CN115321509B - Solid electrolyte lithium titanium aluminum phosphate and preparation method thereof - Google Patents
Solid electrolyte lithium titanium aluminum phosphate and preparation method thereof Download PDFInfo
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- CN115321509B CN115321509B CN202211263737.3A CN202211263737A CN115321509B CN 115321509 B CN115321509 B CN 115321509B CN 202211263737 A CN202211263737 A CN 202211263737A CN 115321509 B CN115321509 B CN 115321509B
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A solid electrolyte lithium aluminum titanium phosphate and a preparation method thereof, the method comprises the following steps: a precursor preparation step, mixing a titanium source and a phosphorus source, and sintering to obtain a precursor; a mixing step, mixing the precursor, a lithium source and an aluminum source to obtain a mixture; and a sintering step, sintering the mixture to obtain a product. The method comprises the steps of mixing and sintering a titanium source and a phosphorus source in advance to obtain a precursor, mixing the precursor with a lithium source and an aluminum source, and then sintering in a solid phase to obtain the titanium aluminum lithium phosphate.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a solid electrolyte lithium titanium aluminum phosphate and a preparation method thereof.
Background
The lithium ion battery has the advantages of high energy density, good cycle performance, high working voltage, no memory effect and the like, and is widely applied to the fields of 3C digital codes, power and energy storage. Because the traditional lithium ion battery uses the liquid electrolyte which is easy to burn, the safety problems such as fire or explosion and the like easily occur in the using process. The solid electrolyte has the advantages of non-inflammability, high thermal stability, high mechanical strength and the like, and can greatly improve the safety performance of the lithium ion battery by replacing the traditional liquid electrolyte.
Solid electrolytes are classified into three major classes, i.e., polymer electrolytes, sulfide electrolytes, and oxide electrolytes, among which lithium aluminum titanium phosphate (Li) 1+x Al x Ti 2-x (PO 4 ) 3 LATP) has the advantages of high ionic conductivity, good chemical stability and thermal stability, low manufacturing cost, and the like, and is a solid electrolyte having the most industrial prospect.
The existing preparation method of the lithium aluminum titanium phosphate comprises a sol-gel method and a solid-phase sintering method, and has a plurality of defects.
The sol-gel method mainly has the following defects: 1) The adopted titanium source is generally titanium tetrachloride, which is very easy to react with moisture in the air to generate HCl acid mist which is harmful to human bodies and the environment; or tetrabutyl titanate is used, the raw material is high in price and cost, the raw material is very easy to react with moisture in the air, the storage is difficult, the raw material is flammable, and potential safety hazards exist. 2) Organic solvents harmful to the human body, such as ethylene glycol, need to be used. 3) The water solvent and the organic solvent need to be removed by heating, and the energy consumption is high. 4) The process is relatively complicated.
The solid-phase sintering method mainly has the following defects: the preparation method generally uses a plurality of raw materials such as lithium sources, titanium sources, aluminum sources, phosphorus sources and the like, and the raw materials are various, have large specific gravity difference and large particle size difference, and are easy to cause uneven mixing, so that the purity of the prepared lithium aluminum titanium phosphate is not high.
Disclosure of Invention
According to a first aspect, in an embodiment, there is provided a method of preparing a solid electrolyte lithium titanium aluminum phosphate, comprising:
a precursor preparation step, which comprises mixing a titanium source and a phosphorus source, and sintering to obtain a precursor;
a mixing step, comprising mixing the precursor, a lithium source and an aluminum source to obtain a mixture;
and a sintering step, which comprises sintering the mixture to obtain a product.
According to a second aspect, in an embodimentIn an embodiment, a solid electrolyte lithium aluminum titanium phosphate is provided, comprising the following formula: li 1+x Al x Ti 2-x (PO 4 ) 3 ，x=0.2~0.6。
According to the solid electrolyte lithium titanium aluminum phosphate and the preparation method thereof in the embodiment, firstly, a titanium source and a phosphorus source are mixed and sintered in advance to obtain a precursor, then the precursor is mixed with a lithium source and an aluminum source, and then the solid phase sintering is carried out to obtain the lithium titanium aluminum phosphate.
