CN109755518B - Preparation method of carbon-coated lithium iron phosphate material - Google Patents
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Abstract
The invention provides a preparation method of a carbon-coated lithium iron phosphate material, which comprises a pulping and dispersing step, a lithium adding step, a grinding step, a drying and granulating step and a sintering step. Adding iron oxyhydroxide, inorganic strong acid, phosphoric acid and a carbon source into a solvent to mix into slurry and disperse, reacting for 1-20 h, wherein the adding amount of the carbon source is 1-7% of the mass percent of carbon in the carbon-coated lithium iron phosphate material; the lithium addition step includes adding a lithium source to the dispersed slurry; the grinding step comprises grinding the slurry after the lithium adding step for 0.5-10 h; the drying and granulating step comprises drying and granulating the slurry by a spray drying method to obtain powder; and the sintering step comprises sintering the powder in inert gas to obtain the carbon-coated lithium iron phosphate material.
Description
Technical Field
The invention relates to the technical field of lithium ion anode materials, in particular to a preparation method of a carbon-coated lithium iron phosphate material.
Background
Lithium ion batteries are preferred power sources for portable electronic devices such as mobile phones and notebook computers because of their outstanding advantages of high operating voltage, high specific capacity, low self-discharge, good cyclicity, long service life, light weight, and small size. In recent years, with the increasing environmental problems, lithium ion batteries are attracting more and more attention in applications of low-exhaust-gas-emission vehicles such as electric vehicles and hybrid vehicles, which puts higher demands on the safety, power and life of the lithium ion batteries.
As an important component of lithium ion batteries, research on positive electrode materials has been a major research focus. As early as 1997, it was found that lithium iron phosphate having an olivine structure can be used as a positive electrode material for lithium ion batteries. Meanwhile, the lithium iron phosphate has the advantages of stable structure, abundant raw material sources, good safety, environmental friendliness, proper voltage level, higher specific capacity and the like, can be used at high temperature, and is favored by extensive scientific research institutions and commercial companies. However, lithium iron phosphate has a fatal disadvantage determined by its lattice structure, that is, extremely low electron conductivity and ion diffusion rate, rapid capacity fading during large current charge and discharge, and poor high rate performance.
At present, the preparation method of the nano lithium iron phosphate mainly comprises a high-temperature solid phase method, a template synthesis method, a hydrothermal method, a coprecipitation method, a sol-gel method and the like. Among them, the high-temperature solid phase method is the method which is most easily industrialized, and is also the mainstream method for the industrialization of lithium iron phosphate at present. The preparation process of the high-temperature solid phase method generally comprises the steps of dispersing and ball-milling iron source, lithium source and phosphorus source compounds, and then sintering at high temperature to obtain the lithium iron phosphate anode material. The iron source of the high-temperature solid phase method mainly comprises iron phosphate, iron oxide and iron oxalate, which are respectively called as an iron phosphate process, an iron oxide process and an iron oxalate process. In the water system iron oxide process using water as a solvent, the reaction process of iron oxide, a phosphorus source, a carbon source and a lithium source is complex in the sintering process, and the material structure changes greatly, so that the crystal structure is poor. Moreover, the carbon layer is difficult to coat, the carbon layer is fragile, crystal grains are easy to grow up, the resistivity is further high, and the charge and discharge performance, the rate capability and the cycle performance are poor.
Disclosure of Invention
The invention aims to provide a preparation method for preparing a carbon-coated lithium iron phosphate material with low resistivity and good charge-discharge performance, rate capability and cycle performance.
In order to solve the technical problems, the invention provides a preparation method of a carbon-coated lithium iron phosphate material, which comprises a pulping and dispersing step, a lithium adding step, a grinding step, a drying and granulating step and a sintering step. Adding iron oxyhydroxide, inorganic strong acid, phosphoric acid and a carbon source into a solvent to mix into slurry and disperse, reacting for 1-20 h, wherein the adding amount of the carbon source is 1-7% of the mass percent of carbon in the carbon-coated lithium iron phosphate material; the lithium addition step includes adding a lithium source to the dispersed slurry; the grinding step comprises grinding the slurry after the lithium adding step for 0.5-10 h; the drying and granulating step comprises drying and granulating the ground slurry by a spray drying method to obtain powder; and the sintering step comprises sintering the powder in inert gas to obtain the carbon-coated lithium iron phosphate material.
