CN103441256A - High-grinding-density lithium titanate preparation method - Google Patents
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Abstract
The invention discloses a high-grinding-density lithium titanate preparation method which comprises the following steps: weighing lithium salt and butyl titanate according to the molar ratio of lithium to titanium being (0.8-0.9):1, then weighing deionized water according to the mass ratio of the deionized water to butyl titanate and lithium salt being (1-5):1, uniformly mixing and drying the above components, and primarily roasting the above components at the temperature of 700-1,000 DEG C for 8-24 hours, then adding carbon black and a binder into the mixture, uniformly mixing the mixture in a grinding machine, eliminating the particle clearances, then putting the mixture into a pelletizer to tablet and pelletize, secondly roasting the mixture at the temperature of 400-1,000 DEG C for 4-8 hours under inert gas shielding atmosphere, then conducting jaw crushing, roller crushing and air flow crushing again, to finally obtain the lithium titanate material with high grinding density and excellent electric performance.
Description
Technical field
The present invention relates to the ion secondary battery cathode material lithium field, relate in particular to a kind of high preparation method who rolls the density lithium titanate.
Background technology
Lithium ion battery is high as a kind of specific energy, the novel secondary chemical cell of environmental protection, just has been subject to each side always and pays close attention to since emerging.Along with over nearly 1 year, the exploitation of lithium ion battery new material and large capacity manufacturing technology, make lithium-ion-power cell become possibility in the application of HEV, is also the main flow of current all types of HEV power driven system research and development.Although the application technology of lithium-ion-power cell in HEV obtained remarkable progress, but the rapid charge characteristic of novel PHEV technology to lithium-ion-power cell, multiplying power discharging property and security performance propose higher requirement, the commercial major obstacle of restriction lithium-ion-power cell HEV is at present: (one) charging interval is long, although the single flying power of lithium ion battery group has all reached the requirement (approximately 65～200Km) of PHEV at present, but owing to being subject to Li-C alloy material of cathode performance limitations, its quick charge capability is poor, charging interval generally needs 3～9 hours again, unsatisfactory, (2) battery pack cost costliness, with Volt, 53KW power output lithium ion battery group system is example, approximately need 10000～15000 U.S. dollar left and right, the battery pack system cost of the 50KW power output of Toyota Prius II is also at least more than 5000 U.S. dollars, this be mainly due to: (1) is the poor stability of lithium ion battery group at present, although the application of high security lithium iron phosphate positive material at present, effectively improved the security performance of lithium ion battery, but in existing Li-C negative pole system owing to there being the active metal lithium, simultaneously owing to being subject to by carbon negative pole performance limitations, lithium ion battery must be used low-flash electrolyte system, battery pack is being heated, overcharge and be subject in the overstocked situation of external force easily to occur blow-up, dangerous situation such as on fire and blast grade, thereby have to add power management module and other supplementary module of large amount of complex during lithium ion battery applications, to guarantee the security performance of system, this is the main cause that causes lithium ion battery cost costliness, (2) used Li-C alloy material of cathode rate charge-discharge poor performance, maintain the HEV job requirement, lithium ion battery is had to adopt the slim design of sacrificing specific energy or increase complicated AC-DC circuit module in the lithium ion battery loop, the effective ratio energy that this has reduced lithium-ion power battery system on the one hand, also increased the cost of lithium-ion battery systems on the other hand, (3) now use the poor shortcoming of Li-C alloy material of cathode cycle life, further increased the use cost of lithium ion battery group in application.But thereby the Novel anode material of exploitation high safety performance fast charging and discharging is one of most critical technology of lithium ion battery HEV popularization and application.