Drawings
FIG. 1 is a process flow diagram of an embodiment;
FIG. 2 is a solid electrolyte of titanium aluminum lithium phosphate Li of example 1 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 XRD pattern of (a);
FIG. 3 is a solid electrolyte of titanium aluminum lithium phosphate Li of example 2 1.4 Al 0.4 Ti 1.6 (PO 4 ) 3 XRD pattern of (a);
FIG. 4 is a solid electrolyte of titanium aluminum lithium phosphate Li of example 3 1.5 Al 0.5 Ti 1.5 (PO 4 ) 3 XRD pattern of (a);
FIG. 5 is a solid electrolyte of titanium aluminum lithium phosphate Li of example 4 1.6 Al 0.6 Ti 1.4 (PO 4 ) 3 XRD pattern of (a);
FIG. 6 is a solid electrolyte lithium aluminum titanium phosphate Li of comparative example 1 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 XRD pattern of (a).
Detailed Description
The present invention will be described in further detail with reference to the following detailed description and accompanying drawings. In the following description, numerous specific details are set forth in order to provide a better understanding of the present application. However, those skilled in the art will readily recognize that some of the features may be omitted in different instances or may be replaced by other materials, methods. In some instances, certain operations related to the present application have not been shown or described in detail in order to avoid obscuring the core of the present application from excessive description, and it is not necessary for those skilled in the art to describe these operations in detail, so that they may be fully understood from the description in the specification and the general knowledge in the art.
Furthermore, the features, operations, or characteristics described in the specification may be combined in any suitable manner to form various embodiments. Also, the various steps or actions in the method descriptions may be transposed or transposed in order, as will be apparent to one of ordinary skill in the art. Thus, the various sequences in the specification and drawings are for the purpose of describing certain embodiments only and are not intended to imply a required sequence unless otherwise indicated where such sequence must be followed.
The numbering of the components as such, e.g., "first", "second", etc., is used herein only to distinguish the objects as described, and does not have any sequential or technical meaning.
According to a first aspect, in an embodiment, there is provided a method of preparing a solid electrolyte lithium titanium aluminium phosphate, comprising:
a precursor preparation step, which comprises mixing a titanium source and a phosphorus source, and sintering to obtain a precursor;
a mixing step, comprising mixing the precursor, a lithium source and an aluminum source to obtain a mixture;
and a sintering step, which comprises sintering the mixture to obtain a product.
In an embodiment, in the precursor preparation step, the titanium source includes, but is not limited to, at least one of titanium dioxide, titanium hydroxide, metatitanic acid, and titanyl sulfate.
In an embodiment, in the precursor preparation step, the phosphorus source includes, but is not limited to, at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate, and ammonium phosphate.
In one embodiment, in the precursor preparation step, the sintering temperature is 300 to 600 ℃.
In one embodiment, in the precursor preparation step, the sintering time is 2 to 6h.
In one embodiment, in the precursor preparation step, the sintering is performed in air.
In one embodiment, in the precursor preparation step, the titanium source and the phosphorus source are mixed according to a molar ratio of Ti: P =1 (2~3).
In an embodiment, in the precursor preparation step, the product obtained by sintering is pulverized to obtain the precursor.
In an embodiment, in the precursor preparation step, the titanium source and the phosphorus source are both powders.
In one embodiment, in the mixing step, the lithium source includes, but is not limited to, at least one of lithium carbonate, lithium hydroxide, lithium nitrate, lithium oxalate, lithium sulfate, lithium phosphate, and lithium dihydrogen phosphate.
In one embodiment, the aluminum source in the mixing step includes, but is not limited to, at least one of alumina, hydrated alumina, aluminum hydroxide, aluminum phosphate, aluminum metaphosphate, and aluminum isopropoxide.
In one embodiment, in the mixing step, the mixing is dry mixing, and no solvent is added to the mixing system.
In one embodiment, the sintering temperature in the sintering step is 750 to 950 ℃.
In one embodiment, in the sintering step, the sintering time is 6 to 14h.
In one embodiment, the precursor, the lithium source and the aluminum source are mixed in a molar ratio of Li: al: ti = (1+x): x (2-x), x =0.2 to 0.6 in the sintering step.
In an embodiment, the sintering step further includes crushing, removing iron, and sieving the product obtained by sintering to obtain the final product.
According to a second aspect, in one embodiment, there is provided a solid electrolyte lithium titanium aluminum phosphate comprising the formula: li 1+x Al x Ti 2-x (PO 4 ) 3 ，x=0.2~0.6。
In an embodiment, the solid electrolyte lithium titanium aluminum phosphate is prepared by the method of any one of the first aspect.
