CN102013489B - Metallic titanium doped carbon-coating lithium iron phosphate and preparation method thereof - Google Patents

Metallic titanium doped carbon-coating lithium iron phosphate and preparation method thereof Download PDF

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CN102013489B
CN102013489B CN2010105227174A CN201010522717A CN102013489B CN 102013489 B CN102013489 B CN 102013489B CN 2010105227174 A CN2010105227174 A CN 2010105227174A CN 201010522717 A CN201010522717 A CN 201010522717A CN 102013489 B CN102013489 B CN 102013489B
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lithium
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iron phosphate
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CN102013489A (en
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韩恩山
朱令之
靳素芳
张俊平
刘吉云
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Hebei University of Technology
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Abstract

The invention discloses metallic titanium doped carbon-coating lithium iron phosphate and a preparation method thereof, which belong to the technical field of battery material preparation. The lithium iron phosphate has the chemical formula: LiFe1-xTixPO4/C, wherein x is greater than 0 and is smaller than or equal to 0.2, and the C has the mass percent of 10%. The preparation method comprises the follow steps of: weighing and proportioning lithium sources, Fe2O3, TiO2 and NH4H2PO4 at the mol ratio of lithium to iron to titanium to phosphorus being 1 to 1-x to x to 1, wherein x is greater than 0 and is smaller than or equal to 0.2; then, grinding the materials after acetone addition, adding a saturated aqueous solution of citric acid after drying to be prepared into rheological phase precursor, grinding the precursor for 3 to 6h at the constant temperature of 400 DEG C under inert atmosphere and pressing the ground precursor into tight cylinder bodies; and finally, raising the temperature to 500 to 900 DEG C and roasting for 5 to 15h at the constant temperature to obtain the product. The prepared material has the characteristics of high capacity and high tap density; and the preparation method is simple, has lower cost and is applied to industrial production.

Description

A kind of metallic titanium doped carbon-coating lithium iron phosphate and preparation method thereof
Technical field
The present invention relates to the battery material preparing technical field, be specially a kind of metallic titanium doped carbon-coating lithium iron phosphate and preparation method thereof.
Background technology
Lithium ion battery is as a kind of high performance green power supply, in various portable type electronic products and communication tool, be widely used in recent years, and progressively be developed as the electrical source of power of electric automobile, thereby promoted it to the future development of safety, environmental protection, low cost and high-energy-density.
Positive electrode is the key component that determines performance of lithium ion battery.Become the focus of various countries' research at LiFePO4 today of more paying attention to safety and environmental protection.LiFePO 4 material is nontoxic, environmentally friendly, raw material sources is abundant, cheap, high temperature stability performance is good, and use fool proof, store up good electrical property, discharge and recharge the life-span and can reach 2000 times with first-class plurality of advantages.
Up to the present, synthetic method about material has a lot of reports, studying more also most possible realization industrialized is high temperature solid-state method, but LiFePO4 has its intrinsic shortcoming,, electric conductivity difference low such as the lithium ion diffusion coefficient etc., weakness such as so the material electrochemical performance that conventional method is prepared are not good, particle diameter skewness, tap density are lower,, tap density serious such as material capacity decay under the large multiplying power only has 1.0g/ml.In order to improve the performance of material, generally be that it is mixed or coats, coat (CN101172599, CN101442117, CN101764205A, CN101777636A), transient metal doped (CN1785799), rear-earth-doped (CN1830764, CN101630738) etc. such as C, above method can improve the performance of LiFePO4 to a certain extent, but the raising of performance is not too remarkable.
Summary of the invention:
The present invention is directed to the deficiency of present material, a kind of metallic titanium doped carbon-coating lithium iron phosphate and preparation method thereof is provided, the material electrochemical performance of the method preparation is good, and especially capacity attenuation is minimum under high current density, and the tap density of this product is higher.This material synthesis method is simple, and cost is lower, is fit to suitability for industrialized production.
Technical scheme of the present invention is:
A kind of metallic titanium doped carbon-coating lithium iron phosphate, the chemical expression of this material is: LiFe 1-xTi xPO 4/ C, 0＜x≤0.2 wherein, the mass percent of C is 10%.