Optionally, the ratio of n (Fe): n (PO)4) (0.96-1.01): 1 in a molar ratio ofIron oxyhydroxide and phosphoric acid, the molar ratio of iron in the iron oxyhydroxide to lithium in the lithium source being n (fe): n (Li) ═ 0.96 to 1.02): (0.98-1.04) the molar ratio of ionizable hydrogen ions in the strong inorganic acid to iron in the iron oxyhydroxide is n (H)+): n (Fe) ═ 0.1 to 0.5: 1, the solid content of the slurry is 20-50%.
Optionally, before the drying and granulating step, a stabilizing additive is added into the slurry to improve the stability of the slurry, wherein the addition amount of the stabilizing additive is 0.1-2% of the total mass of the slurry, and the stabilizing additive is a water-soluble copolymer.
Optionally, the stabilizing auxiliary comprises one or more of a polyalkene water-soluble copolymer, a polyalkene acid water-soluble polymer and an olefine acid copolymer water-soluble polymer.
Optionally, the strong inorganic acid is one or more of hydrochloric acid, nitric acid, sulfuric acid, hydrobromic acid, hydroiodic acid, and chloric acid.
Optionally, the carbon source includes one or more of an organic carbon source and an inorganic carbon source, the organic carbon source is one or more of glucose, sucrose, starch, cyclodextrin and polyethylene glycol, and the inorganic carbon source is one or more of superconducting carbon black (Super P), Ketjen black and acetylene black.
Optionally, the lithium source is one or both of lithium carbonate and lithium hydroxide.
Optionally, spray drying is performed in the drying and granulating step by using a spray dryer, wherein the spray dryer is any one or more of a pressure jet spray dryer, a rotary centrifugal spray dryer and a two-phase flow spray dryer.
Optionally, the temperature range at the inlet of the drying and granulating step is 200-300 ℃, and the temperature range at the outlet of the drying and granulating step is 60-150 ℃.
Optionally, the sintering mode in the sintering step is any one of one-stage sintering, two-stage sintering and three-stage sintering; the heat preservation temperature of the one-stage sintering is 600-750 ℃, and the heat preservation time is 1-10 hours; the two-stage sintering comprises a first stage sintering and a second stage sintering, wherein the heat preservation temperature of the first stage sintering is 300-500 ℃, the heat preservation time is 1-5 hours, the heat preservation temperature of the second stage sintering is 600-750 ℃, and the heat preservation time is 1-10 hours; the three-stage sintering comprises a first stage sintering, a second stage sintering and a third stage sintering, wherein the heat preservation temperature of the first stage sintering is 200-300 ℃, the heat preservation time is 1-5 hours, the heat preservation temperature of the second stage sintering is 450-550 ℃, the heat preservation time is 1-3 hours, the heat preservation temperature of the third stage sintering is 650-750 ℃, and the heat preservation time is 1-5 hours.
As a further preferable embodiment or characteristic, the strong inorganic acid is preferably one or more of nitric acid, hydrochloric acid, and sulfuric acid.
As a further preferred technical scheme or characteristic, the reaction time of the pulping and dispersing step is preferably 1h-5 h.
As a further preferred solution or feature, the time of the grinding step is preferably 1h to 6 h.
As a further preferred solution or feature, the spray dryer is preferably a rotary centrifugal spray dryer or a two-phase flow spray dryer.
As a further preferred technical solution or characteristic, the temperature range at the inlet of the spray drying step is from 230 ℃ to 280 ℃ and the temperature range at the outlet of the spray drying step is from 80 ℃ to 130 ℃.
