CN116014138A - Nanometer lithium iron phosphate and preparation method and application thereof - Google Patents
Nanometer lithium iron phosphate and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides nano lithium iron phosphate and a preparation method and application thereof, and belongs to the technical field of preparation of lithium ion batteries and electrode materials. The process method comprises the steps of firstly preparing polyaniline modified ferric phosphate by adopting ammonium dihydrogen phosphate, ferrous sulfate and aniline, then further preparing polyvinylpyrrolidone coated nano lithium iron phosphate by taking the obtained modified ferric phosphate as a precursor, polyvinylpyrrolidone, lithium carbonate and a reducing agent, and finally coating the polyvinylpyrrolidone coated nano lithium iron phosphate again by adopting tannic acid to obtain the novel nano lithium iron phosphate composite material. The novel nano lithium iron phosphate composite material prepared by the invention has high electrochemical activity and good stability, can well relieve the problem that nano lithium iron phosphate particles are easy to agglomerate, effectively improves the tap density of nano lithium iron phosphate and further ensures the service performance of the lithium ion battery in a low-temperature environment.
Description
Technical Field
The invention belongs to the technical field of preparation of lithium ion batteries and electrode materials, and particularly relates to nano lithium iron phosphate and a preparation method and application thereof.
Background
The performance of lithium ion batteries is mainly dependent on the positive and negative electrode materials, lithium iron phosphate (molecular formula LiFePO 4 Abbreviated LFP) is one of the currently used positive electrode materials of lithium ion batteries, which has safety performance and cycle life that other materials cannot compare: the 1C charge-discharge cycle life reaches 2000 times, and the single battery is charged by 30V without burning or explosion after puncture. Since the discovery in the 90 s, lithium iron phosphate becomes an ideal positive electrode material of a new generation of lithium ion batteries, and is the leading edge of the development field of the current lithium ion batteries.
On the other hand, lithium iron phosphate also has the defects of poor conductive performance, low lithium ion diffusion speed, low tap density and poor low-temperature performance. Aiming at the technical defects of lithium iron phosphate as a positive electrode material, the prior art mainly adopts organic carbon source and metal ion combined doping, nanocrystallization of LFP crystal grains, addition of an additional conductive agent and the like; however, the inherent properties of the lithium iron phosphate material are key to determining the performance, and the method cannot substantially and effectively change the tap density and low-temperature performance of the lithium iron phosphate, which results in significant reduction of capacitance and cycle life at low temperature of the lithium ion battery manufactured by taking the lithium iron phosphate as the positive electrode material, and thus severely limits the practical application of the lithium ion battery.
In view of the above, there is still a need to develop a novel lithium iron phosphate composite material to overcome the defects of low tap density and poor low-temperature discharge performance.
Disclosure of Invention
Aiming at the defects and shortcomings of the lithium iron phosphate in the practical lithium ion battery production application in the background art, the invention aims to provide a nano lithium iron phosphate and a preparation method and application thereof. The technological process of the present invention includes first preparing polyaniline modified ferric phosphate (PAn-FePO) with monoammonium phosphate, ferrous sulfate and aniline 4 ) The invention further uses the obtained modified ferric phosphate as a precursor and polyvinylpyrrolidone (PVP), lithium carbonate and a reducing agent to prepare the poly (vinyl pyrrolidone)The nano lithium iron phosphate coated by the vinyl pyrrolidone is coated again by the tannic acid to obtain the novel nano lithium iron phosphate composite material, which overcomes the defect of the self property of the lithium iron phosphate, can provide stable chemical and electrochemical reaction interfaces, and meets the performance requirement of a high-performance lithium ion battery.
In order to achieve the above purpose, the invention is realized by the following technical scheme:
the invention provides a preparation method of nano lithium iron phosphate, which comprises the following steps:
step 1): dissolving monoammonium phosphate and aniline in deionized water, continuously stirring, adding ferrous sulfate and hydrogen peroxide, filtering and washing a reaction product to obtain PAn-ferric phosphate;
step 2): adding PAn-ferric phosphate obtained in the step 1) into polyvinylpyrrolidone water solution, controlling the temperature at high pressure, centrifuging and collecting precipitate, washing and drying the precipitate, fully mixing the precipitate with lithium carbonate and a reducing agent, sintering, and ball-milling to obtain PVP-nano lithium iron phosphate;
step 3): adding PVP-nano lithium iron phosphate obtained in the step 2) into a tannic acid aqueous solution, carrying out ultrasonic treatment, finally centrifuging, collecting precipitate, washing, drying, roasting and ball-milling to obtain the PVP-nano lithium iron phosphate.