In one embodiment, the invention provides a method for preparing high-purity solid electrolyte lithium titanium aluminum phosphate, which overcomes the problem that the purity of the prepared lithium titanium aluminum phosphate is not high due to uneven mixing of raw materials in a solid phase sintering method.
In one embodiment, as shown in fig. 1, the solution of the present invention comprises: firstly, a precursor TiP is obtained by adopting a titanium source and a phosphorus source to be mixed and sintered 2 O 7 And mixing the precursor with a lithium source and an aluminum source, and finally performing solid-phase sintering to obtain the high-purity lithium aluminum titanium phosphate.
In one embodiment, the invention solves the problem that the purity of the prepared lithium aluminum titanium phosphate is not high due to nonuniform mixing caused by multiple raw materials, large specific gravity difference and large particle size difference in a solid-phase sintering method.
In one embodiment, the invention does not need to use water solvent, organic solvent and other liquids, does not generate waste liquid, and is environment-friendly; the solvent is removed without heating, and the energy consumption is low.
In one embodiment, the process flow of the invention is short and the manufacturing cost is low.
In one embodiment, the preparation method of the high-purity solid electrolyte lithium titanium aluminum phosphate provided by the invention comprises the following steps:
1) Respectively weighing a certain amount of titanium source and a certain amount of phosphorus source according to the molar ratio of Ti to P =1 (2~3), and obtaining a mixture by adopting a dry mixing process. The mixing process does not employ any solvent.
A titanium source: titanium dioxide (TiO) 2 ) Titanium hydroxide [ Ti (OH) 4 ]Metatitanic acid [ TiO (OH) 2 ]Titanyl sulfate (TiOSO) 4 ) The raw material is powder.
A phosphorus source: at least one of ammonium dihydrogen phosphate, diammonium hydrogen phosphate and ammonium phosphate, wherein the raw materials are powder.
2) Heating a mixture of a titanium source and a phosphorus source in air to 300-600 ℃, sintering, keeping the temperature for 2-6 h, naturally cooling, and crushing to obtain precursor powder.
The precursor powder is: titanium pyrophosphate TiP 2 O 7 。
3) The precursor powder, the lithium source and the aluminum source are respectively weighed according to the molar ratio of Li to Al to Ti = (1+x) to x (2-x), and x =0.2 to 0.6, and are mixed by a dry mixing process.
A lithium source: lithium carbonate, lithium hydroxide, lithium nitrate, lithium oxalate, lithium sulfate, lithium phosphate, lithium dihydrogen phosphate.
An aluminum source: at least one of alumina, hydrated alumina, aluminum hydroxide, aluminum phosphate, aluminum metaphosphate, and aluminum isopropoxide.
And (3) dry mixing process: taking various raw material dry powders, and mixing the raw material dry powders by using mixing equipment such as a high-speed mixer, a ball mill, a ribbon mixer, a gravity-free mixer, a double-helix conical mixer and the like under the condition of not using a solvent.
4) Heating the mixture prepared in the step 3) in air to 750 to 950 ℃, preserving heat for 6 to 14h, then naturally cooling, crushing, removing iron and sieving to obtain the high-purity lithium aluminum titanium phosphate Li 1+x Al x Ti 2-x (PO 4 ) 3 。
Example 1
Weighing 159.73g of titanium dioxide and 596.35g of ammonium phosphate according to the molar ratio of Ti: P =1:2, mixing in a dry method, heating in air to 400 ℃, keeping the temperature for 6h, naturally cooling, and crushing the material to obtain precursor powder.
377.08g precursor powder, 48.02g lithium carbonate and 23.39g aluminum hydroxide are weighed and mixed by a dry method according to a molar ratio Li: al: ti =1.3 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 . FIG. 1 is an XRD pattern of a sample synthesized in example 1, diffraction peak positions of the sample, and LiTi 2 (PO 4 ) 3 The standard card of (1) is consistent with no diffraction peak of other substances, and the pure sample is indicatedHigh purity and no impurity.
Example 2
Weighing 231.73g of titanium hydroxide and 581.06g of diammonium hydrogen phosphate according to a molar ratio Ti: P =1 and 2.2, mixing by a dry method, heating in air to 480 ℃, preserving heat for 4 hours, naturally cooling, and crushing the materials to obtain precursor powder.
Weighing 354.90g precursor powder, 58.72g lithium hydroxide and 81.70g aluminum isopropoxide according to a molar ratio Li to Al to Ti =1.4 1.4 Al 0.4 Ti 1.6 (PO 4 ) 3 . FIG. 2 is an XRD pattern of the sample synthesized in example 2, the position of diffraction peak of the sample and LiTi 2 (PO 4 ) 3 The standard cards are consistent, no diffraction peaks of other substances exist, and the purity of the sample is high and no impurities exist.