The preparation method of described metallic titanium doped carbon-coating lithium iron phosphate comprises the steps:
(1) with lithium source, Fe 2O 3, TiO 2And NH 4H 2PO 4Lithium in molar ratio: iron: titanium: phosphorus=1: 1-x: x: 1 ratio weighing is prepared burden, wherein 0＜x≤0.2;
(2) powder that disposes is added acetone and be placed in the ball mill and rotate 2-10h under the speed with 200-500rpm/min, the amount of acetone is 3～5 times of powder volume;
(3) slurry after 100～110 ℃ of lower drying and grinding in baking oven, the saturated aqueous solution that adds afterwards citric acid is made the precursor of rheology phase, and wherein the quality of citric acid is step (1) Raw lithium source, Fe by its phosphorus content 2O 3, TiO 2, NH 4H 2PO 420% of quality sum is calculated;
(4) with above-mentioned precursor under inert atmosphere, heat up with the 1 ℃/min rate of heat addition, in 100 ℃ of constant temperature 2～5h, be warming up to again 400 ℃ of constant temperature 3-6h, grind with taking out after the stove cooling, under 100-200MPa pressure, it is pressed into tight cylinder;
(5) cylinder that presses is warming up to 500-900 ℃ of constant temperature calcining 5-15h under inert atmosphere, is cooled to room temperature with stove and obtains the titanium doped carbon-covering lithium iron phosphate of anode material for lithium-ion batteries.
Described lithium source is lithium carbonate, lithium dihydrogen phosphate or lithium fluoride.
Beneficial effect of the present invention is: the material of the present invention's preparation has high power capacity, and the characteristics of high-tap density and this kind material preparation method are simple, and cost is lower, is fit to suitability for industrialized production.
Utilize the titanium doped LiFe that covers carbon of prescription preparation of the present invention 0.9Ti 0.1PO 4/ C material, 0.2C specific discharge capacity is higher than 150mAh/g, the specific discharge capacity of this material is still up to 98.8mAh/g under large multiplying power 5C, 20 capacity attenuations that circulate are 96.2mAh/g, the capacity attenuation rate only is 2.6%, and decay to 43.4mAh/g without material 20 specific discharge capacities of circulation under large multiplying power 5C of overdoping from 84.3mAh/g, and the capacity attenuation rate is 48.5%, the tap density of this material reaches 1.62g/ml in addition.
To select di-iron trioxide be source of iron to material preparation among the present invention, and conductive agent adds in the material presoma, and a part is used for reducing ferric iron, and unnecessary reduction carbon directly is coated on LiFePO 4On the particle, do not need the coating in later stage to process the conductivity that can improve material, cost is lower, is fit to suitability for industrialized production.In order better to set forth scientific meaning of the present invention and real value, be elaborated below in conjunction with embodiment and accompanying drawing.
Description of drawings:
Accompanying drawing 1 obtains four kinds of product LiFePO for embodiment 1 is made 4/ C, LiFe 0.93Ti 0.07PO 4/ C, LiFe 0.9Ti 0.1PO 4/ C, LiFe 0.83Ti 0.17PO 4The XRD curve of/C can find out that product is the LiFePO4 of olivine-type structure, and the doping of Titanium element does not change the structure of material.
Accompanying drawing 2 obtains four kinds of product LiFePO for embodiment 1 is made 4/ C, LiFe 0.93Ti 0.03PO 4/ C, LiFe 0.9Ti 0.1PO 4/ C, LiFe 0.83Ti 0.17PO 4The first charge-discharge curve of/C under the 0.2C multiplying power.
Accompanying drawing 3 is embodiment 1,2,3 preparation LiFe 0.9Ti 0.1PO 4/ C material is at 0.2C, 0.5C, 2C, the cycle performance curve under the 5C multiplying power.
Accompanying drawing 4 is LiFePO 4/ C and LiFe 0.9Ti 0.1PO 4/ C material is at 0.2C, 0.5C, 2C, the cycle performance curve under the 5C multiplying power.
