CN101222044A - Novel conductive agent doping/coating lithium iron phosphate material and its production method - Google Patents
Novel conductive agent doping/coating lithium iron phosphate material and its production method Download PDFInfo
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- CN101222044A CN101222044A CNA2007101507884A CN200710150788A CN101222044A CN 101222044 A CN101222044 A CN 101222044A CN A2007101507884 A CNA2007101507884 A CN A2007101507884A CN 200710150788 A CN200710150788 A CN 200710150788A CN 101222044 A CN101222044 A CN 101222044A
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Abstract
The invention discloses a novel lithium iron phosphate material which is adulterated /covered with conductive agents and a preparation method thereof. The lithium iron phosphate material of the invention comprises lithium source compounds, iron source compounds, phosphate radical source compounds and the conductive agents of lithium iron phosphates. The technology of the invention is simple; the material is clean and pollution-free; the cost of the material is low. The invention is suitable for industrialized mass production. Specific capacity of the obtained lithium iron phosphate material is high (more than 140 mAh/g); cyclical stability is good (more than 300 times); high rate charging and discharging performance of the lithium iron phosphate material is particularly prominent (5C capacity can still reach 80 mAh/g); conductivity and stacking density are high; diffusivity of protons is improved; contact between active materials and an electrode is increased; internal resistance of the electrode and a battery is reduced; discharging and cyclical stabilities of the electrode are obviously improved. The invention is widely applied to novel high performance lithium ion batteries.
Description
Technical field
The invention belongs to the energy and material technical field, particularly a kind of novel conductive agent doping/coated LiFePO 4 for lithium ion batteries material and preparation method.
Background technology
LiFePO4 is considered to one of the most promising lithium ion battery electrode material after the LiFePO4 that Goodenough in 1997 finds to have olivine structural can reversibly embed and deviate from lithium ion.This material has lot of advantages: do not contain precious metal, raw material cheapness, resource are greatly abundant; Nontoxic, environmentally friendly; Operating voltage moderate (3.4V); Platform identity is good, under little electric current, has smooth charging/discharging voltage curve, is a kind of desirable anode material for lithium-ion batteries; Big (the 170mAhg of theoretical capacity
-1), Stability Analysis of Structures, security performance splendid (O and P make material be difficult to analyse oxygen and decompose with the strong covalent bond strong bonded); High-temperature behavior and good cycle; Volume-diminished during charging, the bulk effect when cooperating with carbon negative pole material is good; Good with most of electrolyte system compatibilities, storge quality is good.But there are two significant disadvantages in LiFePO4: the one, and electric conductance is low, causes high-rate discharge ability poor, and actual specific capacity is low, and under the bigger situation of electric current, electrode polarization is serious, causes discharging and recharging irreversible degree and strengthens, and the electrochemistry capacitance loss is serious; The 2nd, bulk density is low, causes volume and capacity ratio low, and this brings certain difficulty for the practicality of LiFePO4.
In order to improve the electronic conductivity of LiFePO4, main element doping/coating, the method that reduces the product particle diameter and add conductive agent of adopting of a lot of researchs.Wherein remarkable to add the conductive agent effect, and be easy to industrialization, yet the multi-conducting agent is different material with carbon elements and carbon source, can reduce its tap density owing to the adding of conductive agent material with carbon element when the LiFePO4 conductivity improves, and two kinds of shortcomings can not overcome simultaneously.In addition, synthetic method also has certain influence to the performance of LiFePO4.Common synthetic method has high temperature solid-state method, sol-gel process, and hydrothermal synthesis method, microwave method, lithium method etc. is inserted in reduction.It is even that the slotting lithium method of wherein reducing has particle size distribution, tap density height, specific capacity height, advantage of low energy consumption.
Summary of the invention
Purpose of the present invention is intended to solve the technical barrier of above-mentioned present stage, thereby a kind of LiFePO 4 material and preparation method of novel conductive agent doping/coating are provided.The LiFePO 4 material of this method preparation has significantly improved the big electric current application performance and the tap density of LiFePO4.
Technical scheme of the present invention discloses a kind of LiFePO 4 material of novel conductive agent doping/coating, it is characterized in that described LiFePO 4 material comprises: press atomic ratio Li: Fe: P=(0.9-1.2): 1: 1 Li source compound, Fe source compound and phosphate radical source compound, and the quality percentage composition is the conductive agent of target product LiFePO4 1%-30%.
The present invention discloses a kind of novel conductive agent doping/coated LiFePO 4 for lithium ion batteries preparation methods, it is characterized in that described preparation methods comprises:
(1) be that the trivalent iron salt aqueous solution, the concentration of 0.2～2M is that 0.2～2M aqueous phosphatic and concentration are that 1～5M aqueous alkali mixes with concentration, stir that the pH value of control mixed solution is 3～5, controlling anti-temperature is 30～80 ℃;
(2) step (1) gained material is carried out Separation of Solid and Liquid, drying gets the ferric phosphate presoma;
(3) in atomic ratio Li: Fe: P=(0.9-1.2): 1: 1 ratio, step (2) gained ferric phosphate presoma, Li source compound and conductive agent are mixed, grind, wherein the consumption of conductive agent is 1～30wt% of LiFePO4.
