CN105206812A - Method for preparing carbon-coated lithium iron phosphate through one-step hydrothermal method - Google Patents
Method for preparing carbon-coated lithium iron phosphate through one-step hydrothermal method Download PDFInfo
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- CN105206812A CN105206812A CN201510612799.4A CN201510612799A CN105206812A CN 105206812 A CN105206812 A CN 105206812A CN 201510612799 A CN201510612799 A CN 201510612799A CN 105206812 A CN105206812 A CN 105206812A
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- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Abstract
The invention discloses a method for preparing carbon-coated lithium iron phosphate through a one-step hydrothermal method, and belongs to the field of lithium ion secondary battery anode materials. The preparation method solves the problems that a traditional carbon coating process is complex, a carbon-coating layer is not uniform, production cost is high, and electrochemical properties of products are not stable. The method is characterized in that carbon coating is completed in the hydrothermal synthesizing process, a lithium hydroxide starch paste mixture reacts with phosphoric acid to generate lithium phosphate suspension, the generated lithium phosphate suspension is mixed with a ferrite solution and reacts with the ferrite solution in a high-temperature reaction still in the inert atmosphere, the reaction temperature and time are controlled, and filtering, washing, drying and screening are conducted after the reaction ends so that carbon-coated lithium iron phosphate can be obtained. Compared with the prior art, the method has the advantages of being simple in process, low in cost, uniform in carbon-coated lithium iron phosphate granularity distribution, uniform in carbon-coating layer thickness and good in electrochemical performance.
Description
Technical field
The present invention relates to a kind of lithium ion secondary battery anode material field, particularly a kind of preparation method of LiFePO4.
Background technology
Ferric phosphate lithium cell has the advantages such as nontoxic, pollution-free, security performance is good, raw material sources is extensive, low price, and the life-span is long, is the optimal positive electrode of latest generation power lithium-ion battery.But the distinct disadvantage such as LiFePO 4 material exists electronics and ionic conductance is low, limits the commercialized development of this material to a certain extent.
In order to improve electronic conductivity, the lithium ion diffusion coefficient of LiFePO4, wherein a kind of method reduces particle size, reduces the evolving path of Li ion in granule interior.But because existing LiFePO4 production technology mostly is high temperature solid-state method, be difficult to prepare nano level LiFePO4.And hydro thermal method prepares the effective way of nano-scale lithium iron phosphate, and hydro thermal method prepare LiFePO4 have simple to operate, thing mutually evenly, the advantage of homogeneous, the good crystallinity of particle size, improve the discharge performance of material.
Although hydro thermal method can obtain the good LiFePO4 of crystallinity, owing to not having carbon coated, affect the electrical property of material.And at present, adopt existing hydro thermal method to prepare carbon cladded type LiFePO4, could must be prepared by two steps or multi-step process.General processing step is roughly as patent " hydrothermal synthesis method of the lithium ion battery anode material lithium iron phosphate of one-dimensional nano structure " (application number: 201010031395.3): the first step, add lithium hydroxide solution and phosphoric acid respectively, source of iron solution is at the uniform velocity added again with certain speed, the proportioning wherein adding material is mol ratio Li: Fe: P=3.0: 1.0: 1.0 ~ 1.15, stir after 10 ~ 30 minutes, add pH value regulator, the initial pH value of reaction system is made to be 6.5 ~ 8.0, then, in 140 ~ 180 DEG C of reactions 60 ~ 480 minutes; Product filters, wash and drying obtains carbon-free type LiFePO4; Second step, first step product, after mixing by a certain percentage with glucose, 700 DEG C, prepares carbon-coated LiFePO 4 for lithium ion batteries under nitrogen protection condition.
Although above-mentioned technique obtains carbon clad type LiFePO4, but still there is following technical problem: 1. in prior art the high temperature sintering Main Function of second step just to carry out carbon coated, this increases production cost, reduce production efficiency, be unfavorable for that hydro thermal method prepares the popularization of the technique of carbon cladded type LiFePO4; 2. carbon coated in carbon-free LiFePO4 and carbon source ball milling mixed process, can cause the destruction of LiFePO4 surface texture, affect the electrical property of material, carbon source also cannot be coated on the surface of particle uniformly, also can affect the electrical property of material; 3. in the process preparing LiFePO4, need the size controlling to generate lithium iron phosphate particles, usually adopt on the electrical property improving LiFePO 4 material in existing method and regulate reaction temperature and add the size that surfactant controls lithium iron phosphate particles; Like this, not only increase technological process, and increase operation easier.