Embodiment:
Embodiment 1
(1) accurate weighing 0.025molLi 2CO 3, 0.0225molFe 2O 3, 0.005molTiO 2And 0.05molNH 4H 2PO 4Putting into ball grinder prepares burden;
(2) acetone that the powder that disposes is added 4 times of powder volumes is placed in the ball mill and rotates 5h under the speed with 250rpm/min;
(3) slurry after 110 ℃ of lower drying and grinding in baking oven adds the precursor that the saturated aqueous solution that contains the 2.2g citric acid is made the rheology phase afterwards;
(4) with above-mentioned precursor under inert atmosphere, heat up with the 1 ℃/min rate of heat addition, in 100 ℃ of constant temperature 2h, be warming up to again 400 ℃ of constant temperature 5h, grind with taking out after the stove cooling, under 200MPa pressure, it is pressed into tight cylinder;
(5) cylinder that presses is warming up to 850 ℃ of constant temperature calcining 12h under high pure nitrogen atmosphere, be cooled to room temperature with stove and obtain the titanium doped carbon-covering lithium iron phosphate 8.7g of anode material for lithium-ion batteries, wherein the quality of carbon is 0.87g (citric acid participates in reduction reaction and decomposes the afterwards quality of remaining carbon).
Prepare titanium doped carbon-covering lithium iron phosphate material, wherein the theory of iron and titanium elements is than Fe: Ti=0.9: 0.1 (can be expressed as LiFe 0.9Ti 0.1PO 4, following same).
The electrochemical property test of material carries out as follows, first positive electrode is painted electrode slice, the bonding agent that the preparation of electrode slice is adopted is the nmp solution of 0.02mol/L PVDF, take by weighing active material at 85: 8: 7 according to mass ratio, the adhesive solution of acetylene black and respective amount, grind evenly, drip certain adhesive solution, stir and be coated on the aluminium foil, dry 24h under 100 ℃ of conditions, the pole piece that scribbles positive electrode is washed into the disk that diameter is about 10mm, the positive plate activity substance content is controlled between 8～10mg, use the metal lithium sheet conduct to electrode, Celgard2400 is barrier film, and 1mol/LLiPF6/EC+DMC+EMC (volume ratio 1: 1: 1) is electrolyte, be assembled into button cell in (relative humidity≤4%) glove box of logical dry air, battery pack leaves standstill 24h after installing and finishing.
Embodiment 2
(1) accurate weighing 0.025molLi 2CO 3, 0.025molFe 2O 3And 0.05molNH 4H 2PO 4Putting into ball grinder prepares burden;
(2) acetone that the powder that disposes is added 4 times of powder volumes is placed in the ball mill and rotates 5h under the speed with 250rpm/min;
(3) slurry after 110 ℃ of lower drying and grinding in baking oven adds the precursor that the saturated aqueous solution that contains the 2.2g citric acid is made the rheology phase afterwards;
(4) with above-mentioned precursor under inert atmosphere, heat up with the 1 ℃/min rate of heat addition, in 100 ℃ of constant temperature 2h, be warming up to again 400 ℃ of constant temperature 5h, grind with taking out after the stove cooling, under 200MPa pressure, it is pressed into tight cylinder;
(5) cylinder that presses is warming up to 850 ℃ of constant temperature calcining 12h under inert atmosphere, is cooled to room temperature with stove and obtains the titanium doped carbon-covering lithium iron phosphate 8.7g of anode material for lithium-ion batteries.
