CN102332565B - Synthesis method for lithium iron phosphate/carbon composite material - Google Patents

Synthesis method for lithium iron phosphate/carbon composite material Download PDF

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CN102332565B
CN102332565B CN201110296165.4A CN201110296165A CN102332565B CN 102332565 B CN102332565 B CN 102332565B CN 201110296165 A CN201110296165 A CN 201110296165A CN 102332565 B CN102332565 B CN 102332565B
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lithium
composite material
iron phosphate
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王连邦
施梅勤
徐土根
吴晓潭
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Zhejiang University of Technology ZJUT
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Abstract

The invention discloses a synthesis method for a lithium iron phosphate/carbon composite material. The synthesis method is characterized by comprising the following steps of: (1) uniformly mixing lithium phosphate, iron powder, iron phosphate, another lithium source and a carbonous conductive agent precursor, wherein the another lithium source is one or the combination of any of the following components: lithium carbonate, lithium oxalate, lithium acetate, lithium hydroxide and lithium nitrate, and the carbonous conductive agent precursor is one or the combination of any of the following components: glucose, sucrose, citric acid, starch, polyvinyl alcohol, stearic acid and lauric acid; (2) putting the raw material mixture obtained in the step (1) into a ball-milling container and performing full ball milling; and (3) putting the mixture subjected to the ball milling into nitrogen gas and baking the mixture at 600-800 DEG C to prepare the lithium iron phosphate/carbon composite material. The synthesis method is simple in process, and the synthesized lithium iron phosphate/carbon composite material is high in specific capacity and excellent in high-current and cycle performance.