Summary of the invention
Technical assignment of the present invention is for above the deficiencies in the prior art, provides a kind of step is simple, production cost is low one step hydro thermal method to prepare the method for carbon cladded type LiFePO4.
The technical scheme that the present invention solves its technical problem is: a kind of one-step method prepares the method for carbon cladded type LiFePO4, comprises the following steps:
(1) add starch by the LiOH solution of 1 ~ 1.5mol/L, be stirred to gelatinization, starch addition is every mole of LiOH addition is 32.26 ~ 36.36g;
(2) mixed liquor to step (1) gained adds phosphoric acid solution, and phosphoric acid and LiOH react, and generates Li
3pO
4suspension-turbid liquid, by Li
3pO
4suspension-turbid liquid joins in reactor, sealed reactor, and use inert gas to purge reactor by intake valve, discharge inner air, wherein the mol ratio of Li and P is 3.0 ~ 3.3:1;
(3) according to P:Fe=1:1, by inlet valve to Li
3pO
4divalent iron salt solution is added in suspension-turbid liquid; Reactor is warming up to 200 ~ 240 DEG C, insulation 6 ~ 10h, after cooling, washs sediment, dry, and broken, screening can arrive carbon cladded type LiFePO4 product.
The starch described in method that described one step hydro thermal method prepares carbon cladded type LiFePO4 is one or more in soluble starch, water soluble starch, pre-gelatinized starch; Divalent iron salt is one or more in ferrous sulfate, ferrous oxalate, ferrous nitrate, frerrous chloride; High purity inert gas is the one in nitrogen, argon gas.
Compared with prior art, the present invention has following outstanding beneficial effect:
1, use One-step production carbon-coated LiFePO 4 for lithium ion batteries of the present invention, by coated for carbon process conformity in the generative process of LiFePO4, instead of after the generative process of LiFePO4, simplify technological process, save time and cost;
2, after can obtaining the good LiFePO4 of crystallinity, without the need to increasing carbon under high energy ball milling again, coated to carry out carbon to LiFePO4 coated, improves production efficiency;
3, first LiOH and starch mixed solution are carried out gelatinization process, increase solution viscosity, then add phosphoric acid, LiOH wrap up by gelatinization solution environmental, LiOH and phosphatase reaction slow down, and inhibit generation Li
3pO
4particle size and agglomeration, improve the dispersiveness of end product, reduce end product particle size, improve the electrical property of material.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of embodiment 1.
Fig. 2 is the transmission electron microscope picture of embodiment 1.
Fig. 3 is the scanning electron microscope (SEM) photograph of embodiment 2.
Fig. 4 is the scanning electron microscope (SEM) photograph of embodiment 3.
Fig. 5 is the particle size distribution figure of embodiment 1.
Fig. 6 is the particle size distribution figure of embodiment 2.
Fig. 7 is the particle size distribution figure of embodiment 3.
Fig. 8 is chemical property figure under the 0.2C multiplying power of embodiment 1.
Fig. 9 is chemical property figure under the 1C multiplying power of embodiment 1.
Figure 10 is chemical property figure under the 0.2C multiplying power of embodiment 2.
Figure 11 is chemical property figure under the 1C multiplying power of embodiment 2.
Figure 12 is chemical property figure under the 0.2C multiplying power of embodiment 3.
Figure 13 is chemical property figure under the 1C multiplying power of embodiment 3.
Embodiment
Below in conjunction with specification drawings and specific embodiments, the present invention is further described.