As a further preferred technical solution or feature, the sintering manner in the sintering step is preferably two-stage sintering, and more preferably, the temperature of the first-stage sintering is 350 ℃ to 500 ℃, the holding time is 2 hours to 5 hours, the temperature of the second-stage sintering is 675 ℃ to 725 ℃, and the holding time is 1 hour to 5 hours, and the water-soluble copolymer is preferably polyvinyl alcohol.
In summary, in the preparation method of the carbon-coated lithium iron phosphate material of the present invention, iron oxyhydroxide is used as an iron source, phosphoric acid is used as a phosphorus source, and inorganic strong acid is added to increase the mutual reaction of the iron oxyhydroxide. In the liquid phase mixing process, the iron oxyhydroxide and the phosphoric acid are reacted to generate a certain precursor, and the side reaction effect of the drying material in the sintering process is reduced, so that the conductivity, the charge and discharge performance, the rate performance and the like of the product are improved. In addition, the strong inorganic acid provides an acidic environment which can help the carbon coating process, and the coated carbon is not easy to break.
And secondly, the stabilizing auxiliary agent and the precursor have a synergistic effect, so that the stability is further improved, and the occurrence of side effects is reduced.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The ranges mentioned in the present invention are inclusive. Fe and PO mentioned in the invention4And H+Respectively, an iron atom, a phosphate ion and a hydrogen ion, and n denotes the amount of the substance. Although the solvent in the embodiment of the present invention is deionized water, the present invention is not limited to the kind of the solvent, and the solvent may be tap water, industrial water, or other organic solvents.
Example 1
(1) Iron oxyhydroxide and phosphoric acid are mixed according to a molar ratio n (Fe): n (PO)4) 0.98: 1 and the molar ratio of hydrogen ions to iron in the iron oxyhydroxide is n (H)+): n (fe) ═ 0.15: 1, and glucose calculated according to the theoretical carbon content of 3 percent are added into deionized water to be mixed into slurry with the solid content of 30 percent, and the slurry is dispersed and reacted for 120 min.
(2) Adding n (li): n (fe) ═ 1.01: 1, and continuously dispersing for 30 min.
(3) Adding the slurry obtained in the step (2) into a sand mill for grinding for 60 min.
(4) And (4) passing the slurry obtained in the step (3) through a two-phase flow type spray dryer, and drying and granulating at the inlet of 235 ℃ and the outlet of 90 ℃.
(5) And (4) sintering the powder obtained in the step (4) under the protection of nitrogen according to a system of keeping the temperature at 350 ℃ for 3 hours and keeping the temperature at 680 ℃ for 3 hours to obtain a carbon-coated lithium iron phosphate material product with the average discharge capacity of 0.1C being 154mAh/g and the average discharge capacity of 1C being 138 mAh/g.
Example 2
1) Iron oxyhydroxide and phosphoric acid are mixed according to a molar ratio n (Fe): n (PO)4) 0.96: 1 and the molar ratio of hydrogen ions to iron in the iron oxyhydroxide is n (H)+): n (fe) ═ 0.3: 1, adding the nitric acid and the cyclodextrin with the theoretical carbon content of 2 percent into deionized water, mixing to form slurry with the solid content of 25 percent, and dispersing and reacting for 60 min.
2) Adding n (li): n (fe) ═ 1.01: 1, and continuously dispersing for 30 min.
(3) Adding the slurry obtained in the step (2) into a ball mill for grinding for 90 min.
(4) And (4) drying and granulating the slurry obtained in the step (3) by a rotary centrifugal spray dryer at the inlet of 255 ℃ and the outlet of 100 ℃.
(5) And (4) sintering the powder obtained in the step (4) under the protection of nitrogen according to a system of preserving heat at 410 ℃ for 2.5 hours and preserving heat at 690 ℃ for 3 hours to obtain a carbon-coated lithium iron phosphate material product with the average discharge capacity of 0.1C of 151mAh/g and the average discharge capacity of 1C of 132 mAh/g.
