CN111952563A - Preparation method of carbon-coated lithium titanium phosphate negative electrode material - Google Patents

Preparation method of carbon-coated lithium titanium phosphate negative electrode material Download PDF

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CN111952563A
CN111952563A CN202010816170.2A CN202010816170A CN111952563A CN 111952563 A CN111952563 A CN 111952563A CN 202010816170 A CN202010816170 A CN 202010816170A CN 111952563 A CN111952563 A CN 111952563A
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negative electrode
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李昌明
吴涛
叶嘉明
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Wuyi University
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
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    • H—ELECTRICITY
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    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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Abstract

The invention provides a preparation method of a carbon-coated lithium titanium phosphate negative electrode material, which comprises the step of mixing Ti (OC)4H9)4、Li2CO3、NH4H2PO4And C6H8O7Mixing to obtain a mixed solution; then transferring the gel into a water bath, heating to obtain gel, then drying in vacuum to obtain dry gel, and calcining the dry gel to obtain blocky LiTi2(PO4)3(ii) a Ball-milling the mixture into powder; dissolving beta-cyclodextrin and then mixing with LiTi2(PO4)3Mixing uniformly; then the black LiTi is obtained by vacuum drying and calcining under the protection of argon atmosphere2(PO4)3the/C composite negative electrode material. The negative electrode material prepared by the sol-gel method has uniform particle distribution and regular appearance; the invention uses LiTi2(PO4)3The carbon layer is coated on the surface of the negative electrode material, so that the electronic conductivity and the lithium ion diffusion coefficient of the negative electrode material are improved, and the high-rate charge and discharge performance is improved.