Example 3
Weighing 195.74g metatitanic acid and 551.89g ammonium dihydrogen phosphate according to a molar ratio Ti: P =1 of 2.4, mixing by a dry method, heating in air to 430 ℃, preserving heat for 3h, naturally cooling, and crushing the materials to obtain precursor powder.
Weighing 332.72g of precursor powder, 76.43g of lithium oxalate and 50.98g of alumina according to a molar ratio of Li to Al to Ti =1.5 1.5 Al 0.5 Ti 1.5 (PO 4 ) 3 . FIG. 3 is an XRD pattern of the sample synthesized in example 3, the diffraction peak position of the sample and LiTi 2 (PO 4 ) 3 The standard cards are consistent, no diffraction peaks of other substances exist, and the purity of the sample is high and no impurities exist.
Example 4
Weighing 319.73g titanyl sulfate and 574.89g ammonium dihydrogen phosphate according to a molar ratio Ti: P =1, mixing by a dry method, heating in air to 500 ℃, preserving heat for 2h, naturally cooling, and crushing the material to obtain precursor powder.
Weighing 310.53g of precursor powder, 61.76g of lithium phosphate and 42.68g of hydrated alumina according to a molar ratio of Li to Al to Ti =1.6 1.6 Al 0.6 Ti 1.4 (PO 4 ) 3 . FIG. 4 is the XRD pattern of the sample synthesized in example 4, the position of diffraction peak and LiTi 2 (PO 4 ) 3 The standard card of (2) is consistent, no diffraction peak of other substances exists, and the purity of the sample is high and no impurities exist.
Comparative example 1
According to Li 1.3 Al 0.3 Ti 1.7 (PO 4 ) 3 48.20g lithium carbonate, 15.40g alumina, 136.99g titanium oxide and 348.31g ammonium dihydrogen phosphate are weighed according to the stoichiometric ratio respectively, mixed by a dry method, heated to 780 ℃ in air, kept warm for 14 hours, cooled naturally, crushed, deironized and sieved to obtain the solid electrolyte lithium titanium aluminum phosphate. The XRD pattern of this sample is shown in FIG. 6, with significant aluminum phosphate (AlPO) 4 ) And titanium pyrophosphate (TiP) 2 O 7 ) The characteristic peak of the mixed phase indicates that the impurity purity of the prepared lithium aluminum titanium phosphate is low. Therefore, the comparative example has the defects of uneven mixing due to multiple raw material types, large specific gravity difference and large particle size difference, and the purity of the prepared lithium aluminum titanium phosphate is not high.
The ionic conductivities of the solid electrolyte lithium titanium aluminum phosphate prepared in examples 1 and 2 are shown in table 1.
TABLE 1 Ionic conductivity
| Examples | Ion conductivity (S/cm) |
| Example 1 | 3.37*10 -4 |
| Example 2 | 4.78*10 -4 |
It can be seen that the solid electrolyte lithium titanium aluminum phosphate prepared in examples 1 and 2 has higher ionic conductivity.
In one embodiment, the method for preparing lithium aluminum titanium phosphate comprises two steps, wherein in the first step, a titanium source and a phosphorus source are mixed by a dry method, and then the mixture is subjected to solid-phase sintering to obtain a precursor TiP 2 O 7 . Second, the precursor TiP is added 2 O 7 Mixing with a lithium source and an aluminum source by a dry method, and then performing solid-phase sintering to obtain the solid electrolyte lithium aluminum titanium phosphate Li 1+x Al x Ti 2-x (PO 4 ) 3 。
In one embodiment, the invention solves the problem that the purity of the prepared solid electrolyte is low due to nonuniform mixing caused by multiple types of raw materials in the solid-phase sintering method.
In one embodiment, the mixing process disclosed by the invention adopts dry mixing, does not use any solvent, does not generate waste liquid, does not need to heat materials to remove the solvent, and is low in cost and environment-friendly.
The solid-phase sintering method is used for synthesizing the lithium titanium aluminum phosphate, the used raw materials comprise a lithium source, an aluminum source, a titanium source and a phosphorus source (and possibly additives), the types are various (more than or equal to 4), the particle size difference of different raw materials is large, and if dry-method mixing is adopted, the mixing is not uniform, so that the purity of the prepared lithium titanium aluminum phosphate is low. In one embodiment, the titanium source and the phosphorus source are mixed and sintered in advance to obtain a precursor, the precursor is mixed with the lithium source and the aluminum source, and then the mixture is sintered in a solid phase to obtain the titanium aluminum lithium phosphate.
