CN114497565A - High-capacity lithium ferric manganese phosphate cathode material and processing technology - Google Patents
High-capacity lithium ferric manganese phosphate cathode material and processing technology Download PDFInfo
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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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Abstract
The invention relates to the technical field of lithium manganese iron phosphate anode materials, in particular to a high-capacity lithium manganese iron phosphate anode material, which comprises the following materials: a phosphorus source, a lithium source, a carbon source I, a carbon source II, a manganese source and an iron source. A processing technology of a high-capacity lithium ferric manganese phosphate cathode material comprises the following steps: s1: mixing a carbon source I, a manganese source and an iron source according to the proportion of 1: 1.03: 1.1 mixing and putting into a ball mill, adding a solvent and an organic hydrophobic modifier for ball milling to obtain the iron manganese phosphate mixed slurry which is used as a carbon source and is doped in situ. The invention has the beneficial effects that: the coated lithium manganese iron phosphate anode material is prepared by two different carbon sources and two-step in-situ coating, the carbon coating method is more uniform in coating and more excellent in conductivity, the carbon source C1 is composed of sulfur-doped graphene and a conductive polymer, the carbon source C2 is a nitrogen and phosphorus co-doped carbon material, and the dissolution of iron and manganese ions in electrolyte can be effectively inhibited by adding the two carbon sources.
Description
Technical Field
The invention relates to the technical field of lithium manganese iron phosphate anode materials, in particular to a high-capacity lithium manganese iron phosphate anode material and a processing technology thereof.
Background
Lithium ion batteries are widely used because of their advantages of high operating voltage, high specific capacity, safety, stability, good cycle performance, wide operating temperature range, etc. With the popularization of new energy automobiles, a high-performance lithium ion battery is most hopeful to become one of power supplies of electric automobiles, the positive electrode material is the core part of the lithium ion battery, the performance of the positive electrode material directly determines the performance index of a lithium ion battery product, and lithium manganese phosphate and lithium iron phosphate are both good-development-prospect positive electrode materials of the lithium ion battery.
Chinese patent No. CN113651304A provides an organic carbon-coated lithium iron phosphate positive electrode material and a preparation method thereof, belonging to the technical field of preparation of lithium ion battery electrode materials. And (2) performing ball milling and mixing in a high-speed ball milling tank by using one or two of iron phosphate, lithium carbonate, citric acid, glucose and asphalt as a carbon source and alcohol as a solvent, drying the mixed solution, and sintering at a high temperature to obtain the carbon-coated lithium iron phosphate cathode material.
However, the high-capacity lithium manganese iron phosphate cathode material and the processing technology thereof have the disadvantages that the coating method is poor in the manufacturing process, so that the high-capacity lithium manganese iron phosphate cathode material is low in rate performance, poor in cycle stability, high in voltage of lithium manganese phosphate, high in energy density, poor in conductivity, hygroscopic and incapable of meeting the use requirements during large-current charging and discharging, and is not beneficial to wide popularization.
Disclosure of Invention
The invention aims to provide a high-capacity lithium ferric manganese phosphate cathode material and a processing technology thereof, and aims to solve the problems of low rate performance, poor cycle stability, poor conductivity and hygroscopicity in large-current charging and discharging due to the poor coating method in the background technology.
The technical scheme of the invention is as follows: a high-capacity lithium ferric manganese phosphate cathode material comprises the following materials: a phosphorus source, a lithium source, a carbon source I, a carbon source II, a manganese source and an iron source.
A processing technology of a high-capacity lithium ferric manganese phosphate cathode material comprises the following steps:
s1: mixing a carbon source I, a manganese source and an iron source according to the proportion of 1: 1.03: 1.1 mixing and putting into a ball mill, adding a solvent and an organic hydrophobic modifier for ball milling to obtain a carbon source-in-situ doped iron manganese phosphate mixed slurry;
s2: mixing the mixed slurry obtained in the step S1 with a lithium source, a nitrogen residue doped oxide and a carbon source II, and performing secondary ball milling;
s3: placing the mixed slurry into a drying oven for primary drying, and sieving by a sieve;
s4: putting the powder obtained in the step S2 into spray drying equipment, and carrying out spray drying to obtain a precursor spray material;
s5: and heating the precursor material obtained in the step S4 for calcining to obtain the coated lithium manganese iron phosphate cathode material.
