing, the oven dry after, the precursor of lithium ionic cell positive material that obtains having hud typed structure;
(2) preparation of nickel cobalt aluminium positive electrode: the precursor of lithium ionic cell positive material that above-mentioned steps (1) is made mixes with the lithium source, under logical oxygen condition, carry out double sintering, roasting material after the double sintering obtains lithium ion battery anode material nickel cobalt aluminium (NCA material) through fragmentation and subsequent treatment.The average grain diameter of this lithium ion battery anode material nickel cobalt aluminium is 5 μ m～20 μ m.
Among the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, preferred, described nickel salt solution, cobalt salt solution and aluminum salt solution comprise the chlorate aqueous solution, sulfate solution or the nitrate aqueous solution of metallic element correspondence separately respectively.
Among the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described nickel salt, cobalt salt, aluminium salt three's mole proportion optimization is (70～90): (10～30): (1～10).
Among the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described enveloping agent solution is preferably ammoniacal liquor or the ammonium salt solution of 1M～14M.
Among the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described precipitant solution is preferably highly basic or the carbonate solution of 1N～5N.
Among the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, the end liquid that is equipped with in the reactor before the reaction of described primary sedimentation is preferably ammoniacal liquor or ammonium salt solution, and its pH value is preferably 10～12.5, temperature is preferably 45 ℃～70 ℃; The end liquid that is equipped with in the reactor before the described secondary precipitation reaction is preferably strong base solution, and its pH value is preferably 8.5～10.0, temperature is preferably 45 ℃～70 ℃.
The preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, in the described primary sedimentation course of reaction, the pH value of reaction system preferably maintains 10.5～12.5, and the basicity of controlling reaction system simultaneously is 11.0～16.0, and reaction temperature preferably is controlled at 50 ℃～70 ℃.In described secondary precipitation course of reaction, the pH value of reaction system preferably is controlled at 7.0～10.0(and can adopts sodium hydroxide solution to regulate), reaction temperature preferably is controlled at 50 ℃～70 ℃.
The preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, double sintering in the described step (2) comprises one-stage sintering and bis sintering successively, described one-stage sintering is meant that preferably at 400 ℃～650 ℃ roasting temperature 2h～15h, described bis sintering preferably is meant at 680 ℃～800 ℃ roasting temperature 10h～40h.
The mol ratio in precursor of lithium ionic cell positive material and lithium source is preferably 1 among the preparation method of above-mentioned lithium ion battery anode material nickel cobalt aluminium, described step (2): (1.0～1.2).Subsequent treatment in the described step (2) is meant that the roasting material surface after fragmentation coats a spot of cobalt, manganese, magnesium, titanium, zirconium or aluminium element again.Lithium source substance selects conventional lithium source to get final product in the described step (2), preferably comprises one or more the mixture in lithium carbonate, lithium hydroxide, the lithium nitrate.
Compared with prior art, the invention has the advantages that: the lithium ion battery anode material nickel cobalt aluminium (NCA) that utilizes the inventive method preparation, its specific capacity can reach 170 mAh/g～190mAh/g, and 300 all 1C charge and discharge cycles capability retentions are near 90%, and tap density is 2.7 g/cm
3～3.2 g/cm
3, average grain diameter is 5 μ m～20 μ m, as seen, the anode material nickel cobalt aluminium of the present invention's preparation has very high capacity and good cycle performance.In addition, preparation method of the present invention requires low to synthesis device, can realize the automaticity height, and is simple to operate, the production efficiency height, and sintering process is simple, environmental friendliness, waste of raw materials is few, is fit to very much suitability for industrialized production.
Description of drawings
Fig. 1 is the process chart of preparation technology in the embodiment of the invention.
Fig. 2 is the NCA presoma sem photograph that the preparation technology of the embodiment of the invention 1 makes.
Fig. 3 is the NCA sem photograph that the preparation technology of the embodiment of the invention 1 makes.
Fig. 4 is the X-ray diffractogram of the NCA that makes of the preparation technology of the embodiment of the invention 1.
Embodiment
Below in conjunction with Figure of description and specific embodiment the present invention is further described.