Description

Preparation method of carbon-coated lithium titanium phosphate negative electrode material
Technical Field
The invention relates to the technical field of lithium ion battery materials, in particular to a preparation method of a carbon-coated lithium titanium phosphate cathode material.
Background
Lithium ion batteries have been widely studied for their advantages of high energy density, long cycle life, no memory effect, high safety, and the like.
The negative electrode materials currently commercially used are mainly natural graphite and artificial graphite. The theoretical capacity of the traditional graphite material is 372mAh/g, although the traditional graphite material still has enough lithium storage capacity relative to the anode material. However, with the development demand of the field of high-rate rapid charging, graphite cannot meet the performance of rapid charging and discharging.
Lithium titanium phosphate LiTi2(PO4)3The theoretical specific capacity is 138 mAh/g. LiTi2(PO4)3Has a structure of sodium super-ion conductor belonging to the orthorhombic system, space group R3c is formed by PO4Tetrahedron and 4 TiO6Octahedrally connected, each TiO6Octahedron and 6 PO4Since tetrahedra are connected and have a three-dimensional crystal structure and an ion transport channel open along the c-axis, the ion conductivity is high and the structure is stable, but the electron conductivity is low, and modification of the tetrahedra is required to obtain LiTi having excellent electrochemical properties2(PO4)3。
The conventional high-temperature solid phase method is generally used for preparing LiTi2(PO4)3But the particle size of the product is not easy to control, the distribution is not uniform, the appearance is irregular, and the like. And LiTi2(PO4)3Low electron conductivity, and the requirement for LiTi2(PO4)3The modification is carried out by mainly carrying out carbon coating, element doping and the like. The proper carbon coating layer can improve the electronic conductivity of the material and improve the capacity attenuation of the material under high multiplying power.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of a carbon-coated lithium titanium phosphate cathode material, and the invention adopts a sol-gel method to prepare LiTi2(PO4)3To distribute the productUniform and small particles.
The technical scheme of the invention is as follows: a preparation method of a carbon-coated lithium titanium phosphate negative electrode material comprises the following steps:
s1), mixing Ti (OC)4H9)4Dropwise adding into anhydrous ethanol while stirring, and adding Li2CO3；
S2), adding NH4H2PO4And C6H8O7Dissolving in appropriate amount of distilled water, respectively, and pouring the prepared solution into the solution obtained in step S1);
s3), then transferring the mixed solution into a water bath, stirring for 10-15 hours at 60-100 ℃ to obtain gel, then transferring the gel into a vacuum drying oven, and drying for 10-15 hours at 70-90 ℃ to obtain dry gel;
s4), transferring the dried gel into a tubular furnace, and calcining for 8 hours at 800 ℃ in an air atmosphere to obtain blocky LiTi2(PO4)3；
S5), prepared LiTi2(PO4)3Uniformly grinding, moving to a ball milling tank, and carrying out ball milling for 3 hours to obtain powdery LiTi2(PO4)3；
S6, dissolving beta-cyclodextrin in distilled water and heating to accelerate the dissolution, and then mixing with LiTi2(PO4)3Mixing uniformly;
s7), finally, the mixture obtained in the above process is dried in vacuum and calcined in a tube furnace under the protection of flowing argon atmosphere at the temperature of 700-900 ℃ for 1-3 hours to obtain black LiTi2(PO4)3the/C composite negative electrode material.
Preferably, said Li2CO3、Ti(OC4H9)4、NH4H2PO4The molar ratio of Li to Ti to P is 1:2: 3.
Preferably, in step S6), the mass percentage of the β -cyclodextrin is 2 wt.% to 11 wt.%.
The invention has the beneficial effects that:
1. the invention adopts a sol-gel method to synthesize LiTi2(PO4)3The prepared material particles are uniformly distributed and have regular shapes;
2. the invention uses LiTi2(PO4)3The carbon layer is coated on the surface of the negative electrode material, so that the electronic conductivity and the lithium ion diffusion coefficient of the negative electrode material are improved, and the high-rate charge and discharge performance is improved.
Drawings
FIG. 1 is an XRD pattern of carbon-coated lithium titanium phosphate anode materials prepared in examples 1-5 of the present invention;
FIG. 2 is an SEM image of a carbon-coated lithium titanium phosphate anode material prepared in example 2 of the present invention;
FIG. 3 is an SEM image of a carbon-coated lithium titanium phosphate anode material prepared in example 3 of the present invention;
FIG. 4 is an SEM image of a carbon-coated lithium titanium phosphate anode material prepared in example 4 of the present invention;
FIG. 5 is an SEM image of a carbon-coated lithium titanium phosphate anode material prepared in example 5 of the present invention;
FIG. 6 is a TEM image of a carbon-coated lithium titanium phosphate anode material prepared in example 4 of the present invention;
FIG. 7 is a graph of rate capability of carbon-coated lithium titanium phosphate negative electrode materials prepared in examples 1-5 of the present invention;
fig. 8 is a graph of the cycle performance at 0.2C rate for carbon-coated lithium titanium phosphate negative electrode materials prepared in examples 2-5 of the present invention.
Detailed Description
The following further describes embodiments of the present invention with reference to the accompanying drawings:
example 1