Further, the first carbon source is composed of sulfur-doped graphene and a conductive polymer, the second carbon source is a nitrogen and phosphorus co-doped carbon material, the lithium source is at least one of lithium dihydrogen phosphate, lithium carbonate, lithium oxalate, lithium acetate and lithium hydroxide, the phosphorus source is at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate and phosphoric acid, the iron source is at least one of ferrous hydroxide, ferrous chloride, ferrous oxalate and ferrous sulfate, and the manganese source is at least one of manganese chloride, manganese carbonate, manganese acetate, manganese sulfate and manganese oxalate.
Further, the organic hydrophobic modifier is selected from at least one of PVDF and a polyoxyalkylene copolymer.
Further, in the step S1, the feed liquid is firstly coarsely ground until D50 is less than or equal to 1.2 μm, and then is continuously finely ground until D50 is 0.45-0.50 μm.
Furthermore, the rotation speed of ball milling in S1 and S2 is 200-500r/min, the ball milling time is 3-25h, and the secondary ball is ground until D50 is 0.15-0.3 mu.
Further, the primary drying time in the S3 is 1-2.5h, and the drying temperature is 15-100 ℃.
Further, the sieve in S3 is 80-150 meshes.
Further, the temperature of the air inlet is 185-220 ℃ during spray drying in the S4, and the temperature of the outlet air is controlled to be 95-105 ℃.
Further, the calcination temperature in S5 is 450-1000 ℃, and the calcination time is 5-20 h.
The invention provides a high-capacity lithium ferric manganese phosphate anode material and a processing technology thereof through improvement, and compared with the prior art, the invention has the following improvements and advantages:
(1) the carbon coating method is more uniform in coating and more excellent in conductivity, the carbon source C1 is composed of sulfur-doped graphene and a conductive polymer, the carbon source C2 is a nitrogen and phosphorus co-doped carbon material, the dissolution of iron and manganese ions in electrolyte can be effectively inhibited by adding the two carbon sources, the structural collapse of the anode material is prevented, the rate capability and the cycle stability of the anode material are improved, the rate capability is higher during heavy-current charging and discharging, and the cycle stability is stronger.
(2) By adding the phosphorus source and the iron source, the lithium manganese phosphate has high voltage, high energy density and poor conductivity, while the lithium iron phosphate has high thermal stability, environmental friendliness, low cost and slow diffusion rate, and the prepared lithium manganese phosphate anode material has high thermal stability, low impurity content, high tap density and strong conductivity by combining the phosphorus source and the iron source.
(3) Through the added organic hydrophobic modifier, at least part of hydrophobic groups in the organic hydrophobic modifier can be loaded on the lithium manganese iron phosphate material, so that the lithium manganese iron phosphate positive electrode material with certain carbon content and hydrophobic performance can be formed; particularly, when the specific organic hydrophobic modifier is selected, the lithium manganese iron phosphate cathode material has excellent hydrophobic property, the saturated water absorption is less than 100ppm, and the lithium manganese iron phosphate cathode material with ppm-level hydrophobic capacity is realized.
Drawings
The invention is further explained below with reference to the figures and examples:
FIG. 1 is a schematic view of the processing flow structure of the present invention.
Detailed Description
The present invention will be described in detail with reference to fig. 1, and the technical solutions in the embodiments of the present invention will be clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When a component is referred to as being "connected" to another component, it can be directly connected to the other component or intervening components may also be present. When a component is referred to as being "disposed on" another component, it can be directly on the other component or intervening components may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only.