Example 3
(1) Iron oxyhydroxide and phosphoric acid are mixed according to a molar ratio n (Fe): n (PO)4) 0.98: 1 and the molar ratio of hydrogen ions to iron in the iron oxyhydroxide is n (H)+): n (fe) ═ 0.35: 1, and starch with the theoretical carbon content of 5 percent are added into deionized water to be mixed into slurry with the solid content of 20 percent, and the slurry is dispersed and reacted for 90 min.
(2) Adding n (li): n (fe) ═ 1.01: 1, and continuously dispersing for 30 min.
(3) And (3) adding the slurry obtained in the step (2) into a sand mill for grinding for 90 min.
(4) And (4) drying and granulating the slurry obtained in the step (3) by a rotary centrifugal spray dryer at the inlet of 265 ℃ and the outlet of 105 ℃.
(5) And (4) sintering the powder obtained in the step (4) under the protection of nitrogen according to a system of keeping the temperature at 500 ℃ for 2 hours and keeping the temperature at 675 ℃ for 4 hours to obtain a carbon-coated lithium iron phosphate material product with the average discharge capacity of 0.1C of 149mAh/g and the average discharge capacity of 1C of 129 mAh/g.
Example 4
Based on example 1, PVA is added into the slurry in the following specific process:
(1) iron oxyhydroxide and phosphoric acid are mixed according to a molar ratio n (Fe): n (PO)4) 0.98: 1 and the molar ratio of hydrogen ions to iron in the iron oxyhydroxide is n (H)+): n (fe) ═ 0.15: 1, and glucose calculated according to the theoretical carbon content of 3 percent are added into deionized water to be mixed into slurry with the solid content of 30 percent, PVA which is 0.5 percent of the mass of the slurry is added into the slurry, and the dispersion and the reaction are carried out for 120 min.
(2) Adding n (li): n (fe) ═ 1.01: 1, and continuously dispersing for 30 min.
(3) Adding the slurry obtained in the step (2) into a sand mill for grinding for 60 min.
(4) And (4) passing the slurry obtained in the step (3) through a two-phase flow type spray dryer, and drying and granulating at the inlet of 235 ℃ and the outlet of 90 ℃.
(5) And (4) sintering the powder obtained in the step (4) under the protection of nitrogen according to a system of keeping the temperature at 350 ℃ for 3 hours and keeping the temperature at 680 ℃ for 3 hours to obtain a carbon-coated lithium iron phosphate material product with the average discharge capacity of 0.1C of 158mAh/g and the average discharge capacity of 1C of 142 mAh/g.
Comparative example 1
(1) Iron oxyhydroxide and phosphoric acid are mixed according to a molar ratio n (Fe): n (PO)4) 0.98: 1 and glucose calculated according to the theoretical carbon content of 3 percent are added into deionized water to be mixed into slurry with the solid content of 30 percent, and the slurry is dispersed and reacted for 120 min.
(2) Adding n (li): n (fe) ═ 1.01: 1, and continuously dispersing for 30 min.
(3) Adding the slurry obtained in the step (2) into a sand mill for grinding for 60 min.
(4) And (4) passing the slurry obtained in the step (3) through a two-phase flow type spray dryer, and drying and granulating at the inlet of 235 ℃ and the outlet of 90 ℃.
(5) And (4) sintering the powder obtained in the step (4) under the protection of nitrogen according to a system of keeping the temperature at 350 ℃ for 3 hours and keeping the temperature at 680 ℃ for 3 hours to obtain a carbon-coated lithium iron phosphate material product with the average discharge capacity of 0.1C being 144mAh/g and the average discharge capacity of 1C being 113 mAh/g.
Comparative example 2
(1) Iron oxyhydroxide and phosphoric acid are mixed according to a molar ratio n (Fe): n (PO)4) 0.96: 1 and cyclodextrin calculated according to the theoretical carbon content of 2 percent are added into deionized water to be mixed into slurry with the solid content of 25 percent, and the slurry is dispersed and reacted for 60 min.