Embodiment 1:
A kind of preparation method of lithium ion battery anode material nickel cobalt aluminium of the present invention as shown in Figure 1 may further comprise the steps:
(1) preparation of nickel cobalt aluminium presoma: took by weighing nickelous sulfate and cobaltous sulfate crystal in 8: 2 in molar ratio, after water-soluble nickel sulfate solution and cobalt sulfate solution are mixed, the volume that mixes back solution is 6L, wherein concentration of metal ions is 1.0M, this nickel cobalt mixed solution adds in the reactor that volume is 10L (charging rate of nickel cobalt mixed solution is 0.6L/h) with the ammonia spirit of 14M and sodium hydroxide solution and the stream of 2M again, fill 1.0L, pH value in the reactor and be 11.5, temperature is 60 ℃ end liquid (ammoniacal liquor), add thermal agitation and carry out the primary sedimentation reaction; In the primary sedimentation course of reaction, the pH value by sodium hydroxide solution control reaction system is 11.0～11.2, and the basicity of controlling reaction system with ammoniacal liquor is 13.5～14.5 simultaneously, and reaction temperature is controlled at 55 ℃～60 ℃; Treat whole reinforced the finishing of nickel cobalt mixed liquor, carry out Separation of Solid and Liquid behind the ageing 1.0h, again the solid material after separating is carried out cyclic washing with deionized water; Cleaning solution pH value after washing is 10 when following (being not less than 8.5), stop to wash and the solid material being joined in the reactor, it is 8.5～10.0 that the pH value is housed in this reactor, temperature is a liquid at the bottom of 45 ℃～70 ℃ the NaOH, the aluminum nitrate solution 2L that slowly drips 0.2M again in reactor carries out secondary precipitation reaction (charging rate is 0.5L/h), with the pH value of the NaOH regulation system of 2M 7.0～10.0, the control mixing speed is at 300rpm, the reinforced back ageing 1h that finishes carries out Separation of Solid and Liquid, solid matter with deionized water after the separation wash to the cleaning solution conductivity below 50 μ s/cm, 105 ℃ of oven dry, obtain having the precursor of lithium ionic cell positive material of hud typed structure, the electromicroscopic photograph of this presoma as shown in Figure 2;
(2) preparation of nickel cobalt aluminium positive electrode: the precursor of lithium ionic cell positive material that above-mentioned steps (1) is made mixes with lithium source lithium hydroxide, the mol ratio of precursor of lithium ionic cell positive material and lithium hydroxide is 1: 1.03, mix and be placed in the atmosphere furnace that is connected with oxygen, under logical oxygen condition, carry out double sintering, wherein, one-stage sintering is at 550 ℃ of roasting temperature 5h, is warming up to 730 ℃ then and carries out bis sintering, bis sintering roasting 30h; Roasting material after the double sintering is sized mixing with the aluminum nitrate solution of 0.01M through cooling off fragmentation again, and liquid-solid ratio is 1: 2, dries back 550 ℃ of tempering 10h(metallized aluminum elements), obtain lithium ion battery anode material nickel cobalt aluminium (NCA material) as shown in Figure 3.
After testing, the diffracting spectrum of the lithium ion battery anode material nickel cobalt aluminium in the present embodiment as shown in Figure 4, the D50 particle diameter of this lithium ion battery anode material nickel cobalt aluminium is 9.88 μ m, average grain diameter 10.07 μ m, tap density 3.02g/cm
3, processing characteristics is good when being made into the actual effect battery, and capacity is 176mAh/g, and 300 all 1C charge/discharge capacity conservation rates are 89.8%, and battery does not have bad variations such as bulging.60 ℃ are shelved 7 days capacity conservation rates is 85%, capacity restoration rate 88%, no inflatable.
Embodiment 2:
A kind of preparation method of lithium ion battery anode material nickel cobalt aluminium of the present invention as shown in Figure 1 may further comprise the steps:
(1) step of present embodiment (1) is identical with the step (1) of embodiment 1;
(2) preparation of nickel cobalt aluminium positive electrode: the precursor of lithium ionic cell positive material that above-mentioned steps (1) is made mixes with lithium source lithium carbonate, the mol ratio of precursor of lithium ionic cell positive material and lithium carbonate is 1: 1.05, mix and be placed in the atmosphere furnace that is connected with oxygen, under logical oxygen condition, carry out double sintering, wherein, one-stage sintering is at 620 ℃ of roasting temperature 5h, is warming up to 730 ℃ then and carries out bis sintering, bis sintering roasting 30h; Roasting material after the double sintering is sized mixing with the aluminum nitrate solution of 0.01M through cooling off fragmentation again, and liquid-solid ratio is 1: 2, dries back 550 ℃ of tempering 10h, obtains lithium ion battery anode material nickel cobalt aluminium.
Show good processing characteristics after the NCA material that makes of present embodiment becomes the actual effect battery, capacity is 173mAh/g, and 300 all 1C charge/discharge capacity conservation rates are 87.2%, and battery does not have bad variations such as bulging.
Embodiment 3:
A kind of preparation method of lithium ion battery anode material nickel cobalt aluminium of the present invention as shown in Figure 1 may further comprise the steps:
(1) step of present embodiment (1) is identical with the step (1) of embodiment 1;
(2) preparation of nickel cobalt aluminium positive electrode: the precursor of lithium ionic cell positive material that above-mentioned steps (1) is made mixes (wherein the mol ratio of lithium hydroxide and lithium carbonate is 3: 7) with the lithium source of mixing of lithium hydroxide and lithium carbonate, precursor of lithium ionic cell positive material is 1: 1.05 with the mol ratio of mixing the lithium source, mix and be placed in the atmosphere furnace that is connected with oxygen, under logical oxygen condition, carry out double sintering, wherein, one-stage sintering is at 620 ℃ of roasting temperature 5h, be warming up to 730 ℃ then and carry out bis sintering, bis sintering roasting 30h; Roasting material after the double sintering is sized mixing with the aluminum nitrate solution of 0.01M through cooling off fragmentation again, and liquid-solid ratio is 1: 2, dries back 550 ℃ of tempering 10h, obtains lithium ion battery anode material nickel cobalt aluminium.