Novel lithium titanate material-Li
4ti
5o
12have larger lithium ion solid-state diffusion constant and sub-micron (or nanometer) particle diameter and distribute, (maximum can be carried out 50C to have excellent rapid charge characteristic (5 minutes full capacitances of charging capacity>=80%) and repid discharge performance
amultiplying power discharging); Lithium titanate anode does not produce lithium metal in charge and discharge process, simultaneously because lithium titanate anode has excellent fast charging and discharging performance, thereby can be used in conjunction with novel full-bodied noninflammability electricity liquid, battery pack can be born the high temperature impact of 240 ℃, has high security performance; Lithium titanate material has stable spinel structure, at charge and discharge process change in volume less (<0.2%), therefore has good cycle life, and 1000 circulation volume conservation rates of high rate charge-discharge still can reach more than 90%.Lithium titanate anode is compared with traditional Li-C negative pole, in the application of high power type lithium ion electrokinetic cell, has advantage,
Yet the lithium titanate material ubiquity that preparation method commonly used prepares at present rolls the too low situation of density, and this has had a strong impact on the performance of its volumetric specific energy.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of method that height rolls the lithium titanate anode material of density, excellent electrical properties that has concurrently for preparing.
In order to solve the problems of the technologies described above, technical solution of the present invention is as follows:
A kind of high preparation method who rolls the density lithium titanate comprises the following steps:
1) mol ratio according to lithium and titanium is that 0.8～0.9:1 takes lithium salts and butyl titanate, then according to quality than deionized water: (butyl titanate+lithium salts)=1～5:1 takes deionized water, and above-mentioned substance is added in high-speed mixer and mixes;
2) slurry step 1) obtained carries out drying;
3) by step 2) material that obtains carries out bakes to burn the article under 700～1000 ℃, and roasting time is 8～24h, obtains lithium titanate material;
4) lithium titanate material step 3) obtained, simple substance carbon black and the binding agent that accounts for lithium titanate material quality 1～4% add in grinding mill and mix, and get rid of gap between particle by mechanical force simultaneously, and controlling carbon quality in final products is 2%～10%;
5) material step 4) obtained joins in comminutor and carries out compressing tablet and granulation;
6) material obtained in step 5) is carried out to after baking under the inert gas shielding atmosphere, sintering temperature is 400～1000 ℃, and roasting time is 4～8h;
7) material after the step 6) roasting is carried out successively to the pulverizing of jaw formula, pair roller pulverizing and air-flow crushing, can obtain final height and roll the density lithium titanate.
Described lithium salts is any one in lithium carbonate, a hydronium(ion) oxidation lithium, lithium acetate and lithium nitrate.
Described simple substance carbon black is any one in Super P, Ensaco and KS-6.
Described binding agent is any one in sucrose, glucose sugar and citric acid.
Described step 2) drying means in is microwave drying or spray drying; The microwave drying temperature is 100～120 ℃, and the spray drying temperature is 200～240 ℃.
In described step 5), the pressure of comminutor compressing tablet is 10～30Mpa.
In described step 7), the high particle size distribution that rolls the density lithium titanate is D
50=3～15 μ m, carbon content is 2%～10%.
In described step 6), inert gas is N
2.
In described step 1), incorporation time is 3-6 hour.
Height provided by the invention rolls density lithium titanate preparation method, by milling work order, powder granule under the effect as compression, shearing, impact, is got rid of to intergranular space by mechanical force, improves material and rolls density and stress; Then pass through sheeting process further by the powder compacting, particle is combined by mechanism.Mill and not only can increase carbon dust with the contacting of lithium titanate with the introducing of sheeting process, guarantee uniformity that carbon coats and the completeness of high temperature solid state reaction, reduce the actual effect internal resistance of cell, improve the high rate performance of product; And can get rid of intergranular space, that improves product rolls density and energy density.
The accompanying drawing explanation
Fig. 1 is phase (XRD) figure that height that embodiment 1 makes rolls the density lithium titanate anode material;
Fig. 2 is that the height of example 1 preparation rolls pattern (SEM) figure of density lithium titanate anode material under electron microscope;
Fig. 3 is that the height of example 1 preparation rolls density lithium titanate anode material button cell charging and discharging curve;
Fig. 4 is that the height of example 1 preparation rolls density lithium titanate actual effect battery cycle life;
Fig. 5 is that the height of example 1 preparation rolls density lithium titanate actual effect battery multiplying power charging curve;
Fig. 6 is that the height of example 1 preparation rolls density lithium titanate actual effect battery multiplying power discharging curve;
Fig. 7 is that the height of example 1 preparation rolls density lithium titanate actual effect over-charging of battery curve.