(4) with step (3) gained mixture in inert atmosphere in 300～450 ℃ the insulation 4～8 hours, grind behind the natural cooling dusty material;
(5) step (4) gained dusty material is ground, compressing tablet was handled 5～24 hours in 450～650 ℃ in inert atmosphere, grind behind the natural cooling the lithium iron phosphate positive material that mixes of conductive agent.
The invention also discloses the preparation method of the LiFePO 4 material of another kind of novel conductive agent doping/coating, it is characterized in that described preparation methods comprises:
(1) be that the trivalent iron salt aqueous solution, the concentration of 0.2～2M is that 0.2～2M aqueous phosphatic and concentration are that 1～5M aqueous alkali mixes with concentration, stir that the pH value of control mixed solution is 3～5, control reaction temperature is 30～80 ℃;
(2) step (1) gained material is carried out Separation of Solid and Liquid, drying gets the ferric phosphate presoma;
(3) in atomic ratio Li: Fe: P=0.9-1.2: 1: 1 ratio, step (2) gained ferric phosphate presoma, Li source compound are carried out mixed grinding, the gained mixture in inert atmosphere in 300～450 ℃ the insulation 4～8 hours, grind behind the natural cooling dusty material; This dusty material grinds, and compressing tablet was handled 5～24 hours in 450～650 ℃ in inert atmosphere, grind behind the natural cooling lithium iron phosphate positive material;
(4) lithium iron phosphate positive material with step (3) gained is distributed under the ultrasonic wave condition in the conductive agent raw material of preparation, and wherein the consumption of conductive agent is 1～30wt% of LiFePO4, obtains the lithium iron phosphate positive material that conductive agent coats through Overheating Treatment.
Li source compound of the present invention is at least a in lithium carbonate, lithium nitrate, lithium acetate or the lithium hydroxide.
Described Fe source compound is at least a in di-iron trioxide, ferric nitrate, ferrous oxalate or the ferric oxalate.
Described phosphate radical source compound is at least a in ammonium phosphate, diammonium hydrogen phosphate or the ammonium dihydrogen phosphate.
Described conductive agent is sulfide: CoS
2, FeS
2, NiS
2, ZnS
2, TeS
2Or MoS
2In one or more.
Described conductive agent is oxide: SnO, ZnO, TiO
2, ZrO
2, CaO, Y
2O
3, RuO
2, SiO
2In one or more.
Described inert protective atmosphere is: nitrogen or argon gas.The flow velocity of described protective atmosphere is 0.1～10dm
3Min
-1
The invention has the beneficial effects as follows: this technology is simple, cleanliness without any pollution, with low cost, be fit to industrial-scale production, the LiFePO 4 material specific capacity height that obtains (＞140mAh/g), good cycling stability (＞300 circulations), its high-rate charge-discharge capability is outstanding (the 5C capacity still can reach 80mAh/g) especially, have high conductance and bulk density, improved the diffusion of proton, increased active material and contacted, reduced electrode with interelectrode, the internal resistance of cell, significantly improved the discharge and the stable circulation performance of electrode, can in the novel high-performance lithium ion battery, be used widely.
Description of drawings
The XRD test curve of Fig. 1 LiFePO4;
The cyclic voltammetry curve in first week of Fig. 2 LiFePO4.
Embodiment
Specific implementation method of the present invention is as follows:
1) compound concentration is the trivalent iron salt aqueous solution of 0.2-2 mol;
Compound concentration is the aqueous phosphatic of 0.2-2 mol;
Compound concentration is the aqueous alkali of 1-5 mol.
2) solution with above-mentioned preparation mixes, and stirs, and the pH value of control mixed solution is 3-5, and control reaction temperature is 30-80 ℃.
3) with step 2) the gained material carries out Separation of Solid and Liquid, drying, hypophosphite monohydrate iron presoma.
4) NH in molar ratio
2CSNH
2: Co
2+=5: 1 ratio is dissolved in thiocarbamide and cobalt nitrate in the ethanol, places water heating kettle in 180 ℃ of insulations 72 hours, takes out the back and gets cobalt disulfide in 12 hours in 60 ℃ of oven dry.
5), get conductive agent with step 4) gained cobalt disulfide and sucrose mixed grinding.
6) in atomic ratio Li: Fe: P=(0.9-1.2): 1: 1 ratio is mixed step 3) gained ferric phosphate presoma with the lithium source, grinds, and wherein the consumption of conductive agent is the 5-20wt% of LiFePO4.