Comparative example:
(1) first take 3.0 moles of LiOH and be dissolved in the solution that deionized water forms 1.0mol/L, then add 1.0 mole of phosphoric acid, stir and generate Li
3pO
4suspension-turbid liquid;
(2) by Li
3pO
4suspension-turbid liquid joins in reactor, sealed reactor, uses high pure nitrogen to purge reactor by intake valve, discharges inner air.Take 1.0 mol sulfuric acid more ferrous, add in the deionized water of 0.5L, stirring and dissolving, by inlet valve to Li
3pO
4feSO is added in suspension-turbid liquid
4solution.The proportioning wherein adding material is mol ratio Li:Fe:P=3.0:1.0:1.0, reactor is warming up to 200 DEG C, insulation 6h, after Temperature fall, and washing, dry, obtain initial product.
(3) add in ball mill by initial product and 10g glucose again, add in 200ml absolute ethyl alcohol, ball milling 1h, after drying, under nitrogen protection condition, 700 DEG C of insulation 6h, namely obtain carbon covering property LiFePO4.
Embodiment 1:
(1) LiOH first weighing 3.0 moles dissolves the solution being made into 1.2mol/L in deionized water, after being heated to 60 DEG C, adds 100g soluble starch, is stirred to complete gelatinization;
(2) again in step 1 gained mixed serum in add the phosphoric acid of mol ratio Li:P=3.0:1.0, i.e. 1 mole of phosphoric acid, be incubated at 80 DEG C, Keep agitation, obtains Li
3pO
4suspension-turbid liquid; Gelatinization is there is because soluble starch joins in the LiOH solution of heat, gelatinization reaction is there is because soluble starch joins in LiOH solution, intragranular starch molecule stretches diffusion to all directions, outside stripping granule, to expand between the starch molecule that comes can connection mutually, be wound around, forms one and netted contains hydrocolloid.When starch enters the particle disintegration stage of gelatinization reaction, solution viscosity is maximum, enables starch molecule be coated on around LiOH, inhibits LiOH and phosphatase reaction speed, and inhibits the Li that the two generates
3pO
4particle size and agglomeration, improve the dispersiveness of end product, reduce end product particle size.Then by the Li of step 2 gained
3pO
4suspension-turbid liquid joins in reactor, sealed reactor, uses high pure nitrogen or argon gas to purge reactor by intake valve, discharges inner air;
(3) take the ferrous sulfate of Fe:P=1.0:1.0 again, namely 1 mol sulfuric acid is ferrous, adds in 0.5L deionized water, stirring and dissolving, by the Li of inlet valve gained in step 2
3pO
4feSO is added in suspension-turbid liquid
4solution.Reactor is warming up to 200 DEG C, insulation 8h, after Temperature fall, washs sediment, dry, and broken, screening can arrive carbon cladded type LiFePO4 product; Starch solution step in pyroprocess of gelatinization completes carbon-coated LiFePO 4 for lithium ion batteries, by the coated process conformity of carbon in the generative process of LiFePO4, instead of after the generative process of LiFePO4, simplifies technological process, saves time and cost.
In described one-step technology, the proportioning adding material is mol ratio Li:Fe:P=3.0:1.0:1.0.Because viscosity after the gelatinization of the soluble starch aqueous solution is large, inhibit the Li that LiOH and phosphoric acid generate
3pO
4particle size and agglomeration, so, make Li
3pO
4with FeSO
4the LiFePO that reaction generates
4granularity less.And the starch solution of gelatinization in the generative process of LiFePO4, complete carbon coated, more energy-conservation.
The ferrous sulfate of processing step (3) also can be other ferrous solution, as ferrous nitrate, ferrous oxalate etc.
Embodiment 2:
(1) LiOH first weighing 3.3 moles is dissolved in ionized water the solution being made into 1.5mol/L, adds 120g water soluble starch under normal temperature, is stirred to dissolve completely to form mixed liquor;
(2) again in step 1 gained mixed liquor in add the phosphoric acid of mol ratio Li:P=3.3:1.0, i.e. 1 mole of phosphoric acid, Keep agitation generates Li
3pO
4suspension-turbid liquid; By Li
3pO
4suspension-turbid liquid joins in reactor, sealed reactor, uses high-purity argon gas to purge reactor by intake valve, discharges inner air;
(3) take the ferrous sulfate of Fe:P=1.0:1.0 again, namely 1 mol sulfuric acid is ferrous, adds in the deionized water of 0.5L, stirring and dissolving, by inlet valve to Li
3pO
4feSO is added in suspension-turbid liquid
4solution.The proportioning wherein adding material is mol ratio Li:Fe:P=3.1:1.0:1.0, reactor is warming up to 240 DEG C, and insulation 10h, after Temperature fall, washs sediment, dry, and broken, screening can arrive carbon cladded type LiFePO4 product.