This example provides a method for preparing a lithium titanium phosphate anode material without carbon coating, and as a comparative example, the example specifically includes the following steps:
s1), mixing Ti (OC)4H9)4Dropwise adding into anhydrous ethanol while stirring, and adding Li2CO3；
S2) Reacting NH4H2PO4And C6H8O7Dissolving in appropriate amount of distilled water, respectively, and pouring the prepared solution into the solution of step S1), wherein Li is added2CO3、Ti(OC4H9)4、NH4H2PO4Mixing according to the molar ratio of Li to Ti to P being 1 to 2 to 3;
s3), then transferring the mixed solution into a water bath, stirring for 12 hours at 80 ℃ to obtain gel, then transferring the gel into a vacuum drying oven, and drying for 12 hours at 80 ℃ to obtain dried gel;
s4), transferring the dried gel into a tubular furnace, and calcining for 8 hours at 800 ℃ in an air atmosphere to obtain blocky LiTi2(PO4)3；
S5), prepared LiTi2(PO4)3Uniformly grinding, moving to a ball milling tank, and carrying out ball milling for 3 hours to obtain powdery LiTi2(PO4)3And is denoted as pure-LTP.
Example 2
The embodiment provides a preparation method of a carbon-coated lithium titanium phosphate negative electrode material, which comprises the following steps:
s1), mixing Ti (OC)4H9)4Dropwise adding into anhydrous ethanol while stirring, and adding Li2CO3；
S2), adding NH4H2PO4And C6H8O7Dissolving in appropriate amount of distilled water, respectively, and pouring the prepared solution into the solution of step S1), wherein Li is added2CO3、Ti(OC4H9)4、NH4H2PO4Mixing according to the molar ratio of Li to Ti to P being 1 to 2 to 3;
s3), then transferring the mixed solution into a water bath, stirring for 12 hours at 80 ℃ to obtain gel, then transferring the gel into a vacuum drying oven, and drying for 12 hours at 80 ℃ to obtain dried gel;
s4), transferring the dried gel into a tube furnace, and calcining at 800 ℃ in an air atmosphereFiring for 8 hours to obtain massive LiTi2(PO4)3；
S5), prepared LiTi2(PO4)3Uniformly grinding, moving to a ball milling tank, and carrying out ball milling for 3 hours to obtain powdery LiTi2(PO4)3，
S6), dissolving 2 wt.% beta-cyclodextrin in distilled water and heating to accelerate the dissolution, followed by mixing with LiTi2(PO4)3Mixing uniformly;
s7), finally, the mixture obtained in the above process is dried in vacuum and calcined in a tube furnace for 1-3 hours at 800 ℃ under the protection of flowing argon atmosphere to obtain black LiTi2(PO4)3An SEM image of the carbon-coated lithium titanium phosphate anode material prepared in the example is shown in FIG. 2, and the/C composite anode material is marked as LTP-1.
Example 3
The embodiment provides a preparation method of a carbon-coated lithium titanium phosphate negative electrode material, which comprises the following steps:
s1), mixing Ti (OC)4H9)4Dropwise adding into anhydrous ethanol while stirring, and adding Li2CO3；
S2), adding NH4H2PO4And C6H8O7Dissolving in appropriate amount of distilled water, respectively, and pouring the prepared solution into the solution of step S1), wherein Li is added2CO3、Ti(OC4H9)4、NH4H2PO4Mixing according to the molar ratio of Li to Ti to P being 1 to 2 to 3;
s3), then transferring the mixed solution into a water bath, stirring for 12 hours at 80 ℃ to obtain gel, then transferring the gel into a vacuum drying oven, and drying for 12 hours at 80 ℃ to obtain dried gel;
s4), transferring the dried gel into a tubular furnace, and calcining for 8 hours at 800 ℃ in an air atmosphere to obtain blocky LiTi2(PO4)3；
S5), prepared LiTi2(PO4)3Uniformly grinding, moving to a ball milling tank, and carrying out ball milling for 3 hours to obtain powdery LiTi2(PO4)3，
S6), dissolving 5 wt.% beta-cyclodextrin in distilled water and heating to accelerate the dissolution, followed by mixing with LiTi2(PO4)3Mixing uniformly;
s7), finally, the mixture obtained in the above process is dried in vacuum and calcined in a tube furnace for 1-3 hours at 800 ℃ under the protection of flowing argon atmosphere to obtain black LiTi2(PO4)3An SEM image of the carbon-coated lithium titanium phosphate anode material prepared in the example is shown in FIG. 3, and the/C composite anode material is marked as LTP-2.
Example 4
The embodiment provides a preparation method of a carbon-coated lithium titanium phosphate negative electrode material, which comprises the following steps:
s1), mixing Ti (OC)4H9)4Dropwise adding into anhydrous ethanol while stirring, and adding Li2CO3；
S2), adding NH4H2PO4And C6H8O7Dissolving in appropriate amount of distilled water, respectively, and pouring the prepared solution into the solution of step S1), wherein Li is added2CO3、Ti(OC4H9)4、NH4H2PO4Mixing according to the molar ratio of Li to Ti to P being 1 to 2 to 3;
s3), then transferring the mixed solution into a water bath, stirring for 12 hours at 80 ℃ to obtain gel, then transferring the gel into a vacuum drying oven, and drying for 12 hours at 80 ℃ to obtain dried gel;
s4), transferring the dried gel into a tubular furnace, and calcining for 8 hours at 800 ℃ in an air atmosphere to obtain blocky LiTi2(PO4)3；
S5), prepared LiTi2(PO4)3Uniformly grinding, moving to a ball milling tank, and carrying out ball milling for 3 hours to obtain powdery LiTi2(PO4)3，
S6), dissolving 8 wt.% beta-cyclodextrin in distilled water and heating to accelerate the dissolution, followed by mixing with LiTi2(PO4)3Mixing uniformly;