Embodiment
Below in conjunction with accompanying drawing and instantiation, height provided by the invention being rolled to density lithium titanate preparation method has been described in detail.
A kind of high preparation method who rolls the density lithium titanate, comprise the steps:
1) take respectively lithium carbonate 498g, butyl titanate 5564g and deionized water 30310g, add high-speed mixer mixing 4h, guarantee that each component mixes;
2) by the above-mentioned slurry microwave drying obtained in step 1), baking temperature is 100 ℃;
3) by step 2) dry complete material adds bakes to burn the article in bell furnace, and the roasting standard is 800 ℃ of 8h;
4) by the step 3) bakes to burn the article, complete material 1500g, 30g Super P and 15g sucrose add in mixing roll and mill;
5) step 4) is milled complete material adds in comminutor and carries out the compressing tablet granulation, and the pressure of comminutor is 10Mpa;
6) by the step 5) granulation, complete material is placed in N
2in baking furnace as protective gas, under 400 ℃ of conditions, insulation 4h carries out after baking;
7) by the step 6) roasting, complete material carries out the pulverizing of jaw formula successively, pair roller is pulverized and air-flow crushing, and after pulverizing, the granularity of lithium titanate product is D
50=3.251 μ m, carbon content is 2.18%.
A kind of high preparation method who rolls the density lithium titanate, comprise the steps:
1) take respectively lithium nitrate 929.5g, butyl titanate 5564g and deionized water 19480g, add high-speed mixer mixing 3h, guarantee that each component mixes;
2) by the above-mentioned slurry microwave drying obtained in step 1), baking temperature is 110 ℃;
3) by step 2) dry complete material adds bakes to burn the article in bell furnace, and the roasting standard is 900 ℃ of 12h;
4) by the step 3) bakes to burn the article, complete material 1500g, 30g Ensaco and 15g glucose add in mixing roll and mill;
5) step 4) is milled complete material adds in comminutor and carries out the compressing tablet granulation, and the pressure of comminutor is 10Mpa;
6) by the step 5) granulation, complete material is placed in N
2in baking furnace as protective gas, under 500 ℃ of conditions, insulation 6h carries out after baking;
7) by the step 6) roasting, complete material carries out the pulverizing of jaw formula successively, pair roller is pulverized and air-flow crushing, and after pulverizing, the granularity of lithium titanate product is D
50=10.251 μ m, carbon content is 2.24%.
A kind of high preparation method who rolls the density lithium titanate, comprise the steps:
1) take respectively lithium acetate 868.5g, butyl titanate 5564g and deionized water 12906g, add high-speed mixer mixing 5h, guarantee that each component mixes;
2) by the above-mentioned slurry microwave drying obtained in step 1), baking temperature is 115 ℃;
3) by step 2) dry complete material adds bakes to burn the article in bell furnace, and the roasting standard is 800 ℃ of 24h;
4) by the step 3) bakes to burn the article, complete material 1500g, 90g KS-6 and 45g citric acid add in mixing roll and mill;
5) step 4) is milled complete material adds in comminutor and carries out the compressing tablet granulation, and the pressure of comminutor is 30Mpa;
6) by the step 5) granulation, complete material is placed in N
2in baking furnace as protective gas, under 600 ℃ of conditions, insulation 8h carries out after baking;
7) by the step 6) roasting, complete material carries out the pulverizing of jaw formula successively, pair roller is pulverized and air-flow crushing, and after pulverizing, the granularity of lithium titanate product is D
50=12.231 μ m, carbon content is 6.17%.