The present invention has been described in terms of specific examples, which are provided to aid in understanding the invention and are not intended to be limiting. For a person skilled in the art to which the invention pertains, several simple deductions, modifications or substitutions may be made according to the idea of the invention.
Claims (9)
1. A method of preparing a solid electrolyte lithium titanium aluminum phosphate comprising:
a precursor preparation step, mixing a titanium source and a phosphorus source according to a molar ratio of Ti to P =1 (2~3), and sintering to obtain a precursor; the mixing is dry mixing, and no solvent is added in a mixing system;
a mixing step, mixing the precursor, a lithium source and an aluminum source to obtain a mixture; the mixing is dry mixing, and no solvent is added in a mixing system;
sintering, namely sintering the mixture to obtain a product; mixing the precursor, a lithium source and an aluminum source according to the molar ratio of Li to Al to Ti = (1+x) to x (2-x), wherein x =0.2 to 0.6; the prepared solid electrolyte lithium titanium aluminum phosphate has the following chemical formula: li 1+ x Al x Ti 2-x (PO 4 ) 3 ，x=0.2~0.6。
2. The method according to claim 1, wherein in the precursor preparation step, the titanium source is selected from at least one of titanium dioxide, titanium hydroxide, metatitanic acid, titanyl sulfate;
in the precursor preparation step, the phosphorus source is at least one selected from ammonium dihydrogen phosphate, diammonium hydrogen phosphate and ammonium phosphate.
3. The method according to claim 1, wherein in the precursor preparation step, the sintering temperature is 300 to 600 ℃;
in the precursor preparation step, the sintering time is 2 to 6h.
4. The method of claim 1, wherein in the precursor preparation step, the sintering is performed in air.
5. The method according to claim 1, wherein in the precursor preparation step, the product obtained by sintering is pulverized to obtain the precursor.
6. The method of claim 1, wherein in the precursor preparation step, the titanium source and the phosphorus source are both powders.
7. The method of claim 1, wherein in the mixing step, the lithium source is selected from at least one of lithium carbonate, lithium hydroxide, lithium nitrate, lithium oxalate, lithium sulfate, lithium phosphate, lithium dihydrogen phosphate;
in the mixing step, the aluminum source is at least one selected from the group consisting of aluminum oxide, hydrated aluminum oxide, aluminum hydroxide, aluminum phosphate, aluminum metaphosphate, and aluminum isopropoxide.
8. The method of claim 1, wherein in the sintering step, the sintering temperature is 750 to 950 ℃;
in the sintering step, the sintering time is 6 to 14h.
9. The method of claim 1, wherein the sintering step further comprises crushing, removing iron, and sieving the sintered product to obtain the final product.
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| WO2013156116A1 (en) * | 2012-04-19 | 2013-10-24 | Karlsruher Institut für Technologie | Method for producing li-ion conductive lithium aluminium titanium phosphates and use thereof as a solid-state electrolyte |
| CN107768631A (en) * | 2017-10-16 | 2018-03-06 | 桑顿新能源科技有限公司 | A kind of lithium-rich manganese base material for coating titanium phosphate aluminium lithium and preparation method thereof |
| CN109244428A (en) * | 2018-11-05 | 2019-01-18 | 桑顿新能源科技有限公司 | A kind of coating modification method of nickelic ternary material |
| CN110462912A (en) * | 2017-03-30 | 2019-11-15 | Tdk株式会社 | All-solid-state battery |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013156116A1 (en) * | 2012-04-19 | 2013-10-24 | Karlsruher Institut für Technologie | Method for producing li-ion conductive lithium aluminium titanium phosphates and use thereof as a solid-state electrolyte |
| CN110462912A (en) * | 2017-03-30 | 2019-11-15 | Tdk株式会社 | All-solid-state battery |
| CN107768631A (en) * | 2017-10-16 | 2018-03-06 | 桑顿新能源科技有限公司 | A kind of lithium-rich manganese base material for coating titanium phosphate aluminium lithium and preparation method thereof |
| CN109244428A (en) * | 2018-11-05 | 2019-01-18 | 桑顿新能源科技有限公司 | A kind of coating modification method of nickelic ternary material |
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