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. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The invention provides a high-capacity lithium manganese iron phosphate cathode material and a processing technology thereof through improvement, and as shown in figure 1, the high-capacity lithium manganese iron phosphate cathode material comprises the following materials: a phosphorus source, a lithium source, a carbon source I, a carbon source II, a manganese source and an iron source.
A processing technology of a high-capacity lithium ferric manganese phosphate cathode material comprises the following steps:
s1: mixing a carbon source I, a manganese source and an iron source according to the proportion of 1: 1.03: 1.1 mixing and putting into a ball mill, adding a solvent and an organic hydrophobic modifier for ball milling to obtain a carbon source-in-situ doped iron manganese phosphate mixed slurry;
s2: mixing the mixed slurry obtained in the step S1 with a lithium source, a nitrogen residue doped oxide and a carbon source II, and performing secondary ball milling;
s3: placing the mixed slurry into a drying oven for primary drying, and sieving by a sieve;
s4: putting the powder obtained in the step S2 into spray drying equipment, and carrying out spray drying to obtain a precursor spray material;
s5: and heating the precursor material obtained in the step S4 for calcining to obtain the coated lithium manganese iron phosphate cathode material.
Further, the first carbon source is composed of sulfur-doped graphene and a conductive polymer, the second carbon source is a nitrogen and phosphorus co-doped carbon material, the lithium source is at least one of lithium dihydrogen phosphate, lithium carbonate, lithium oxalate, lithium acetate and lithium hydroxide, the phosphorus source is at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate and phosphoric acid, the iron source is at least one of ferrous hydroxide, ferrous chloride, ferrous oxalate and ferrous sulfate, and the manganese source is at least one of manganese chloride, manganese carbonate, manganese acetate, manganese sulfate and manganese oxalate.
Further, the organic hydrophobic modifier is selected from at least one of PVDF and a polyoxyalkylene copolymer.
Further, in the step S1, the feed liquid is firstly coarsely ground until D50 is less than or equal to 1.2 μm, and then is continuously finely ground until D50 is 0.45 μm.
Further, the rotation speed of ball milling in the S1 and S2 is 200r/min, the time of ball milling is 3h, and secondary balls are ground to be 0.15 mu in D50.
Further, the time for the primary drying in S3 is 1h, and the drying temperature is 15 ℃.
Further, the mesh in S3 is located at 80 mesh.
Further, the temperature of the air inlet is 185 ℃ during spray drying in the step S4, and the temperature of the outlet air is controlled at 95 ℃.
Further, the temperature of the calcination in S5 was 450 ℃, and the calcination time was 5 h.
Example one
A high-capacity lithium ferric manganese phosphate cathode material comprises the following materials: a phosphorus source, a lithium source, a carbon source I, a carbon source II, a manganese source and an iron source.
A processing technology of a high-capacity lithium ferric manganese phosphate cathode material comprises the following steps:
s1: mixing a carbon source I, a manganese source and an iron source according to the proportion of 1: 1.03: 1.1 mixing and putting into a ball mill, adding a solvent and an organic hydrophobic modifier for ball milling to obtain a carbon source-in-situ doped iron manganese phosphate mixed slurry;
s2: mixing the mixed slurry obtained in the step S1 with a lithium source, a nitrogen residue doped oxide and a carbon source II, and performing secondary ball milling;
s3: placing the mixed slurry into a drying oven for primary drying, and sieving by a sieve;
s4: putting the powder obtained in the step S2 into spray drying equipment, and carrying out spray drying to obtain a precursor spray material;
s5: and heating the precursor material obtained in the step S4 for calcining to obtain the coated lithium manganese iron phosphate cathode material.
Further, the first carbon source is composed of sulfur-doped graphene and a conductive polymer, the second carbon source is a nitrogen and phosphorus co-doped carbon material, the lithium source is at least one of lithium dihydrogen phosphate, lithium carbonate, lithium oxalate, lithium acetate and lithium hydroxide, the phosphorus source is at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate and phosphoric acid, the iron source is at least one of ferrous hydroxide, ferrous chloride, ferrous oxalate and ferrous sulfate, and the manganese source is at least one of manganese chloride, manganese carbonate, manganese acetate, manganese sulfate and manganese oxalate.