Preferably, the molar ratio of the ammonium dihydrogen phosphate, the aniline, the ferrous sulfate and the hydrogen peroxide in the step 1) is 1.8:1:3.2:0.35.
Preferably, in the step 1), the temperature of the deionized water is 40-50 ℃; the ferrous sulfate is added, and a pH regulator is also added to control the pH value to be 1.5-3, and the temperature is raised to 90-120 ℃.
Preferably, the aqueous solution of polyvinylpyrrolidone in step 2) contains 2g of polyvinylpyrrolidone, 50 ml of ethanol and 50 ml of deionized water per 100 ml; the high-pressure temperature-controlled treatment temperature is 175-190 ℃.
Preferably, the solid-to-liquid ratio of the PAn-ferric phosphate to the polyvinylpyrrolidone aqueous solution in the step 2) is 1:10, g/mL; the molar ratio of PAn-ferric phosphate to lithium carbonate to reducing agent is 1 (0.7-0.9): 1.5-2.4); the reducing agent is hydrazine hydrate.
Preferably, the sintering temperature in the step 2) is 450-500 ℃ and the sintering time is 2h.
Preferably, the solid-to-liquid ratio of the PVP-nano lithium iron phosphate to the tannic acid aqueous solution in the step 3) is 1:5, g/mL; the concentration of tannic acid in the aqueous tannic acid solution was 2.5mg/mL.
Preferably, the ultrasonic frequency of the ultrasonic treatment in the step 3) is 60kHz; the roasting temperature is 650-750 ℃ and the time is 30min.
Aiming at the problem that the tap density is difficult to improve due to larger stacking gaps of micron-sized lithium iron phosphate, the prior art expects to reduce the gaps by stacking small particles or fill the gaps of large particles with small particles through nanocrystallization of lithium iron phosphate crystal grains so as to improve the tap density. However, in practical application, the smaller the granularity of the lithium iron phosphate crystal grains is, the more easily the lithium iron phosphate crystal grains are agglomerated, so that a plurality of small particles are mutually bonded and agglomerated into secondary particles, and the larger secondary particles are stacked again, so that the tap density is lower than that of micron-sized lithium iron phosphate. In view of the above problems and practical drawbacks, the present inventors firstly regulate the reaction temperature and pH from the lithium iron phosphate crystal grain itself and the surface properties, and simultaneously add aniline during the reaction process of ammonium dihydrogen phosphate and ferrous sulfate to prepare polyaniline-modified ferric phosphate, and on this basis, further prepare polyvinylpyrrolidone-coated nano lithium iron phosphate with the modified ferric phosphate as a precursor; the nano lithium iron phosphate coated by polyvinylpyrrolidone prepared by the invention not only greatly improves the conductivity and electrochemical activity of the lithium iron phosphate, but also has low impurity phase content and small negative influence on low-temperature discharge performance. For the agglomeration problem of nano lithium iron phosphate, the invention further adopts tannic acid to carry out secondary coating on the nano lithium iron phosphate coated by polyvinylpyrrolidone, and constructs a homogenized 3D conductive carbon network based on the cooperation of polyvinylpyrrolidone and tannic acid, so that the lithium iron phosphate has high electrochemical activity and good stability, can well alleviate the problem that nano lithium iron phosphate particles are easy to agglomerate, effectively improves the tap density of the nano lithium iron phosphate, and further ensures the service performance of the lithium ion battery in a low-temperature environment.
The invention provides nano lithium iron phosphate, which is prepared by adopting the method.
The invention also provides a positive electrode material for the lithium ion battery, which comprises the nano lithium iron phosphate.
Compared with the prior art, the invention has the beneficial effects that:
aiming at the defects of the self property of lithium iron phosphate and the limitations of the conventional technical means, the novel nano lithium iron phosphate composite material is prepared by taking polyaniline modified ferric phosphate as a precursor and adopting polyvinylpyrrolidone and tannic acid to coat the polyaniline modified ferric phosphate twice, so that the problem that nano lithium iron phosphate particles are easy to agglomerate is effectively solved, the tap density of the nano lithium iron phosphate is improved, the service performance of a lithium ion battery in a low-temperature environment is further ensured, and the nano lithium iron phosphate composite material has good market competitiveness.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described in the following examples. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. The term "and/or" as used herein includes any and all combinations of one or more of the associated listed items.