s7), finally, the mixture obtained in the above process is dried in vacuum and calcined in a tube furnace for 1-3 hours at 800 ℃ under the protection of flowing argon atmosphere to obtain black LiTi2(PO4)3the/C composite negative electrode material is marked as LTP-3, the SEM image of the carbon-coated lithium titanium phosphate negative electrode material prepared in the embodiment is shown in FIG. 4, the TEM image of the carbon-coated lithium titanium phosphate negative electrode material prepared in the embodiment is shown in FIG. 6, and LiTi is observed in the high-resolution transmission electron microscope image of FIG. 62(PO4)3The surface is coated with a carbon layer with the thickness of about 5nm, which shows that the proper amount of carbon coating can improve the LiTi2(PO4)3The conductivity of the lithium titanium phosphate anode material is improved, and the active material is protected from reacting with HF in the electrolyte, so that the carbon-coated lithium titanium phosphate anode material prepared by the embodiment has the advantages of optimal electrochemical performance, more uniform particles and optimal performance.
Example 5
The embodiment provides a preparation method of a carbon-coated lithium titanium phosphate negative electrode material, which comprises the following steps:
s1), mixing Ti (OC)4H9)4Dropwise adding into anhydrous ethanol while stirring, and adding Li2CO3；
S2), adding NH4H2PO4And C6H8O7Dissolving in appropriate amount of distilled water, respectively, and pouring the prepared solution into the solution of step S1), wherein Li is added2CO3、Ti(OC4H9)4、NH4H2PO4Mixing according to the molar ratio of Li to Ti to P being 1 to 2 to 3;
s3), then transferring the mixed solution into a water bath, stirring for 12 hours at 80 ℃ to obtain gel, then transferring the gel into a vacuum drying oven, and drying for 12 hours at 80 ℃ to obtain dried gel;
s4), transferring the dried gel into a tubular furnace, and calcining for 8 hours at 800 ℃ in an air atmosphere to obtain blocky LiTi2(PO4)3；
S5), prepared LiTi2(PO4)3Uniformly grinding, moving to a ball milling tank, and carrying out ball milling for 3 hours to obtain powdery LiTi2(PO4)3，
S6), dissolving 11 wt.% beta-cyclodextrin in distilled water and heating to accelerate the dissolution, followed by mixing with LiTi2(PO4)3Mixing uniformly;
s7), finally, the mixture obtained in the above process is dried in vacuum and calcined in a tube furnace for 1-3 hours at 800 ℃ under the protection of flowing argon atmosphere to obtain black LiTi2(PO4)3An SEM image of the carbon-coated lithium titanium phosphate anode material prepared in this example is shown in FIG. 5, which is recorded as LTP-4.
FIG. 1 is an XRD pattern of the negative electrode materials prepared in examples 1 to 5, and carbon-uncoated LiTi prepared by a sol-gel method2(PO4)3And subsequently carbon coated LiTi2(PO4)3All have no hetero-peak and are pure-phase LiTi2(PO4)3Materials showing preparation of pure phase LiTi by sol-gel method2(PO4)3. All diffraction peaks in the figure are sharp, indicating that the prepared LiTi2(PO4)3The crystallinity is good. In addition, for all LiTi2(PO4)3No diffraction peak of carbon was observed for the/C composite anode material, indicating that the coated carbon content was low or that carbon was present in the form of amorphous carbon.
As can be seen from the SEM images of fig. 2, 3, and 5, there is a large particle generation, indicating that the lithium titanium phosphate undergoes agglomeration or melting behavior during calcination and carbonization in step S7). While the particles shown in fig. 4 are small and dispersed, it is indicated that no agglomeration or melting behavior occurs in the calcination carbonization in step S7) in example 4, which may be because the amount of the added β -cyclodextrin is proper, and no agglomeration or melting behavior occurs due to the synergistic effect between the β -cyclodextrin and the raw material, so that the obtained carbon-coated lithium titanium phosphate material is relatively dispersed particles, and thus the electrochemical performance of the carbon-coated lithium titanium phosphate anode material prepared in example 4 is optimal.
FIG. 7 is a graph showing rate characteristics of the negative electrode materials prepared in examples 1 to 5, and it can be seen from FIG. 7 that the discharge capacities of the negative electrode materials prepared in examples 1 to 5 all show different degrees of deterioration with increase in charge and discharge rate, i.e., with increase in current, but the deterioration of the material not coated with carbon is the greatest, indicating that the deterioration is at LiTi2(PO4)3The carbon coating of the material can improve the performance.
The electrochemical performance of the carbon-coated lithium titanium phosphate negative electrode material prepared in example 4 is optimal, which indicates that an appropriate carbon coating amount (or the addition amount of β -cyclodextrin) is provided, and the performance of the material is reduced due to too little or too much carbon coating amount, so that the electrochemical performance of the material can be better improved by a proper amount of carbon coating amount, and the discharge capacity of the material is improved.
FIG. 8 is a graph of cycle performance at 0.2C rate for negative electrode materials prepared in examples 2 to 5, from which it can be seen that for different coating amounts of LiTi2(PO4)3the/C composite material was cycled 50 times at 0.2C rate, wherein the discharge capacity of example 4 was the highest and the capacity retention rate was also higher, so the amount of added beta-cyclodextrin was LiTi of 8 wt.%2(PO4)3The electrochemical performance of the/C composite negative electrode material is optimal.
The foregoing embodiments and description have been presented only to illustrate the principles and preferred embodiments of the invention, and various changes and modifications may be made therein without departing from the spirit and scope of the invention as hereinafter claimed.