Further, the organic hydrophobic modifier is selected from at least one of PVDF and a polyoxyalkylene copolymer.
In S1, the feed liquid is first coarsely ground until D50 is less than or equal to 1.2 μm, and then finely ground until D50 is 0.46 μm.
Furthermore, the rotation speed of ball milling in the S1 and S2 is 300r/min, the time of ball milling is 10h, and secondary balls are ground to be 0.2 mu in D50.
Further, the time for the primary drying in S3 is 1.6h, and the drying temperature is 45 ℃.
Further, the mesh in S3 is located at 100 mesh.
Further, the temperature of the air inlet is 197 ℃ during spray drying in the S4, and the air outlet temperature is controlled at 98 ℃.
Further, the temperature of calcination in S5 was 650 ℃, and the calcination time was 10 h.
Example two
A high-capacity lithium ferric manganese phosphate cathode material comprises the following materials: a phosphorus source, a lithium source, a carbon source I, a carbon source II, a manganese source and an iron source.
A processing technology of a high-capacity lithium ferric manganese phosphate cathode material comprises the following steps:
s1: mixing a carbon source I, a manganese source and an iron source according to the proportion of 1: 1.03: 1.1 mixing and putting into a ball mill, adding a solvent and an organic hydrophobic modifier for ball milling to obtain a carbon source-in-situ doped iron manganese phosphate mixed slurry;
s2: mixing the mixed slurry obtained in the step S1 with a lithium source, a nitrogen residue doped oxide and a carbon source II, and performing secondary ball milling;
s3: placing the mixed slurry into a drying oven for primary drying, and sieving by a sieve;
s4: putting the powder obtained in the step S2 into spray drying equipment, and carrying out spray drying to obtain a precursor spray material;
s5: and heating the precursor material obtained in the step S4 for calcining to obtain the coated lithium manganese iron phosphate cathode material.
Further, the first carbon source is composed of sulfur-doped graphene and a conductive polymer, the second carbon source is a nitrogen and phosphorus co-doped carbon material, the lithium source is at least one of lithium dihydrogen phosphate, lithium carbonate, lithium oxalate, lithium acetate and lithium hydroxide, the phosphorus source is at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate and phosphoric acid, the iron source is at least one of ferrous hydroxide, ferrous chloride, ferrous oxalate and ferrous sulfate, and the manganese source is at least one of manganese chloride, manganese carbonate, manganese acetate, manganese sulfate and manganese oxalate.
Further, the organic hydrophobic modifier is selected from at least one of PVDF and a polyoxyalkylene copolymer.
Further, in the step S1, the feed liquid is firstly coarsely ground until D50 is less than or equal to 1.2 μm, and then is continuously finely ground until D50 is 0.48 μm.
Further, the rotation speed of ball milling in the S1 and S2 is 400r/min, the time of ball milling is 17h, and secondary balls are ground to be 0.25 mu in D50.
Further, the time for the primary drying in S3 is 2.1h, and the drying temperature is 75 ℃.
Further, the mesh in S3 is 130 mesh.
Further, the temperature of the air inlet is 210 ℃ during spray drying in the step S4, and the temperature of the outlet air is controlled at 103 ℃.
Further, the temperature of the calcination in S5 was 850 ℃, and the calcination time was 16 h.
EXAMPLE III
A high-capacity lithium ferric manganese phosphate cathode material comprises the following materials: a phosphorus source, a lithium source, a carbon source I, a carbon source II, a manganese source and an iron source.