A kind of high preparation method who rolls the density lithium titanate, comprise the steps:
1) take respectively a hydronium(ion) oxidation lithium 565g, butyl titanate 5564g, deionized water 6129g, add high-speed mixer mixing 4h, guarantees that each component mixes;
2) by the above-mentioned slurry spray drying obtained in step 1), baking temperature is 200 ℃;
3) by step 2) dry complete material adds bakes to burn the article in bell furnace, and the roasting standard is 800 ℃ of 12h;
4) by the step 3) bakes to burn the article, complete material 1500g, 120g Super P and 60g sucrose add in mixing roll and mill;
5) step 4) is milled complete material adds in comminutor and carries out the compressing tablet granulation, and the pressure of comminutor is 10Mpa;
6) by the step 5) granulation, complete material is placed in N
2in baking furnace as protective gas, under 700 ℃ of conditions, insulation 4h carries out after baking;
7) by the step 6) roasting, complete material carries out the pulverizing of jaw formula successively, pair roller is pulverized and air-flow crushing, and after pulverizing, the granularity of lithium titanate product is D
50=14.842 μ m, carbon content is 8.21%.
A kind of high preparation method who rolls the density lithium titanate, comprise the steps:
1) take respectively a hydronium(ion) oxidation lithium 602g, butyl titanate 5564g, deionized water 9269g, add high-speed mixer mixing 4h, guarantees that each component mixes;
2) by the above-mentioned slurry spray drying obtained in step 1), baking temperature is 240 ℃;
3) by step 2) dry complete material adds bakes to burn the article in bell furnace, and the roasting standard is 800 ℃ of 12h;
4) by the step 3) bakes to burn the article, complete material 1500g, 30g Super P and 15g sucrose add in mixing roll and mill;
5) step 4) is milled complete material adds in comminutor and carries out the compressing tablet granulation, and the pressure of comminutor is 10Mpa;
6) by the step 5) granulation, complete material is placed in N
2in baking furnace as protective gas, under 800 ℃ of conditions, insulation 4h carries out after baking;
7) by the step 6) roasting, complete material carries out the pulverizing of jaw formula successively, pair roller is pulverized and air-flow crushing, and after pulverizing, the granularity of lithium titanate product is D
50=13.251 μ m, carbon content is 2.24%.
The experiment situation:
What table 1 tap density test chart had been listed lithium ion secondary battery cathode material lithium titanate that above-described embodiment makes rolls the density measurement result.
In table, data can be found out, it is higher that lithium titanate material prepared by the present invention rolls density, is greater than 2.2g/cm
3, much larger than the lithium titanate material of general goods, show that the present invention has effectively improved lithium titanate material and rolled density, and the raising that rolls density can improve the specific energy density of lithium titanate battery.
Table 1 tap density test chart
| Sample | Roll density/g.cm ～3 |
| The commercialization lithium titanate | 1.8 |
| Example 1 | 2.25 |
| Example 2 | 2.28 |
| Example 3 | 2.23 |
| Example 4 | 2.31 |
| Example 5 | 2.27 |
Table 2 has been listed the capacitance of cycle charge discharge first and the actual effect cycle performance of battery that utilizes ion secondary battery cathode material lithium that above-described embodiment makes to make button cell.The test condition of button cell is LR2032,0.1C, 1.0～3.0V, vs.Li
+/ Li; The test condition of actual effect battery is, ICP053048, and 5C, 2.0～2.9V, the charging/discharging apparatus of use discharges and recharges instrument for blue electricity.
Table 2 cycle performance test chart
In table, data can be found out, lithium titanate anode material cycle performance prepared by the present invention is fine, and the capability retention after 1000 weeks is still more than 100%.
Fig. 1 is phase (XRD) figure that the height of example 1 preparation rolls the density lithium titanate anode material, and the lithium titanate product prepared is as seen from the figure compared with standard diagram does not have obvious dephasign.