In the present embodiment, use the water soluble starch that can be dissolved in cold water, described normal temperature refers between 15 DEG C to 25 DEG C, is advisable with 25 DEG C.In order to increase gelatinization effect better, the amount of LiOH is larger.
Embodiment 3:
(1) LiOH first weighing 3.1 moles dissolves the solution being made into 1.0mol/L in deionized water, adds 100g pre-gelatinized starch at 40 DEG C, is stirred to dissolve completely to form gelatinized corn starch;
(2) again in step 1 gained mixed liquor in add the phosphoric acid of mol ratio Li:P=3.1:1.0, i.e. 1 mole of phosphoric acid, stir at 40 DEG C and generate Li
3pO
4suspension-turbid liquid; Li
3pO
4suspension-turbid liquid is ultrasonic mixing under 200Hz frequency, and the ultrasonic air bubble be present in mixed liquor that makes shakes under sound wave effect, when reaching certain limit, growth occurs and cavitation is played in collapse, utilizes ultrasonic cavitation effect, makes Li
3pO
4mix and control Li with starch molecule in solution
3pO
4particle size, to be evenly distributed.By the Li after ultrasonic mixing
3pO
4suspension-turbid liquid joins in reactor, sealed reactor, uses high-purity argon gas to purge reactor by intake valve, discharges inner air;
(3) take the ferrous sulfate of Fe:P=1.0:1.0 again, namely 1 mol sulfuric acid is ferrous, adds in the deionized water of 0.5L, stirring and dissolving, by inlet valve to Li
3pO
4feSO is added in suspension-turbid liquid
4solution.The proportioning wherein adding material is mol ratio Li:Fe:P=3.3:1.0:1.0, reactor is warming up to 210 DEG C, and insulation 6h, after Temperature fall, washs sediment, dry, and broken, screening can arrive carbon cladded type LiFePO4 product.
The electrochemical property test of comparative example, embodiment 1, embodiment 2, embodiment 3 product the results are shown in Table 1.
As can be seen from the data of table 1, compare with employing two-step method comparative example, the product that embodiment 1, embodiment 2, embodiment 3 generate shows splendid chemical property.
The chemical property analysis result of table 1 product:
Fig. 1,2 is the scanning electron microscope (SEM) photograph that the scanning electron microscope (SEM) photograph of embodiment 1 and transmission electron microscope picture, Fig. 3,4 are respectively embodiment 2,3, this shows, the carbon-coated lithium iron phosphate composite uniform particles prepared by this inventive method, pattern is homogeneous, particle surface carbon Jacket thickness is even, covered effect is good, and the carbon-coated lithium iron phosphate composite grain graininess that wherein embodiment 3 is obtained is minimum.
Fig. 4 ~ 6 are the grain size distribution of embodiment 1,2,3, and as seen from the figure, the carbon-coated lithium iron phosphate composite particle size distribution obtained by this inventive method concentrates on 1 ~ 10um, uniform particles.
Fig. 8 ~ 13 are the chemical property figure of embodiment 1,2,3, as seen from the figure, under 0.2C multiplying power and 1C multiplying power, all can obtain good specific discharge capacity.
It should be noted that; particular of the present invention is to invention has been detailed description; for a person skilled in the art, the various apparent change carried out it when not deviating from the spirit and scope of the present invention is all within protection scope of the present invention.