Example 1
A method for preparing nano lithium iron phosphate, comprising the following steps:
1. and respectively weighing ammonium dihydrogen phosphate, aniline, ferrous sulfate and hydrogen peroxide (30%) according to a molar ratio of 1.8:1:3.2:0.35 for standby, dissolving the ammonium dihydrogen phosphate and the aniline in deionized water at 45 ℃ for continuous stirring for 30min, adding the ferrous sulfate and the hydrogen peroxide, adding phosphoric acid (85%) to control the pH value to be 2.2, heating to 108 ℃ for reaction for 3h, and cooling, filtering and washing the product after the reaction is finished to obtain the PAn-ferric phosphate.
2. PAn-ferric phosphate is added into polyvinylpyrrolidone aqueous solution (solid-liquid ratio is 1:10, g/mL; each 100 mL polyvinylpyrrolidone aqueous solution contains 2g polyvinylpyrrolidone, 50 mL ethanol and 50 mL deionized water), the temperature of a high-pressure reaction kettle is kept at 185 ℃ for 6 hours, then the precipitate is centrifugally collected, washed and dried, the obtained product is fully mixed with lithium carbonate and hydrazine hydrate (PAn-ferric phosphate: lithium carbonate: hydrazine hydrate molar ratio is 1:0.8:2), and PVP-nano lithium iron phosphate is obtained after sintering at 480 ℃ for 2 hours and ball milling.
3. Adding PVP-nano lithium iron phosphate into tannic acid aqueous solution (solid-liquid ratio is 1:5, g/mL), performing ultrasonic treatment at 60kHz for 30min, centrifugally collecting precipitate, washing and drying, roasting the obtained product at 700 ℃ for 30min, and performing ball milling to obtain nano lithium iron phosphate composite material (the tap density is 1.28 g/cm) 3 )。
The nano lithium iron phosphate composite material/aluminum sheet prepared in the embodiment is taken as a positive electrode, a lithium sheet is taken as a negative electrode, and 1MLiPF 6 EC, DEC, DMC (volume ratio 1:1:1) as electrolyte, and testing the low-temperature discharge performance: the specific discharge capacity is 153mAh/g at 25 ℃/0.5C, and 130mAh/g at 25 ℃/5C; -a discharge capacity retention rate of 77% at 15 ℃/0.5C and 71% at 15 ℃/5C; the specific discharge capacity is measured to be 106mAh/g after 1000 charge-discharge cycles at 15 ℃/0.5 ℃.
Example 2
A method for preparing nano lithium iron phosphate, comprising the following steps:
1. and respectively weighing ammonium dihydrogen phosphate, aniline, ferrous sulfate and hydrogen peroxide (30%) according to a molar ratio of 1.8:1:3.2:0.35 for standby, dissolving the ammonium dihydrogen phosphate and the aniline in deionized water at 45 ℃ for continuous stirring for 30min, adding the ferrous sulfate and the hydrogen peroxide, adding phosphoric acid (85%) to control the pH value to be 1.8, heating to 120 ℃ and raising the temperature for reacting for 2.5h, and cooling, filtering and washing the product after the reaction is finished to obtain the PAn-ferric phosphate.
2. PAn-ferric phosphate is added into polyvinylpyrrolidone aqueous solution (solid-liquid ratio is 1:10, g/mL; each 100 mL polyvinylpyrrolidone aqueous solution contains 2g polyvinylpyrrolidone, 50 mL ethanol and 50 mL deionized water), the temperature of a high-pressure reaction kettle is controlled at 175 ℃ for 6 hours, then the precipitate is centrifugally collected, washed and dried, the obtained product is fully mixed with lithium carbonate and hydrazine hydrate (PAn-ferric phosphate: lithium carbonate: hydrazine hydrate molar ratio is 1:0.7:2.4), and PVP-nano lithium iron phosphate is obtained after sintering at 500 ℃ for 2 hours.
3. Adding PVP-nano lithium iron phosphate into tannic acid aqueous solution (solid-liquid ratio is 1:5, g/mL), performing ultrasonic treatment at 60kHz for 30min, centrifugally collecting precipitate, washing and drying, roasting the obtained product at 750 ℃ for 30min, and performing ball milling to obtain nano lithium iron phosphate composite material (the tap density is 1.22 g/cm) 3 )。
The nano lithium iron phosphate composite material/aluminum sheet prepared in the embodiment is taken as a positive electrode, a lithium sheet is taken as a negative electrode, and 1MLiPF 6 EC, DEC, DMC (volume ratio 1:1:1) as electrolyte, and testing the low-temperature discharge performance: the specific discharge capacity is 146mAh/g at 25 ℃/0.5C, and 127mAh/g at 25 ℃/5C; -a discharge capacity retention rate of 74% at 15 ℃/0.5C and 66% at 15 ℃/5C; the specific discharge capacity is measured to be 95mAh/g after 1000 charge-discharge cycles at 15 ℃/0.5 ℃.