Show good processing characteristics after the NCA material that makes of present embodiment becomes the actual effect battery, capacity is 175mAh/g, and 300 all 1C charge/discharge capacity conservation rates are 87.9%, and battery does not have bad variations such as bulging.
By above each embodiment as seen, the anode material for lithium-ion batteries NCA high comprehensive performance of the present invention's preparation has characteristics such as capacity height, good cycle.
Claims (10)
1. the preparation method of a lithium ion battery anode material nickel cobalt aluminium may further comprise the steps:
(1) preparation of nickel cobalt aluminium presoma: nickel salt solution and cobalt salt solution are mixed, mixing back solution metal ion concentration is 0.5M～2.0M, again enveloping agent solution, precipitant solution are added with described mixing back solution and stream and be equipped with in the reactor of end liquid, add thermal agitation and carry out the primary sedimentation reaction, treat fully to begin the slip that overflows is carried out Separation of Solid and Liquid after the reaction, again the solid material after separating is washed; When the cleaning solution pH value after the washing reaches 8.5～11.5, stop to wash and the solid material is joined in the reactor that end liquid is housed, the aluminum salt solution and the precipitant solution that slowly drip 0.1M～1.0M again in reactor are carried out the secondary precipitation reaction, constantly stir, make aluminium element be deposited to this solid material surface gradually, fully after the reaction, the slip that overflows is carried out Separation of Solid and Liquid, solid product after the separation through the washing, the oven dry after, the precursor of lithium ionic cell positive material that obtains having hud typed structure;
(2) preparation of nickel cobalt aluminium positive electrode: the precursor of lithium ionic cell positive material that above-mentioned steps (1) is made mixes with the lithium source, under logical oxygen condition, carry out double sintering, roasting material after the double sintering obtains lithium ion battery anode material nickel cobalt aluminium through fragmentation and subsequent treatment.
2. the preparation method of lithium ion battery anode material nickel cobalt aluminium according to claim 1, it is characterized in that described nickel salt solution, cobalt salt solution and aluminum salt solution comprise the chlorate aqueous solution, sulfate solution or the nitrate aqueous solution of metallic element correspondence separately respectively.
3. the preparation method of lithium ion battery anode material nickel cobalt aluminium according to claim 1 is characterized in that, described nickel salt, cobalt salt, aluminium salt three's mole proportioning is (70～90): (10～30): (1～10).
4. the preparation method of lithium ion battery anode material nickel cobalt aluminium according to claim 1 is characterized in that, described enveloping agent solution is ammoniacal liquor or the ammonium salt solution of 1M～14M.
5. the preparation method of lithium ion battery anode material nickel cobalt aluminium according to claim 1 is characterized in that, described precipitant solution is highly basic or the carbonate solution of 1N～5N.
6. according to the preparation method of each described lithium ion battery anode material nickel cobalt aluminium in the claim 1～5, it is characterized in that, the end liquid that is equipped with in the reactor before the reaction of described primary sedimentation is ammoniacal liquor or ammonium salt solution, and its pH value is 10～12.5, temperature is 45 ℃～70 ℃; The end liquid that is equipped with in the reactor before the described secondary precipitation reaction is strong base solution, and its pH value is 8.5～10.0, temperature is 45 ℃～70 ℃.
7. according to the preparation method of each described lithium ion battery anode material nickel cobalt aluminium in the claim 1～5, it is characterized in that, in the described primary sedimentation course of reaction, the pH value of reaction system maintains 10.5～12.5, the basicity of controlling reaction system simultaneously is 11.0～16.0, and reaction temperature is controlled at 50 ℃～70 ℃.
8. according to the preparation method of each described lithium ion battery anode material nickel cobalt aluminium in the claim 1～5, it is characterized in that in the described secondary precipitation course of reaction, the pH value of reaction system is controlled at 7.0～10.0, reaction temperature is controlled at 50 ℃～70 ℃.
9. according to the preparation method of each described lithium ion battery anode material nickel cobalt aluminium in the claim 1～5, it is characterized in that, double sintering comprises one-stage sintering and bis sintering successively in the described step (2), described one-stage sintering is meant that at 400 ℃～650 ℃ roasting temperature 2h～15h, described bis sintering is meant at 680 ℃～800 ℃ roasting temperature 10h～40h.
10. according to the preparation method of each described lithium ion battery anode material nickel cobalt aluminium in the claim 1～5, it is characterized in that the mol ratio in precursor of lithium ionic cell positive material and lithium source is 1 in the described step (2): (1.0～1.2); Described subsequent treatment is meant that the roasting material surface after fragmentation coats a spot of cobalt, manganese, magnesium, titanium, zirconium or aluminium element again.
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