Claims (4)
1. one step hydro thermal method prepares a method for carbon cladded type LiFePO4, it is characterized in that: its preparation method comprises following processing step:
(1) add starch by LiOH solution, be stirred to gelatinization;
(2) mixed liquor to step (1) gained adds phosphoric acid solution, and phosphoric acid and LiOH react, and generates Li
3pO
4suspension-turbid liquid, by Li
3pO
4suspension-turbid liquid joins in reactor, sealed reactor, and use inert gas to purge reactor by intake valve, discharge inner air, wherein the mol ratio of Li and P is 3.0 ~ 3.3:1;
(3) according to P:Fe=1:1, by inlet valve to Li
3pO
4divalent iron salt solution is added in suspension-turbid liquid; Reactor is warming up to 200 ~ 240 DEG C, insulation 6 ~ 10h, after cooling, washs sediment, dry, and broken, screening can arrive carbon cladded type LiFePO4 product.
2. one step hydro thermal method according to claim 1 prepares the method for carbon cladded type LiFePO4, it is characterized in that: the LiOH solution concentration in described step (1) is 1 ~ 1.5mol/L.
3. one step hydro thermal method according to claim 1 prepares the method for carbon cladded type LiFePO4, it is characterized in that: the starch addition in described step (1) is every mole of LiOH addition is 32.26 ~ 36.36g.
4. one step hydro thermal method according to claim 1 prepares the method for carbon cladded type LiFePO4, it is characterized in that: described divalent iron salt is the one in ferrous sulfate, ferrous nitrate or ferrous oxalate.
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|---|---|---|---|
| CN201710631188.3A CN107317018B (en) | 2015-09-24 | 2015-09-24 | Method for preparing microparticle carbon-coated lithium iron phosphate by one-step hydrothermal method |
| CN201510612799.4A CN105206812B (en) | 2015-09-24 | 2015-09-24 | The method that one step hydro thermal method prepares carbon coating type LiFePO4 |
| CN201710630504.5A CN107293728B (en) | 2015-09-24 | 2015-09-24 | Method for preparing carbon-coated lithium iron phosphate by using water-soluble starch one-step hydrothermal method |
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| CN201510612799.4A CN105206812B (en) | 2015-09-24 | 2015-09-24 | The method that one step hydro thermal method prepares carbon coating type LiFePO4 |
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| CN201710630504.5A Division CN107293728B (en) | 2015-09-24 | 2015-09-24 | Method for preparing carbon-coated lithium iron phosphate by using water-soluble starch one-step hydrothermal method |
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| CN201510612799.4A Active CN105206812B (en) | 2015-09-24 | 2015-09-24 | The method that one step hydro thermal method prepares carbon coating type LiFePO4 |
| CN201710630504.5A Active CN107293728B (en) | 2015-09-24 | 2015-09-24 | Method for preparing carbon-coated lithium iron phosphate by using water-soluble starch one-step hydrothermal method |
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| CN110480004B (en) * | 2019-08-29 | 2021-11-09 | 南京理工大学 | Method for preparing carbon-coated nano aluminum powder by hydrothermal method |
| CN114335479A (en) * | 2021-12-31 | 2022-04-12 | 欣旺达电动汽车电池有限公司 | Carbon-coated lithium iron phosphate positive electrode material, preparation method thereof and lithium ion battery |
| CN115367724B (en) * | 2022-08-20 | 2023-08-04 | 河北择赛生物科技有限公司 | Method for producing lithium iron phosphate by using biomass agent |
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| CN101752564A (en) * | 2010-01-20 | 2010-06-23 | 河北工业大学 | Hydrothermal synthesis method of LiFePO4 of anode material of lithium ion battery with one-dimensional nanometer structure |
| CN103022425A (en) * | 2011-09-26 | 2013-04-03 | 比亚迪股份有限公司 | Preparation method of lithium iron phosphate material and lithium-ion battery |
| KR20130143151A (en) * | 2012-06-14 | 2013-12-31 | 주식회사 동진쎄미켐 | Positive active material for rechargeable lithium battery, method of preparing the same, and rechargeable lithium battery including the same |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN107293728B (en) | 2020-02-25 |
| CN107317018B (en) | 2020-06-26 |
| CN107293728A (en) | 2017-10-24 |
| CN105206812B (en) | 2017-09-22 |
| CN107317018A (en) | 2017-11-03 |
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