Example 3
A method for preparing nano lithium iron phosphate, comprising the following steps:
1. and respectively weighing ammonium dihydrogen phosphate, aniline, ferrous sulfate and hydrogen peroxide (30%) according to a molar ratio of 1.8:1:3.2:0.35 for standby, dissolving the ammonium dihydrogen phosphate and the aniline in deionized water at 45 ℃ for continuous stirring for 30min, adding the ferrous sulfate and the hydrogen peroxide, adding phosphoric acid (85%) to control the pH value to 2.8, heating to 90 ℃ and raising the temperature for reaction for 3.5h, and cooling, filtering and washing the product after the reaction is finished to obtain PAn-ferric phosphate.
2. PAn-ferric phosphate is added into polyvinylpyrrolidone aqueous solution (solid-liquid ratio is 1:10, g/mL; each 100 mL polyvinylpyrrolidone aqueous solution contains 2g polyvinylpyrrolidone, 50 mL ethanol and 50 mL deionized water), the temperature of a high-pressure reaction kettle is controlled at 190 ℃ for 6 hours, then the precipitate is centrifugally collected, washed and dried, the obtained product is fully mixed with lithium carbonate and hydrazine hydrate (PAn-ferric phosphate: lithium carbonate: hydrazine hydrate molar ratio is 1:0.9:1.5), and PVP-nano lithium iron phosphate is obtained after sintering at 450 ℃ for 2 hours and ball milling.
3. Adding PVP-nano lithium iron phosphate into tannic acid aqueous solution (solid-liquid ratio is 1:5, g/mL), performing ultrasonic treatment at 60kHz for 30min, centrifugally collecting precipitate, washing and drying, roasting the obtained product at 650 ℃ for 30min, and performing ball milling to obtain nano lithium iron phosphate composite material (the tap density is 1.25 g/cm) 3 )。
The nano lithium iron phosphate composite material/aluminum sheet prepared in the embodiment is taken as a positive electrode, a lithium sheet is taken as a negative electrode, and 1MLiPF 6 EC, DEC, DMC (volume ratio 1:1:1) as electrolyte, and testing the low-temperature discharge performance: the specific discharge capacity is 148mAh/g at 25 ℃/0.5C, and 129mAh/g at 25 ℃/5C; -a discharge capacity retention rate of 76% at 15 ℃/0.5C and 68% at 15 ℃/5C; the specific discharge capacity is 101mAh/g after 1000 charge-discharge cycles at 15 ℃/0.5 ℃.
Comparative example 1
Except that aniline was not added in step 1, i.e., the subsequent process was performed using ferric phosphate prepared from monoammonium phosphate and ferrous sulfate, and the rest was the same as in example 1. The tap density of the obtained nano lithium iron phosphate is 0.83g/cm 3 。
The nano lithium iron phosphate composite material/aluminum sheet prepared in the comparative example is used as a positive electrode, a lithium sheet is used as a negative electrode, and 1MLiPF 6 EC, DEC, DMC (volume ratio 1:1:1) as electrolyte, and testing the low-temperature discharge performance: the specific discharge capacity is 137mAh/g at 25 ℃/0.5C, and 116mAh/g at 25 ℃/5C; -a discharge capacity retention rate of 73% at 15 ℃/0.5C and 65% at 15 ℃/5C; the specific discharge capacity was found to be 78mAh/g after 1000 charge-discharge cycles at 15℃and 0.5 ℃.
Comparative example 2
The difference is that the PAn-ferric phosphate obtained in the step 1 is directly and fully mixed with lithium carbonate and hydrazine hydrate (the molar ratio of PAn-ferric phosphate to lithium carbonate to hydrazine hydrate is 1:0.8:2) without adopting polyvinylpyrrolidone aqueous solution and high-pressure temperature control treatment. The tap density of the obtained nano lithium iron phosphate is 0.75g/cm 3 。
The nano lithium iron phosphate composite material/aluminum sheet prepared in the comparative example is used as a positive electrode, a lithium sheet is used as a negative electrode, and 1MLiPF 6 EC, DEC, DMC (volume ratio 1:1:1) as electrolyte, and testing the low-temperature discharge performance: the specific discharge capacity is 147mAh/g at 25 ℃/0.5C, and 129mAh/g at 25 ℃/5C; -a discharge capacity retention rate of 59% at 15 ℃/0.5C and 44% at 15 ℃/5C; the specific discharge capacity was measured to be 59mAh/g after 1000 charge-discharge cycles at 15℃and 0.5 ℃.