Description

A kind of synthetic method of lithium iron phosphate/carbon composite material
Technical field:
The present invention relates to a kind of synthetic method of lithium iron phosphate/carbon composite material, this composite material can be used as anode material for lithium-ion batteries and uses.
Background technology:
Since the LiFePO4 that the people such as A.K.Padhi in 1997 report has an olivine-type structure can be used as anode material for lithium-ion batteries, due to its good chemical property, abundant raw material sources, preferably security performance, the feature such as can under hot environment, use to be subject to the favor of vast scientific research institution and commercial company.
At present, the preparation method of LiFePO4 mainly contains high temperature solid-state method, microwave process for synthesizing, sol-gel process, liquid phase deposition etc.High temperature solid-state method technique is simple, is applicable to large-scale production, but the common mixing of reactant is inhomogeneous, synthetic material particle is larger, and divalence source of iron cost is higher, easily occurs the shortcomings such as ferric iron impurity in preparation process, cause material property poor, a batch homogeneity for material can not be guaranteed; Microwave process for synthesizing is also a kind of solid phase method synthetic method, and it has the reaction time short (3-10min), and energy consumption is low, combined coefficient is high, the advantages such as uniform particles, but the method requires comparatively strict to process conditions and input cost is too high, is not suitable for carrying out large-scale production; The advantage of sol-gal process is that its precursor solution chemical uniformity is good, Gel heat-treatment temperature is low, powder granule particle diameter is little and narrowly distributing, powder sintering performance is good, course of reaction is easy to control, equipment is simple, but that gel drying shrinks is large, synthesis cycle is long, suitability for industrialized production difficulty is larger; The electrochemical performances of lithium iron phosphate that liquid phase co-electrodeposition method prepares is better, but whole process all carries out under nitrogen protection atmosphere, and complex process, is unfavorable for industrialization.
In high temperature sintering and charging and discharging lithium battery process, usually have the loss of part lithium salts, mainly comprise following three aspects: (1), in high-temperature sintering process, part lithium salts decomposes causes it with Li 2the form of O and volatilizing; (2), in the time of charging and discharging lithium battery, lithium and electrolyte react and form SEI, have consumed part lithium; (3) positive electrode shows as the increase of volume and reduces along with the deintercalation meeting of lithium is corresponding in charge and discharge process, repeatedly, after circulation, can cause part-structure generation deformation, and the lithium ion of dissolving arrives negative pole through barrier film, sticks on negative pole.Therefore, in traditional preparation process, conventionally can add excessive phosphoric acid lithium salts, to make up the impact that in said process, lithium salts loss is caused.But because lithium phosphate is a kind of non-conductor of electricity, if add excess phosphoric acid lithium can cause the LiFePO4 electron mobility of congenital conductivity deficiency lower.
Summary of the invention:
The technical problem to be solved in the present invention is to provide a kind of synthetic method of lithium iron phosphate/carbon composite material, and this synthetic method craft is simple, and the lithium iron phosphate/carbon composite material specific capacity of synthesized is high, and large electric current and cycle performance are good.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A synthetic method for lithium iron phosphate/carbon composite material, comprises the steps:
(1) lithium phosphate, iron powder, ferric phosphate, another lithium source and carbon containing conductive agent presoma are mixed; Described another one lithium source is selected from following a kind of or several combination arbitrarily: lithium carbonate, lithium oxalate, lithium acetate, lithium hydroxide, lithium nitrate, and described is selected from following a kind of or several combination arbitrarily containing carbonaceous conductive presoma: glucose, sucrose, citric acid, starch, polyvinyl alcohol, stearic acid, laurate; The molar ratio of described lithium phosphate, iron powder, ferric phosphate is 1: 1: 2.06, described another lithium source is 1.02～2 according to the mol ratio that makes lithium, iron, phosphorus, oxygen in final raw mixture: add at 1.02: 1.02: 4.08, described carbon containing conductive agent presoma is 2～25wt.% of theoretical LiFePO4 quality;
(2) step (1) gained raw mixture is placed in to ball mill container and carries out abundant ball milling;
(3) mixture after ball milling is placed in to nitrogen in 600～800 DEG C of roastings, can makes described lithium iron phosphate/carbon composite material.
The present invention's raw material used as can lithium phosphate, ferric phosphate and another kind of lithium source can contain the crystallization water, for example lithium phosphate uses Li 3pO 40.5H 2o, ferric phosphate uses FePO 44H 2o, described iron powder uses reduced iron powder in addition, can reduce costs like this.
Further, in step (1), in raw mixture, also can add compound corresponding to doped chemical, the oxide of for example doped chemical, nitrate, oxalates, carbonate, hydroxide etc., described doped chemical can be selected from following a kind of or multiple combination arbitrarily: fluorine, chlorine, bromine, iodine, sulphur, nickel, cobalt, manganese, copper, zinc, titanium, silver, magnesium, zirconium, vanadium, molybdenum, aluminium, chromium, rare earth element, preferably doped chemical is: fluorine, chlorine, nickel, cobalt, copper, silver, rare earth element.Those skilled in the art can select compound corresponding to suitable doped chemical as required from prior art.
Further, the addition of compound corresponding to described doped chemical is taking the ratio of the molal quantity of doped chemical and the molal quantity of theoretical LiFePO4 as 0～1: 1.02.
Further, in step (1), described carbon containing conductive agent presoma is preferably 3～12wt.% of theoretical LiFePO4 quality.
Further, the Ball-milling Time in step (2) is 1～20 hour, is preferably 2～10 hours.
Further, the roasting time in step (3) is 1～20 hour, is preferably 4～12 hours.
The lithium iron phosphate/carbon composite material that the present invention makes can be used as anode material for lithium-ion batteries and uses.
Compared with prior art, the method for synthesizing lithium ionic cell positive pole material lithium iron phosphate of the present invention has following outstanding feature:
(1) one or more combinations in use lithium carbonate, lithium oxalate, lithium acetate, lithium hydroxide, lithium nitrate are as the lithium source that excessive part lithium is provided, the loss of lithium salts in sintering and charge and discharge process can be compensated like this, nonconducting lithium phosphate can be effectively avoided again existing in synthetic product.