Prepare the LiFePO 4 material that covers carbon, wherein the theory of each element is than being LiFePO 4
Embodiment 3
(1) accurate weighing 0.025molLi 2CO 3, 0.02325molFe 2O 3, 0.0035molTiO 2And 0.05molNH 4H 2PO 4Putting into ball grinder prepares burden;
(2) acetone that the powder that disposes is added 4 times of powder volumes is placed in the ball mill and rotates 5h under the speed with 250rpm/min;
(3) slurry after 110 ℃ of lower drying and grinding in baking oven adds the precursor that the saturated aqueous solution that contains the 2.2g citric acid is made the rheology phase afterwards;
(4) with above-mentioned precursor under inert atmosphere, heat up with the 1 ℃/min rate of heat addition, in 100 ℃ of constant temperature 2h, be warming up to again 400 ℃ of constant temperature 5h, grind with taking out after the stove cooling, under 200MPa pressure, it is pressed into tight cylinder;
(5) cylinder that presses is warming up to 850 ℃ of constant temperature calcining 12h under inert atmosphere, is cooled to room temperature with stove and obtains the titanium doped carbon-covering lithium iron phosphate 8.7g of anode material for lithium-ion batteries.
Prepare the titanium doped LiFePO 4 material that covers carbon, wherein the theory of each element is than being LiFe 0.93Ti 0.07PO 4
Embodiment 4
(1) accurate weighing 0.025molLi 2CO 3, 0.02175molFe 2O 3, 0.0085molTiO 2And 0.05molNH 4H 2PO 4Putting into ball grinder prepares burden;
(2) acetone that the powder that disposes is added 4 times of powder volumes is placed in the ball mill and rotates 5h under the speed with 250rpm/min;
(3) slurry after 110 ℃ of lower drying and grinding in baking oven adds the precursor that the saturated aqueous solution that contains the 2.2g citric acid is made the rheology phase afterwards;
(4) with above-mentioned precursor under inert atmosphere, heat up with the 1 ℃/min rate of heat addition, in 100 ℃ of constant temperature 2h, be warming up to again 400 ℃ of constant temperature 5h, grind with taking out after the stove cooling, under 200MPa pressure, it is pressed into tight cylinder;
(5) cylinder that presses is warming up to 850 ℃ of constant temperature calcining 12h under inert atmosphere, is cooled to room temperature with stove and obtains the titanium doped carbon-covering lithium iron phosphate 8.7g of anode material for lithium-ion batteries.
Prepare the titanium doped LiFePO 4 material that covers carbon, wherein the theory of each element is than being LiFe 0.87Ti 0.13PO 4
The cell parameter data of table 1 embodiment 1,2,3 and four kinds of materials of 4 preparations
Upper table is embodiment 1,2, the cell parameter data of four kinds of materials of 3 and 4 preparations, and the XRD data of these data from accompanying drawing 1 draw, as can be seen from the table LiFe 0.9Ti 0.1PO 4The a value of/C material is less, and the c value is larger, and namely the c/a value is larger, and the lithium ion diffusion of this material of this kind is easier, and namely the conductivity of material is better.
The charge-discharge performance test of battery is at room temperature carried out, carry out the constant current charge-discharge test with Wuhan gold promise cell tester, embodiment 1,2, four kinds of materials first charge-discharge under the 0.2C multiplying power of 3 and 4 preparations, when the charging/discharging voltage scope is 2.4～4.2V, capacity reaches respectively 151mAh/g, 142mAh/g, 146mAh/g and 121mAh/g, as shown in Figure 2, the LiFe of preparation among the visible embodiment 1 0.9Ti 0.1PO 4The first discharge specific capacity of/C material is larger.Fig. 4 is embodiment 1 and 2 cycle performance curves under different discharging currents, can find out no matter be material LiFe among the embodiment 1 under little electric current or the large electric current 0.9Ti 0.1PO 4The specific discharge capacity of/C all large and decay little, LiFe under large multiplying power 5C especially 0.9Ti 0.1PO 4The specific discharge capacity of/C material is 98.1mAh/g still, circulates for 20 weeks, and capacity attenuation is 96.2mAh/g, and the capacity attenuation rate only is 1.9%, unadulterated material in the embodiment 2.