Comparative example 3
PVP-nano lithium iron phosphate prepared in the step 2 of the embodiment 1 is taken. The tap density was measured to be 0.71g/cm 3 。
PVP-nanometer lithium iron phosphate/aluminum sheet as positive electrode, lithium sheet as negative electrode, 1M LiPF 6 EC, DEC, DMC (volume ratio 1:1:1) as electrolyte, and testing the low-temperature discharge performance: the specific discharge capacity is 146mAh/g at 25 ℃/0.5C, and 130mAh/g at 25 ℃/5C; -a discharge capacity retention rate of 55% at 15 ℃/0.5C and 39% at 15 ℃/5C; the specific discharge capacity is 54mAh/g after 1000 charge-discharge cycles at 15 ℃/0.5 ℃.
The embodiments described above represent only a few preferred embodiments of the present invention, which are described in more detail and are not intended to limit the present invention. It should be noted that various changes and modifications can be made to the present invention by those skilled in the art, and any modifications, equivalent substitutions, improvements, etc. which are within the spirit and principle of the present invention are included in the scope of the present invention.
Claims (10)
1. The preparation method of the nano lithium iron phosphate is characterized by comprising the following steps of:
step 1): dissolving monoammonium phosphate and aniline in deionized water, continuously stirring, adding ferrous sulfate and hydrogen peroxide, filtering and washing a reaction product to obtain PAn-ferric phosphate;
step 2): adding PAn-ferric phosphate obtained in the step 1) into polyvinylpyrrolidone water solution, controlling the temperature at high pressure, centrifuging and collecting precipitate, washing and drying the precipitate, fully mixing the precipitate with lithium carbonate and a reducing agent, sintering, and ball-milling to obtain PVP-nano lithium iron phosphate;
step 3): adding PVP-nano lithium iron phosphate obtained in the step 2) into a tannic acid aqueous solution, carrying out ultrasonic treatment, finally centrifuging, collecting precipitate, washing, drying, roasting and ball-milling to obtain the PVP-nano lithium iron phosphate.
2. The method for preparing nano lithium iron phosphate according to claim 1, wherein the molar ratio of ammonium dihydrogen phosphate, aniline, ferrous sulfate and hydrogen peroxide in step 1) is 1.8:1:3.2:0.35.
3. The method for preparing nano lithium iron phosphate according to claim 1, wherein in the step 1), the temperature of deionized water is 40-50 ℃; while adding ferrous sulfate, phosphoric acid is also required to be added to control the pH value to be 1.5-3, and the temperature is raised to 90-120 ℃.
4. The method for preparing nano lithium iron phosphate according to claim 1, wherein the aqueous solution of polyvinylpyrrolidone in step 2) contains 2g of polyvinylpyrrolidone, 50 ml of ethanol and 50 ml of deionized water per 100 ml; the high-pressure temperature-controlled treatment temperature is 175-190 ℃.
5. The method for preparing nano lithium iron phosphate according to claim 1, wherein the solid-to-liquid ratio of PAn-ferric phosphate to polyvinylpyrrolidone aqueous solution in step 2) is 1:10, g/mL; the molar ratio of PAn-ferric phosphate to lithium carbonate to reducing agent is 1 (0.7-0.9): 1.5-2.4); the reducing agent is hydrazine hydrate.
6. The method for preparing nano lithium iron phosphate according to claim 1, wherein the sintering temperature in step 2) is 450-500 ℃ and the sintering time is 2h.
7. The method for preparing nano lithium iron phosphate according to claim 1, wherein the solid-to-liquid ratio of the PVP-nano lithium iron phosphate to the tannic acid aqueous solution in step 3) is 1:5, g/mL; the concentration of tannic acid in the aqueous tannic acid solution was 2.5mg/mL.
8. The method for preparing nano lithium iron phosphate according to claim 1, wherein the ultrasonic frequency of the ultrasonic treatment in the step 3) is 60kHz; the roasting temperature is 650-750 ℃ and the time is 30min.
9. A nano lithium iron phosphate prepared by the method of any one of claims 1-8.
10. A positive electrode material for a lithium ion battery comprising the nano lithium iron phosphate according to claim 9.
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| CN117142450A (en) * | 2023-09-05 | 2023-12-01 | 湖北三峡实验室 | Method for preparing lithium iron phosphate anode material by taking tea polyphenol as carbon source |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117142450A (en) * | 2023-09-05 | 2023-12-01 | 湖北三峡实验室 | Method for preparing lithium iron phosphate anode material by taking tea polyphenol as carbon source |
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