(2) Adding n (li): n (fe) ═ 1.01: 1, and continuously dispersing for 30 min.
(3) Adding the slurry obtained in the step (2) into a ball mill for grinding for 90 min.
(4) And (4) drying and granulating the slurry obtained in the step (3) by a rotary centrifugal spray dryer at the inlet of 255 ℃ and the outlet of 100 ℃.
(5) And (4) sintering the powder obtained in the step (4) under the protection of nitrogen according to a system of preserving heat for 2.5 hours at 410 ℃ and preserving heat for 3 hours at 690 ℃ to obtain a carbon-coated lithium iron phosphate material product with the average discharge capacity of 0.1C of 139mAh/g and the average discharge capacity of 1C of 106 mAh/g.
Comparative example 3
(1) Iron oxyhydroxide and phosphoric acid are mixed according to a molar ratio n (Fe): n (PO)4) 0.98: 1 and starch calculated according to the theoretical carbon content of 5 percent are added into deionized water, mixed into slurry with the solid content of 20 percent, dispersed and reacted for 90 min.
(2) Adding n (li): n (fe) ═ 1.01: 1, and continuously dispersing for 30 min.
(3) And (3) adding the slurry obtained in the step (2) into a sand mill for grinding for 90 min.
(4) And (4) drying and granulating the slurry obtained in the step (3) by a rotary centrifugal spray dryer at the inlet of 265 ℃ and the outlet of 105 ℃.
(5) And (4) sintering the powder obtained in the step (4) under the protection of nitrogen according to a system of keeping the temperature at 500 ℃ for 2 hours and keeping the temperature at 675 ℃ for 4 hours to obtain a carbon-coated lithium iron phosphate material product with the average discharge capacity of 0.1C of 141mAh/g and the average discharge capacity of 1C of 102 mAh/g.
Electrochemical performance tests were performed on the carbon-coated lithium iron phosphate material products prepared in the above examples 1 to 4 and comparative examples 1 to 3, and the results are shown in table 1 below.
TABLE 1 results of electrochemical Performance test of examples 1-4 and comparative examples 1-3
From the data, it can be seen that when no strong inorganic acid is added, the 1C average discharge capacity and the 5C average discharge capacity of the carbon-coated lithium iron phosphate material product are both very low, and the electrochemical performance is obviously not satisfactory. With the increasing concentration of the ionizable hydrogen ions, the 1C average discharge capacity and the 5C average discharge capacity are also increased, and the electrochemical performance is better and better. And the electrochemical performance is further remarkably improved by adding the stabilizing additive.
The preparation method of the carbon-coated lithium iron phosphate material takes the hydroxyl ferric oxide as an iron source and the phosphoric acid as a phosphorus source, and utilizes the addition of inorganic strong acid to increase the mutual reaction of the hydroxyl ferric oxide. In the liquid phase mixing process, the iron oxyhydroxide and the phosphoric acid are reacted to generate a certain precursor, and the side reaction effect of the drying material in the sintering process is reduced, so that the conductivity, the charge and discharge performance, the rate performance and the like of the product are improved. In addition, the strong inorganic acid provides an acidic environment which can help the carbon coating process, and the coated carbon is not easy to break.
And secondly, the stabilizing auxiliary agent and the precursor have a synergistic effect, so that the stability is further improved, and the occurrence of side effects is reduced. The preparation method of the carbon-coated lithium iron phosphate material has the advantages of simple preparation process, easy realization, high preparation efficiency and high adaptability of industrial production.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (11)
1. A preparation method of a carbon-coated lithium iron phosphate material is characterized by comprising the following steps:
pulping and dispersing: adding iron oxyhydroxide, inorganic strong acid, phosphoric acid and a carbon source into a solvent to mix into slurry and disperse, and reacting for 1-20 h, wherein the adding amount of the carbon source is calculated by the mass percent of carbon in the carbon-coated lithium iron phosphate material being 1-7%;
a lithium adding step: adding a lithium source to the dispersed slurry;
grinding: grinding the slurry after the step of adding lithium for 0.5-10 h;
drying and granulating: drying and granulating the ground slurry by a spray drying method to obtain powder; and
sintering: and sintering the powder in inert gas to obtain the carbon-coated lithium iron phosphate material.