(2) positive electrode that prepared by the present invention, LiFePO4 good crystallinity, chemical property good (high, the large electric current of specific capacity and cycle performance are good), material composition and proportioning are easily controlled, good stability between batch.
(3) the present invention adopts mechanical ball milling-high temperature solid-state method synthesis technique, technique simple possible.
(4) the present invention adopts relatively inexpensive reduced iron powder and four water ferric phosphates as source of iron, with low cost.
Brief description of the drawings:
Fig. 1 presses the prepared LiFePO of embodiment 1 4the x-ray diffraction pattern of/C composite material;
Fig. 2 presses the prepared LiFePO of embodiment 1 4the stereoscan photograph of/C composite material;
Fig. 3 presses the prepared LiFePO of embodiment 1 4/ C composite material is anodal, and lithium sheet is the cycle characteristics curve chart of the lithium ion battery that assembles of negative pole.
Embodiment:
With specific embodiment, technical scheme of the present invention is described further below, but protection scope of the present invention is not limited to this:
Embodiment 1:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.2g lithium carbonate, 2.7g citric acid, mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make evengranular LiFePO 4/ C powder.
The lithium iron phosphate/carbon making has been done to X-ray diffraction, and as shown in Figure 1, prepared LiFePO4 is olivine-type rhombic system pure phase structure, does not have the peak of other impurity in spectrogram.Fig. 2 is LiFePO 4/ C powder amplifies the stereoscan photograph of 10000 times, and as seen from the figure, product particle size is about 1 micron.
By active material LiFePO 4/ C powder, acetylene black, Kynoar, with the mass ratio ratio of 8: 1: 1, take altogether 0.5g and are dissolved in the pyrrolidones of appropriate 1-methyl-2, mix rear pulp and are applied to vacuum drying on aluminium foil and make positive plate.After being beaten to sheet, the electrode slice of oven dry accurately weighs its quality, as anode.Simultaneously, taking lithium sheet as to electrode, micropore shaped polyethylene is barrier film, 1.0mol/L LiPF 6+ DMC is electrolyte, in the System One glove box that is full of argon gas, is assembled into 2032 button cells with tablet press machine.
In 2.5V～4.2V voltage range, battery is carried out to constant current charge-discharge loop test.Fig. 3 is with 1C (170mAg -1) multiplying power charging, 1C (170mAg -1) and 10C (1700mAg -1) the cycle performance of battery figure of multiplying power discharging, as shown in Figure 3, material prepared by the present invention has stable cycle performance, the advantage that specific capacity is high under large electric current.
Embodiment 2:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.17g lithium carbonate, 2.7g citric acid, mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make evengranular LiFePO 4/ C powder.
Embodiment 3:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.27g lithium carbonate, 2.7g citric acid, mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make evengranular LiFePO 4/ C powder.
Embodiment 4:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.51g lithium oxalate, 2.7g citric acid, mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make evengranular LiFePO 4/ C powder.
Embodiment 5:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.57g lithium acetate, 2.7g citric acid, mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make evengranular LiFePO 4/ C powder.
Embodiment 6:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.33g lithium hydroxide, 2.7g citric acid, mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make evengranular LiFePO 4/ C powder.
Embodiment 7:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.29g lithium nitrate, 2.7g citric acid, mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make evengranular LiFePO 4/ C powder.
Embodiment 8:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.29g lithium carbonate, 2.4g sucrose, mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make evengranular LiFePO 4/ C powder.
Embodiment 9:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.29g lithium carbonate, 1.8g stearic acid, mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make evengranular LiFePO 4/ C powder.
Embodiment 10:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.29g lithium carbonate, 3.1g starch, mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make evengranular LiFePO 4/ C powder.
Embodiment 11:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.2g lithium carbonate, 2.7g citric acid, 0.2gCo (NO 3) 2mix.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make the even LiFePO doped with cobalt element 4/ C powder.
Embodiment 12:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.2g lithium carbonate, 2.7g citric acid, 0.21gCeO 2mix.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make the even LiFePO doped with Ce elements 4/ C powder.
Embodiment 13:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.2g lithium carbonate, 2.7g citric acid, 0.22gNH 4f mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make the even LiFePO doped with fluorine element 4/ C powder.
Embodiment 14:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.2g lithium carbonate, 2.7g citric acid, 0.34g nickel phosphate mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make the even LiFePO doped with nickel element 4/ C powder.
Embodiment 15:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.2g lithium carbonate, 2.7g citric acid, 0.17gCuO mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make the even LiFePO doped with copper 4/ C powder.
Embodiment 16:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.2g lithium carbonate, 2.7g citric acid, 0.15gAgO mixes.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make the even LiFePO doped with silver element 4/ C powder.
Embodiment 17:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33gFePO 44H 2o, 0.2g lithium carbonate, 2.7g citric acid, 0.38gLa 2o 3mix.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make the even LiFePO doped with lanthanum element 4/ C powder.
Embodiment 18:
Take 3.48gLi 3pO 40.5H 2o, 1.68g reduced iron powder, 9.33fFePO 44H 2o, 0.2g lithium carbonate, 2.7g citric acid, 0.23gTiO 2mix.Put it in ball mill container ball milling 3 hours, be then placed in 750 DEG C of high-temperature roastings of nitrogen 15 hours, can make the even LiFePO doped with titanium elements 4/ C powder.
The LiFePO that above-described embodiment 2-18 makes 4/ C powder obtains lithium ion battery according to the method assembling of embodiment 1, carries out electrochemical property test according to conventional method, the results are shown in Table 1, table 2, table 3 and table 4:
Table 1
Figure BDA0000094618750000081
Table 2
Figure BDA0000094618750000082
Table 3
Figure BDA0000094618750000091
Table 4
Figure BDA0000094618750000092