Fig. 2 is that the height of example 1 preparation rolls pattern (SEM) figure of density lithium titanate anode material under electron microscope, and the lithium titanate product made as seen from the figure is the spherical existence of class, and spherical structure is conducive to its raising that rolls density.
Fig. 3 is that the height of example 1 preparation rolls density lithium titanate anode material button cell charging and discharging curve, and specific capacity has reached 167.5mAh/g first as seen from the figure, and enclosed pasture efficiency has reached 99.7% first.
Fig. 4 is that the height of example 1 preparation rolls density lithium titanate actual effect battery cycle life, and the lithium titanate product prepared as seen from the figure has good cycle performance, and the capability retention of 1000 circulations has reached more than 100%.
Fig. 5 and Fig. 6 are that the height of example 1 preparation rolls the charging of density lithium titanate anode material actual effect battery multiplying power and multiplying power discharging property curve, and the lithium titanate product high rate performance that can be prepared by figure is fine.
Fig. 7 is that the height of example 1 preparation rolls density lithium titanate actual effect over-charging of battery curve, overcharges not blast of actual effect battery in process, and security performance is good.
Claims (10)
1. the one kind high preparation method who rolls the density lithium titanate is characterized in that: comprise the following steps:
1) mol ratio according to lithium and titanium is that 0.8～0.9:1 takes lithium salts and butyl titanate, then according to quality than deionized water: (butyl titanate+lithium salts)=1～5:1 takes deionized water, and above-mentioned substance is added in high-speed mixer and mixes;
2) slurry step 1) obtained carries out drying;
3) by step 2) material that obtains carries out bakes to burn the article under 700～1000 ℃, and roasting time is 8～24h, obtains lithium titanate material;
4) lithium titanate material step 3) obtained, simple substance carbon black and the binding agent that accounts for lithium titanate material quality 1～4% add in grinding mill and mix, and get rid of gap between particle by mechanical force simultaneously, and controlling carbon quality in final products is 2%～10%;
5) material step 4) obtained joins in comminutor and carries out compressing tablet and granulation;
6) material obtained in step 5) is carried out to after baking under the inert gas shielding atmosphere, sintering temperature is 400～1000 ℃, and roasting time is 4～8h;
7) material after the step 6) roasting is carried out successively to the pulverizing of jaw formula, pair roller pulverizing and air-flow crushing, obtain final height and roll the density lithium titanate.
2. preparation method as claimed in claim 1, it is characterized in that: described lithium salts is any one in lithium carbonate, a hydronium(ion) oxidation lithium, lithium acetate and lithium nitrate.
3. preparation method as claimed in claim 1, it is characterized in that: described simple substance carbon black is any one in Super P, Ensaco and KS-6.
4. preparation method as claimed in claim 1, it is characterized in that: described binding agent is any one in sucrose, glucose sugar and citric acid.
5. preparation method as claimed in claim 1, it is characterized in that: in described step 6), inert gas is N
2.
6. preparation method as claimed in claim 1 is characterized in that: the pressure in described step 5) during the comminutor compressing tablet is 10～30Mpa.
7. preparation method as claimed in claim 1 is characterized in that: in described step 7), the high particle size distribution that rolls the density lithium titanate is D
50=3～15 μ m.
8. preparation method as claimed in claim 1, it is characterized in that: in described step 1), incorporation time is 3-6 hour.
9. preparation method as claimed in claim 1 is characterized in that: described step 2), drying means is microwave drying or spray drying.
10. preparation method as claimed in claim 9, it is characterized in that: described microwave drying temperature is 100～120 ℃, the spray drying temperature is 200～240 ℃.
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| CN106876675A (en) * | 2017-03-23 | 2017-06-20 | 福建翔丰华新能源材料有限公司 | A kind of lithium ion battery preparation method of lithium titanate composite cathode material of silicon/carbon/graphite |
| CN108365213A (en) * | 2018-04-04 | 2018-08-03 | 湖南格兰博智能科技有限责任公司 | A kind of preparation method and lithium ion battery of lithium titanate anode material |
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