A processing technology of a high-capacity lithium ferric manganese phosphate cathode material comprises the following steps:
s1: mixing a carbon source I, a manganese source and an iron source according to the proportion of 1: 1.03: 1.1 mixing and putting into a ball mill, adding a solvent and an organic hydrophobic modifier for ball milling to obtain a carbon source-in-situ doped iron manganese phosphate mixed slurry;
s2: mixing the mixed slurry obtained in the step S1 with a lithium source, a nitrogen residue doped oxide and a carbon source II, and performing secondary ball milling;
s3: placing the mixed slurry into a drying oven for primary drying, and sieving by a sieve;
s4: putting the powder obtained in the step S2 into spray drying equipment, and carrying out spray drying to obtain a precursor spray material;
s5: and heating the precursor material obtained in the step S4 for calcining to obtain the coated lithium manganese iron phosphate cathode material.
Further, the first carbon source is composed of sulfur-doped graphene and a conductive polymer, the second carbon source is a nitrogen and phosphorus co-doped carbon material, the lithium source is at least one of lithium dihydrogen phosphate, lithium carbonate, lithium oxalate, lithium acetate and lithium hydroxide, the phosphorus source is at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate and phosphoric acid, the iron source is at least one of ferrous hydroxide, ferrous chloride, ferrous oxalate and ferrous sulfate, and the manganese source is at least one of manganese chloride, manganese carbonate, manganese acetate, manganese sulfate and manganese oxalate.
Further, the organic hydrophobic modifier is selected from at least one of PVDF and a polyoxyalkylene copolymer.
Further, in the step S1, the feed liquid is firstly coarsely ground until D50 is less than or equal to 1.2 μm, and then is continuously finely ground until D50 is 0.5 μm.
Furthermore, the rotation speed of ball milling in the S1 and S2 is 500r/min, the ball milling time is 25h, and secondary balls are ground to be 0.3 mu in D50.
Further, the time for primary drying in S3 is 2.5h, and the drying temperature is 100 ℃.
Further, the mesh screen in S3 is 150 mesh.
Further, the temperature of the air inlet is 220 ℃ during spray drying in the S4, and the air outlet temperature is controlled at 105 ℃.
Further, the temperature of the calcination in S5 was 1000 ℃, and the calcination time was 20 h.
The working principle of the invention is as follows: the processing technology of the high-capacity lithium ferric manganese phosphate anode material comprises the following steps of mixing a carbon source I, a manganese source and an iron source according to a ratio of 1: 1.03: 1.1 mixing and placing the mixture into a ball mill, adding a solvent and an organic hydrophobic modifier for ball milling, coarsely milling until D50 is less than or equal to 1.2 mu m, continuously and finely milling until D50 is 0.45-0.50 mu, the ball milling rotation speed is 500 plus one jar of organic hydrophobic modifier, the ball milling time is 3-25h to obtain iron manganese phosphate mixed slurry in situ doping as a carbon source, then adding a lithium source, a nitrogen residue doped oxide and a carbon source for mixing and carrying out secondary ball milling, the ball milling rotation speed is 500 plus one jar of organic hydrophobic modifier and the ball milling time is 3-25h, the secondary ball is milled until D50 is 0.15-0.3 mu, then placing the mixed slurry into a drying box for drying for 1-2.5h, the temperature is 15-100 ℃, and passing through a 80-150 mesh sieve, placing the obtained powder into spray drying equipment for spray drying, the air inlet temperature is 185 plus one jar of organic hydrophobic modifier during spray drying, controlling the air outlet temperature at 95-105 ℃ to obtain a precursor spray material, and heating and calcining the obtained precursor material to obtain the coated lithium manganese iron phosphate cathode material.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (10)
1. A high-capacity lithium ferric manganese phosphate cathode material is characterized in that: comprises the following materials: a phosphorus source, a lithium source, a carbon source I, a carbon source II, a manganese source and an iron source.