Claims (9)

1. a synthetic method for lithium iron phosphate/carbon composite material, is characterized in that: described synthetic method comprises the steps:
(1) Lin Suan Li ﹑ Tie Fen ﹑ Lin Suan another lithium source of Tie ﹑ and carbon containing conductive agent presoma are mixed; Described another one lithium source is selected from following a kind of or several combination arbitrarily: carbon acid lithium ﹑ oxalic acid lithium ﹑ acetic acid lithium ﹑ lithium nitrate, and described is selected from following a kind of or several combination arbitrarily containing carbonaceous conductive presoma: the hard fat acid of the Portugal grape sugar ﹑ sugarcane sugar ﹑ lemon lemon acid poly-second alkene alcohol ﹑ of ﹑ shallow lake powder ﹑ ﹑ laurate; The molar ratio of described Lin Suan Li ﹑ Tie Fen ﹑ ferric phosphate is 1:1:2.06, described another lithium source is that 1.02～2:1.02:1.02:4.08 adds according to the mol ratio that makes final raw mixture Zhong Li ﹑ Tie ﹑ Lin ﹑ oxygen, and described carbon containing conductive agent presoma is 2～25wt.% of theoretical LiFePO4 quality;
(2) step (1) gained raw mixture is placed in to ball mill container and carries out abundant ball milling;
(3) mixture after ball milling is placed in to nitrogen in 600～800 DEG C of roastings, can makes described lithium iron phosphate/carbon composite material.
2. the synthetic method of lithium iron phosphate/carbon composite material according to claim 1, is characterized in that: described lithium phosphate uses Li 3pO 40.5H 2o, described iron powder uses reduced iron powder, and described ferric phosphate uses FePO 44H 2o.
3. the synthetic method of lithium iron phosphate/carbon composite material according to claim 1, it is characterized in that: in described raw mixture, also add compound corresponding to doped chemical, described doped chemical can be selected from following a kind of or any multiple combination: Fu ﹑ Lv ﹑ Xiu ﹑ Dian ﹑ Liu ﹑ Nie ﹑ Gu ﹑ Meng ﹑ Tong ﹑ Xin ﹑ Tai ﹑ Yin ﹑ Mei ﹑ Gao ﹑ Fan ﹑ Mu ﹑ Lv ﹑ chromium, rare earth element.
4. the synthetic method of lithium iron phosphate/carbon composite material according to claim 3, is characterized in that: the addition of compound corresponding to described doped chemical is taking the ratio of the molal quantity of doped chemical and the molal quantity of theoretical LiFePO4 as 0～1:1.02.
5. according to the synthetic method of the lithium iron phosphate/carbon composite material one of claim 1～3 Suo Shu, it is characterized in that: described carbon containing conductive agent presoma is 3～12wt.% of theoretical LiFePO4 quality.
6. according to the synthetic method of the lithium iron phosphate/carbon composite material one of claim 1～3 Suo Shu, it is characterized in that: the Ball-milling Time in step (2) is 1～20 hour.
7. the synthetic method of lithium iron phosphate/carbon composite material according to claim 6, is characterized in that: the Ball-milling Time in step (2) is 2～10 hours.
8. according to the synthetic method of the lithium iron phosphate/carbon composite material one of claim 1～3 Suo Shu, it is characterized in that: the roasting time in step (3) is 1～20 hour.
9. the synthetic method of lithium iron phosphate/carbon composite material according to claim 8, is characterized in that: the roasting time in step (3) is 4～12 hours.
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CN102916183A (en) * 2012-10-16 2013-02-06 上海锦众信息科技有限公司 Preparation method of lithium iron phosphate composite material of lithium ion battery
CN104466118B (en) * 2014-12-27 2017-03-01 桂林理工大学 The method of composite mixed combination in-situ polymerization synthesized high-performance lithium iron phosphate positive material
CN106602027A (en) * 2016-12-30 2017-04-26 深圳市沃特玛电池有限公司 Modified positive electrode material for lithium iron phosphate battery and preparation method of modified positive electrode material and lithium-ion battery
CN108054373B (en) * 2017-12-24 2020-06-26 扬州工业职业技术学院 Lithium iron phosphate/carbon composite material and application thereof in lithium battery
CN108682853B (en) * 2018-04-24 2020-09-08 江西省金锂科技股份有限公司 Preparation method of lithium iron phosphate and lithium iron phosphate cathode material prepared by same
CN109081322A (en) * 2018-11-12 2018-12-25 渤海大学 A kind of method that ihleite method extracts iron standby LiFePO4 in lateritic nickel ore
CN110620278B (en) * 2019-09-25 2021-07-02 深圳清华大学研究院 Method for recovering anode material of waste lithium iron phosphate battery
CN111261969B (en) * 2020-02-05 2021-08-17 中国科学院化学研究所 Method for recycling and regenerating lithium iron phosphate waste battery anode material
CN112573500A (en) * 2020-12-24 2021-03-30 浙江工业大学 Preparation method of vanadium-doped lithium iron phosphate-carbon composite material taking iron powder as raw material

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