7) with step 6) gained mixture in argon gas atmosphere in 350 ℃ the insulation 4-8 hour, grind behind the natural cooling dusty material.
8) step 7) gained dusty material is ground, compressing tablet was handled 5-20 hour in 450-650 ℃ in argon gas atmosphere, grind behind the natural cooling the lithium iron phosphate positive material that mixes of conductive agent.
If with above-mentioned steps 6)-8) change following steps into, can prepare the lithium iron phosphate positive material that conductive agent coats.
6) in atomic ratio Li: Fe: P=0.9-1.2: 1: 1 ratio, step 5) gained ferric phosphate presoma, Li source compound are carried out mixed grinding, the gained mixture in inert atmosphere in 300～450 ℃ the insulation 4～8 hours, grind behind the natural cooling dusty material; This dusty material grinds, and compressing tablet was handled 5～24 hours in 450～650 ℃ in inert atmosphere, grind behind the natural cooling lithium iron phosphate positive material;
7) lithium iron phosphate positive material with the step 6) gained joins in the conductive agent raw material of preparation, and ultrasonic wave disperseed 0.5 hour, and wherein the consumption of conductive agent is 1～30wt% of LiFePO4, obtains the lithium iron phosphate positive material that conductive agent coats through Overheating Treatment.
Embodiment 1
Take by weighing Fe (NO
3)
39H
2O 4.04g, NH
4H
2PO
41.15g, be dissolved in respectively in the 100mL deionized water, drip and mix, stirring is 5 in 60 ℃ of adding 1 mol ammoniacal liquor to pH value of solution values down, filtration washing is also dry down at 80 ℃.Gained presoma and 0.388g Li
2CO
3, 0.079gCoS
2Mixed grinding, the porcelain crucible of packing into.At flow velocity is 1dm
3Min
-199.999% argon gas stream in, with 3 ℃ of min
-1Speed be warming up to 350 ℃, kept 4 hours, naturally cool to room temperature, grind compressing tablet, be warming up to 500 ℃ with the phase same rate again, kept 18 hours.Naturally cool to room temperature with stove, take out the product porphyrize and get described doped iron phosphate lithium.
The XRD of product sees shown in Figure 1, as shown in Figure 1, utilizes this method to synthesize the LiFePO4 of olivine-type, CoS
2Coating do not change its crystal formation, and do not have other impurity peaks in the spectrogram, the product purity height.By first all cyclic voltammetry curves of Fig. 2 LiFePO4 as can be known, product only has a pair of redox peak, corresponding one group of charge and discharge platform, and two peak areas are close, illustrate that it has higher coulombic efficiency.
Take by weighing Fe (NO
3)
39H
2O 4.04g, NH
4H
2PO
41.15g, be dissolved in respectively in the 100mL deionized water, drip and mix, stirring is 5 in 60 ℃ of adding 1 mol ammoniacal liquor to pH value of solution values down, filtration washing is also dry down at 80 ℃.Gained presoma and 0.388g Li
2CO
3, mixed grinding, the porcelain crucible of packing into is 1dm at flow velocity
3Min
-199.999% argon gas stream in, with 3 ℃ of min
-1Speed be warming up to 350 ℃, kept 4 hours, naturally cool to room temperature, grind compressing tablet, be warming up to 700 ℃ with the phase same rate again, kept 18 hours.Naturally cool to room temperature with stove, take out the product porphyrize and get LiFePO4.Take by weighing 0.0607g Co (AC)
24H
2O and 0.0927g NH
2CSNH
2Be dissolved in the 20mL ethanol, add the LiFePO4 that 0.3g makes, ultrasonic wave disperseed 0.5 hour, and mixture places reactor in 180 ℃ of insulations 72 hours then, naturally cools to room temperature, washing, and 100 ℃ of vacuumizes get CoS
2The LiFePO4 that coats.
Embodiment 3
Take by weighing Fe (NO
3)
39H
2O 4.04g, NH
4H
2PO
41.15g, be dissolved in respectively in the 100mL deionized water, drip and mix, stirring is 5 in 60 ℃ of adding 1 mol ammoniacal liquor to pH value of solution values down, filtration washing is also dry down at 80 ℃.Gained presoma and 0.388g Li
2CO
3, mixed grinding, the porcelain crucible of packing into is 1dm at flow velocity
3Min
-199.999% argon gas stream in, with 3 ℃ of min
-1Speed be warming up to 350 ℃, kept 4 hours, naturally cool to room temperature, grind compressing tablet, be warming up to 700 ℃ with the phase same rate again, kept 18 hours.Naturally cool to room temperature with stove, take out the product porphyrize and get LiFePO4.Take by weighing 0.1128g SnCl
2Be dissolved in the 25mL water with 0.0435g CTAB, add the LiFePO4 that 0.3g makes, ultrasonic wave disperseed 0.5 hour, and dripped 0.398mL 6.5molL
-1KOH solution, filter, 100 ℃ of vacuumizes get the LiFePO4 that nano SnO coats.