2. A processing technology of a high-capacity lithium ferric manganese phosphate cathode material is characterized by comprising the following steps: the method comprises the following steps:
s1: mixing a carbon source I, a manganese source and an iron source according to the proportion of 1: 1.03: 1.1 mixing and putting into a ball mill, adding a solvent and an organic hydrophobic modifier for ball milling to obtain a carbon source-in-situ doped iron manganese phosphate mixed slurry;
s2: mixing the mixed slurry obtained in the step S1 with a lithium source, a nitrogen residue doped oxide and a carbon source II, and performing secondary ball milling;
s3: placing the mixed slurry into a drying oven for primary drying, and sieving by a sieve;
s4: putting the powder obtained in the step S2 into spray drying equipment, and carrying out spray drying to obtain a precursor spray material;
s5: and heating the precursor material obtained in the step S4 for calcining to obtain the coated lithium ferric manganese phosphate cathode material.
3. The processing technology of the lithium ferric manganese phosphate cathode material with high capacity according to claim 1, characterized in that: the carbon source I is composed of sulfur-doped graphene and a conductive polymer, the carbon source II is a nitrogen and phosphorus co-doped carbon material, the lithium source is at least one of lithium dihydrogen phosphate, lithium carbonate, lithium oxalate, lithium acetate and lithium hydroxide, the phosphorus source is at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate and phosphoric acid, the iron source is at least one of ferrous hydroxide, ferrous chloride, ferrous oxalate and ferrous sulfate, and the manganese source is at least one of manganese chloride, manganese carbonate, manganese acetate, manganese sulfate and manganese oxalate.
4. The processing technology of the lithium ferric manganese phosphate cathode material with high capacity according to claim 2, characterized in that: the organic hydrophobic modifier is at least one selected from PVDF and a polyoxyalkylene copolymer.
5. The processing technology of the lithium ferric manganese phosphate cathode material with high capacity according to claim 2, characterized in that: in the S1, the feed liquid is firstly coarsely ground until the D50 is less than or equal to 1.2 mu m, and then the feed liquid is continuously finely ground until the D50 is 0.45-0.50 mu.
6. The processing technology of the lithium ferric manganese phosphate cathode material with high capacity according to claim 2, characterized in that: the rotation speed of ball milling in the S1 and S2 is 200-500r/min, the ball milling time is 3-25h, and the secondary ball is finely ground until the D50 is 0.15-0.3 mu.
7. The processing technology of the lithium ferric manganese phosphate cathode material with high capacity according to claim 2, characterized in that: the primary drying time in the S3 is 1-2.5h, and the drying temperature is 15-100 ℃.
8. The processing technology of the lithium ferric manganese phosphate cathode material with high capacity according to claim 2, characterized in that: the sieve in the S3 is positioned at 80-150 meshes.
9. The processing technology of the lithium ferric manganese phosphate cathode material with high capacity according to claim 2, characterized in that: and the temperature of the air inlet is 185-220 ℃ during spray drying in the S4, and the temperature of the air outlet is controlled to be 95-105 ℃.
10. The processing technology of the lithium ferric manganese phosphate cathode material with high capacity according to claim 2, characterized in that: the calcining temperature in the S5 is 450-1000 ℃, and the calcining time is 5-20 h.
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| CN113582151A (en) * | 2021-07-28 | 2021-11-02 | 段镇忠 | Lithium ferric manganese phosphate cathode material and preparation method and application thereof |
| CN115676801A (en) * | 2022-11-22 | 2023-02-03 | 无锡零一未来新材料技术研究院有限公司 | Conductive agent coated positive electrode material, preparation method thereof and electrochemical energy storage device |
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| CN113582151A (en) * | 2021-07-28 | 2021-11-02 | 段镇忠 | Lithium ferric manganese phosphate cathode material and preparation method and application thereof |
| CN113582151B (en) * | 2021-07-28 | 2024-03-22 | 段镇忠 | Lithium iron manganese phosphate anode material and preparation method and application thereof |
| CN115676801A (en) * | 2022-11-22 | 2023-02-03 | 无锡零一未来新材料技术研究院有限公司 | Conductive agent coated positive electrode material, preparation method thereof and electrochemical energy storage device |
| CN115676801B (en) * | 2022-11-22 | 2024-05-10 | 无锡零一未来新材料技术研究院有限公司 | Conductive agent coated positive electrode material, preparation method thereof and electrochemical energy storage device |
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