Claims (3)

1. A preparation method of a carbon-coated lithium titanium phosphate negative electrode material is characterized by comprising the following steps:
s1), mixing Ti (OC)4H9)4Dropwise adding into anhydrous ethanol while stirring, and adding Li2CO3；
S2), adding NH4H2PO4And C6H8O7Dissolving in appropriate amount of distilled water, respectively, and pouring the prepared solution into the solution obtained in step S1) to obtain corresponding mixed solution;
s3), then transferring the mixed solution into a water bath, stirring for 10-15 hours at 60-100 ℃ to obtain gel, then transferring the gel into a vacuum drying oven, and drying for 10-15 hours at 70-90 ℃ to obtain dry gel;
s4), transferring the dried gel into a tubular furnace, and calcining for 8 hours at 800 ℃ in an air atmosphere to obtain blocky LiTi2(PO4)3；
S5), prepared LiTi2(PO4)3Uniformly grinding, moving to a ball milling tank, and carrying out ball milling for 3 hours to obtain powdery LiTi2(PO4)3；
S6, dissolving beta-cyclodextrin in distilled water and heating to accelerate the dissolution, and then mixing with LiTi2(PO4)3Mixing uniformly;
s7), finally, the mixture obtained in the above process is dried in vacuum and calcined in a tube furnace under the protection of flowing argon atmosphere at the temperature of 700-900 ℃ for 1-3 hours to obtain black LiTi2(PO4)3the/C composite negative electrode material.
2. The method for preparing a carbon-coated lithium titanium phosphate anode material according to claim 1, wherein the method comprises the following steps: said Li2CO3、Ti(OC4H9)4、NH4H2PO4The molar ratio of Li to Ti to P is 1:2: 3.
3. The method for preparing a carbon-coated lithium titanium phosphate anode material according to claim 1, wherein the method comprises the following steps: in step S6), the mass percent of the beta-cyclodextrin is 2 wt.% to 11 wt.%.
CN202010816170.2A 2020-08-14 2020-08-14 Preparation method of carbon-coated lithium titanium phosphate negative electrode material Pending CN111952563A (en)

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CN113707877A (en) * 2021-08-23 2021-11-26 湖州南木纳米科技有限公司 Surface modified titanium magnesium phosphate material and preparation method and application thereof
CN114335514A (en) * 2021-11-29 2022-04-12 台州闪能科技有限公司 Nano lithium titanium phosphate @ carbon nanotube composite material and preparation method thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113707877A (en) * 2021-08-23 2021-11-26 湖州南木纳米科技有限公司 Surface modified titanium magnesium phosphate material and preparation method and application thereof
CN114335514A (en) * 2021-11-29 2022-04-12 台州闪能科技有限公司 Nano lithium titanium phosphate @ carbon nanotube composite material and preparation method thereof
CN114335514B (en) * 2021-11-29 2023-07-11 台州闪能科技有限公司 Nano titanium lithium phosphate@carbon nano tube composite material and preparation method thereof

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Application publication date: 20201117