Embodiment 5
(1) accurate weighing 0.05mol LiH 2PO 4, 0.0225mol Fe 2O 3With 0.005mol TiO 2Putting into ball grinder prepares burden;
(2) acetone that the powder that disposes is added 4 times of powder volumes is placed in the ball mill and rotates 5h under the speed with 250rpm/min;
(3) slurry after 110 ℃ of lower drying and grinding in baking oven adds the precursor that the saturated aqueous solution that contains the 1.8g citric acid is made the rheology phase afterwards;
(4) with above-mentioned precursor under inert atmosphere, heat up with the 1 ℃/min rate of heat addition, in 100 ℃ of constant temperature 2h, be warming up to again 400 ℃ of constant temperature 5h, grind with taking out after the stove cooling, under 200MPa pressure, it is pressed into tight cylinder;
(5) cylinder that presses is warming up to 850 ℃ of constant temperature calcining 12h under inert atmosphere, is cooled to room temperature with stove and obtains the titanium doped carbon-covering lithium iron phosphate 8.7g of anode material for lithium-ion batteries.
Prepare the titanium doped LiFePO 4 material that covers carbon, wherein the theory of each element is than being LiFe 0.9Ti 0.1PO 4
Embodiment 6
(1) accurate weighing 0.05mol LiF, 0.0225mol Fe 2O 3, 0.005mol TiO 2With 0.05mol NH 4H 2PO 4Putting into ball grinder prepares burden;
(2) acetone that the powder that disposes is added 4 times of powder volumes is placed in the ball mill and rotates 5h under the speed with 250rpm/min;
(3) slurry after 110 ℃ of lower drying and grinding in baking oven adds the precursor that the saturated aqueous solution that contains the 2.1g citric acid is made the rheology phase afterwards;
(4) with above-mentioned precursor under inert atmosphere, heat up with the 1 ℃/min rate of heat addition, in 100 ℃ of constant temperature 2h, be warming up to again 400 ℃ of constant temperature 5h, grind with taking out after the stove cooling, under 200MPa pressure, it is pressed into tight cylinder;
(5) cylinder that presses is warming up to 850 ℃ of constant temperature calcining 12h under inert atmosphere, is cooled to room temperature with stove and obtains the titanium doped carbon-covering lithium iron phosphate 8.7g of anode material for lithium-ion batteries.
Prepare the titanium doped LiFePO 4 material that covers carbon, wherein the theory of each element is than being LiFe 0.9Ti 0.1PO 4
From the cycle performance curve of embodiment 1,5 and 6 three kinds of materials that prepare, namely accompanying drawing 3 can be found out with Li 2CO 3For the chemical property of lithium source synthetic material better, under different multiplying capacity higher and under large multiplying power 5C decay be minimum.

Claims (1)

1. the preparation method of a metallic titanium doped carbon-coating lithium iron phosphate is characterized by the chemical expression that the method prepares material and is: LiFe 1-xTi xPO 4/ C, 0.07＜x≤0.2 wherein, the mass percent of C is 10%; Comprise the steps:
(1) with lithium source, Fe 2O 3, TiO 2And NH 4H 2PO 4Lithium in molar ratio: iron: titanium: phosphorus=1: 1-x: x: 1 ratio weighing is prepared burden, wherein 0.07＜x≤0.2;
(2) powder that disposes is added acetone and be placed in the ball mill and rotate 2-10h under the speed with 200-500rpm/min, the amount of acetone is 3～5 times of powder volume;
(3) slurry after 100～110 ℃ of lower drying and grinding in baking oven, the saturated aqueous solution that adds afterwards citric acid is made the precursor of rheology phase, and wherein the amount of citric acid is step (1) Raw lithium source, Fe by its phosphorus content 2O 3, TiO 2And NH 4H 2PO 420% of quality sum is calculated;
(4) with above-mentioned precursor under inert atmosphere, heat up with the 1 ℃/min rate of heat addition, in 100 ℃ of constant temperature 2～5h, be warming up to again 400 ℃ of constant temperature 3-6h, grind with taking out after the stove cooling, under 100-200MPa pressure, it is pressed into tight cylinder;
(5) cylinder that presses is warming up to 500-900 ℃ of constant temperature calcining 5-15h under inert atmosphere, is cooled to room temperature with stove and obtains the titanium doped carbon-covering lithium iron phosphate of anode material for lithium-ion batteries;
Described lithium source is lithium carbonate, lithium dihydrogen phosphate or lithium fluoride.
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EXPY Termination of patent right or utility model