Claims (10)
1. the LiFePO 4 material of a novel conductive agent doping/coating, it is characterized in that described LiFePO 4 material comprises: press atomic ratio Li: Fe: P=0.9-1.2: 1: 1 Li source compound, Fe source compound and phosphate radical source compound, and the quality percentage composition is the conductive agent of target product LiFePO4 1%-30%.
2. the preparation method of the LiFePO 4 material of the novel conductive agent doping/coating of a claim 1 is characterized in that described preparation methods comprises:
(1) be that the trivalent iron salt aqueous solution, the concentration of 0.2～2M is that 0.2～2M aqueous phosphatic and concentration are that 1～5M aqueous alkali mixes with concentration, stir that the pH value of control mixed solution is 3～5, control reaction temperature is 30～80 ℃;
(2) step (1) gained material is carried out Separation of Solid and Liquid, drying gets the ferric phosphate presoma;
(3) in atomic ratio Li: Fe: P=0.9-1.2: 1: 1 ratio, step (2) gained ferric phosphate presoma, Li source compound and conductive agent are mixed, grind, wherein the consumption of conductive agent is 1～30wt% of LiFePO4;
(4) with step (3) gained mixture in inert atmosphere in 300～450 ℃ the insulation 4～8 hours, grind behind the natural cooling dusty material.
(5) step (4) gained dusty material is ground, compressing tablet was handled 5～24 hours in 450～650 ℃ in inert atmosphere, grind behind the natural cooling the lithium iron phosphate positive material that mixes of conductive agent.
3. the preparation method of the LiFePO 4 material of the novel conductive agent doping/coating of a claim 1 is characterized in that described preparation methods comprises:
(1) be that the trivalent iron salt aqueous solution, the concentration of 0.2～2M is that 0.2～2M aqueous phosphatic and concentration are that 1～5M aqueous alkali mixes with concentration, stir that the pH value of control mixed solution is 3～5, control reaction temperature is 30～80 ℃;
(2) step (1) gained material is carried out Separation of Solid and Liquid, drying gets the ferric phosphate presoma;
(3) in atomic ratio Li: Fe: P=0.9-1.2: 1: 1 ratio, step (2) gained ferric phosphate presoma, Li source compound are carried out mixed grinding, the gained mixture in inert atmosphere in 300～450 ℃ the insulation 4～8 hours, grind behind the natural cooling dusty material; This dusty material grinds, and compressing tablet was handled 5～24 hours in 450～650 ℃ in inert atmosphere, grind behind the natural cooling lithium iron phosphate positive material;
(4) lithium iron phosphate positive material with step (3) gained is distributed under the ultrasonic wave condition in the conductive agent raw material of preparation, and wherein the consumption of conductive agent is 1～30wt% of LiFePO4, obtains the lithium iron phosphate positive material that conductive agent coats through Overheating Treatment.
4. according to the preparation method of the LiFePO 4 material of claim 2 or 3 described novel conductive agent doping/coatings, it is characterized in that described Li source compound is at least a in lithium carbonate, lithium nitrate, lithium acetate or the lithium hydroxide.
5. according to the preparation method of the LiFePO 4 material of claim 2 or 3 described novel conductive agent doping/coatings, it is characterized in that described Fe source compound is at least a in di-iron trioxide, ferric nitrate, ferrous oxalate or the ferric oxalate.
6. according to the preparation method of the LiFePO 4 material of claim 2 or 3 described novel conductive agent doping/coatings, it is characterized in that described phosphate radical source compound is at least a in ammonium phosphate, diammonium hydrogen phosphate or the ammonium dihydrogen phosphate.
7. according to the preparation method of the LiFePO 4 material of claim 2 or 3 described novel conductive agent doping/coatings, it is characterized in that described conductive agent is sulfide: CoS
2, FeS
2, NiS
2, ZnS
2, TeS
2Or MoS
2In one or more.
8. according to the preparation method of the LiFePO 4 material of claim 2 or 3 described novel conductive agent doping/coatings, it is characterized in that described conductive agent is oxide: SnO, ZnO, TiO
2, ZrO
2, CaO, Y
2O
3, RuO
2, SiO
2In one or more.
9. according to claim 2 or 3 described novel conductive agent doping/coated LiFePO 4 for lithium ion batteries preparation methods, it is characterized in that described inert protective atmosphere is: nitrogen or argon gas.
10. according to claim 2 or 3 described novel conductive agent doping/coated LiFePO 4 for lithium ion batteries preparation methods, it is characterized in that: the flow velocity of described protective atmosphere is 0.1～10dm
3Min
-1
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