2. The method for producing a carbon-coated lithium iron phosphate material according to claim 1, wherein the ratio of n (fe): n (PO)4) = 0.96-1.01: 1, the molar ratio of iron in the iron oxyhydroxide to lithium in the lithium source being n (fe): n (Li) = (0.96-1.02): (0.98-1.04) the mole ratio of the ionizable hydrogen ions in the inorganic strong acid to the iron in the iron oxyhydroxide is n (H)+): n (Fe) = (0.1 to 0.5): 1, the solid content of the slurry is 20-50%.
3. The method for preparing a carbon-coated lithium iron phosphate material according to claim 1, wherein a stabilizing additive is added to the slurry to improve the stability of the slurry before the drying and granulating step, the amount of the stabilizing additive is 0.1 to 2% of the total mass of the slurry, and the stabilizing additive is a water-soluble copolymer.
4. The method for preparing a carbon-coated lithium iron phosphate material according to claim 3, wherein the stabilizing additive comprises one or more of a polyalkenyl alcohol water-soluble copolymer, a polyalkenyl acid water-soluble polymer, and an olefinic acid copolymer water-soluble polymer.
5. The method of claim 1, wherein the strong inorganic acid is one or more of hydrochloric acid, nitric acid, sulfuric acid, hydrobromic acid, hydroiodic acid, and chloric acid.
6. The method of claim 1, wherein the carbon source comprises one or more of an organic carbon source and an inorganic carbon source, the organic carbon source comprises one or more of glucose, sucrose, starch, cyclodextrin and polyethylene glycol, and the inorganic carbon source comprises one or more of superconducting carbon black, ketjen black and acetylene black.
7. The method of preparing a carbon-coated lithium iron phosphate material according to claim 1, wherein the lithium source is one or both of lithium carbonate and lithium hydroxide.
8. The method for preparing a carbon-coated lithium iron phosphate material according to claim 1, wherein the drying and granulating step is performed by spray drying using a spray dryer, and the spray dryer is one or more of a pressure jet spray dryer, a rotary centrifugal spray dryer, and a two-phase flow spray dryer.
9. The method for preparing a carbon-coated lithium iron phosphate material according to claim 8, wherein the temperature at the inlet of the drying and granulating step is in the range of 200 ℃ to 300 ℃, and the temperature at the outlet of the drying and granulating step is in the range of 60 ℃ to 150 ℃.
10. The method for preparing a carbon-coated lithium iron phosphate material according to claim 1, wherein the sintering in the sintering step is any one of a one-stage sintering, a two-stage sintering, and a three-stage sintering; the heat preservation temperature of the one-stage sintering is 600-750 ℃, and the heat preservation time is 1-10 hours; the two-stage sintering comprises a first stage sintering and a second stage sintering, wherein the heat preservation temperature of the first stage sintering is 300-500 ℃, the heat preservation time is 1-5 hours, the heat preservation temperature of the second stage sintering is 600-750 ℃, and the heat preservation time is 1-10 hours; the three-stage sintering comprises a first stage sintering, a second stage sintering and a third stage sintering, wherein the heat preservation temperature of the first stage sintering is 200-300 ℃, the heat preservation time is 1-5 hours, the heat preservation temperature of the second stage sintering is 450-550 ℃, the heat preservation time is 1-3 hours, the heat preservation temperature of the third stage sintering is 650-750 ℃, and the heat preservation time is 1-5 hours.
11. The method for preparing a carbon-coated lithium iron phosphate material according to claim 3, wherein the water-soluble copolymer is polyvinyl alcohol.
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