A method for manufacturing a solid electrolyte
The preparation of solid electrolytes through the ultra-gravity method solves the problems of bulky equipment, low efficiency and poor particle consistency in existing technologies, realizes the preparation of small-sized particles and improves battery performance, and is suitable for large-scale production.
Patent Information
- Application Number
- CN202411188035.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-28
- Publication Date
- 2025-09-09
- Estimated Expiration
- 2044-08-28
AI Technical Summary
The existing technology for preparing ceramic solid electrolytes has problems such as large equipment, low production efficiency, poor particle consistency, and high cost, and it is difficult to prepare nano-sized powder materials.
The ultra-gravity method is used to control crystal growth through an ultra-gravity reactor. The mixed reaction of lithium source, aluminum source, titanium source and phosphorus source is used, combined with aging, precipitation, drying and calcination treatment to prepare solid electrolyte particles less than 1 μm.
It improves production efficiency, reduces equipment requirements, achieves improved particle consistency and electrical performance, reduces energy consumption, and is suitable for large-scale production.
Smart Images

Figure CN118970157B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of lithium ion batteries, and in particular to a method for manufacturing a solid electrolyte. Background Art
[0002] Solid-state electrolytes are currently being widely researched as alternatives to liquid electrolytes in lithium-ion batteries. Among various material types, ceramic solid electrolytes offer higher safety than traditional lithium-ion batteries using electrolytes due to their non-flammability, excellent ionic conductivity at room temperature, and chemical stability.
[0003] As for solid-state electrolytes, considering oxidation stability, electrical conductivity and cost, lithium aluminum titanium phosphate (LATP) is currently a very promising solid-state electrolyte material because of its low cost, non-flammability, environmental friendliness, and good mechanical and chemical stability.
[0004] Common methods for synthesizing LATP include co-precipitation, solid-phase sintering, and sol-gel methods. Generally speaking, the co-precipitation method has disadvantages such as slow feed rates, low production efficiency, poor product consistency, bulky equipment, and a slow preparation process. The solid-phase sintering method, on the other hand, typically consumes high energy, takes a long reaction time, is prone to the formation of impurities, and is prone to uneven mixing. The resulting powder particles exhibit poor consistency and are large in size (typically greater than 10μm). This requires additional processing, such as mechanical ball milling or sand milling, increasing production costs. To obtain nanosized LATP powders, the sol-gel method is typically used. However, the sol-gel method requires the use of organic solvents such as ethanol and ethylene glycol, which increases the equipment requirements during the manufacturing process. Therefore, there is an urgent need for a better, more convenient method for producing solid-state electrolytes that can produce small particles. Summary of the Invention
[0005] The object of the present invention is to provide a method for manufacturing a solid electrolyte, comprising: dissolving a lithium source and an aluminum source in deionized water to obtain a first liquid; dissolving a titanium source and ammonia water in deionized water to obtain a second liquid; dissolving a phosphorus source in deionized water to obtain a third liquid; mixing the first liquid and the second liquid at a first flow rate to obtain a fourth liquid; mixing the third liquid and the fourth liquid at the first flow rate to obtain a fifth liquid; and processing the fifth liquid to obtain a solid electrolyte.
[0006] Preferably, the lithium source includes one or more compounds selected from the group consisting of lithium hydroxide (LiOH), lithium carbonate (Li2CO3), lithium acetate (C2H3LiO2), and lithium nitrate (LiNO3), and hydrates thereof; the aluminum source includes one or more compounds selected from the group consisting of aluminum oxide (Al2O3), aluminum nitrate nonahydrate (Al(NO3)3·9(H2O)), aluminum chloride (AlCl3), aluminum hydroxide (Al(OH)3), aluminum acetate (C6H9AlO6), and aluminum sulfate 18hydrate (Al2(SO4)3·18H2O), and hydrates thereof.
[0007] Preferably, the titanium source includes one or more of tetrabutyl titanate (Ti(C4H9O)4), titanium tetrachloride (TiCl4), titanium dichloride (TiCl2), titanate esters and their derivatives; the phosphorus source includes one or more of ammonium dihydrogen phosphate (NH4H2PO4), diammonium hydrogen phosphate ((NH4)2HPO4), and phosphoric acid (H3PO4).
[0008] Preferably, the first flow rate ranges from 0.1 L / min to 100 L / min.
[0009] Preferably, the first liquid and the second liquid are mixed at a rotation speed of 500 rpm to 5000 rpm to obtain the fourth liquid; and the third liquid and the fourth liquid are mixed at a rotation speed of 500 rpm to 5000 rpm to obtain the fifth liquid.
[0010] Preferably, the chemical formula of the solid electrolyte is Li 1+x Al x Ti 2-x (PO4)3, where 0<x<0.5.
[0011] Preferably, the first liquid and the second liquid flow into a supergravity reactor and are mixed in a supergravity manner to obtain the fourth liquid. The flow rate of the first liquid and the second liquid into the supergravity reactor is 0.1 L / min to 100 L / min. When synthesizing the fourth liquid, the rotation speed of the support inside the packing is 500 rpm to 5000 rpm, the reaction temperature is 80 to 100°C, and the pH value is 8 to 12.
[0012] Preferably, the third liquid and the fourth liquid flow into the supergravity reactor and are mixed in a supergravity manner to obtain the fifth liquid. The flow rate of the third liquid and the fourth liquid flowing into the supergravity reactor is 0.1L / min to 100L / min. When synthesizing the fifth liquid, the rotation speed of the support inside the packing is 500rpm to 5000rpm, and the reaction temperature is 80 to 100°C.
[0013] Preferably, the inner support of the filler of the high-gravity reactor is columnar or mesh-shaped.
[0014] Preferably, the treatment includes aging treatment, precipitation treatment, separation treatment, drying treatment, and calcination treatment. The aging treatment time of the fifth liquid is 6 to 18 hours, the aging treatment temperature of the fifth liquid is 80 to 100°C, the calcination treatment temperature of the fifth liquid is 700 to 950°C, the calcination treatment time of the fifth liquid is 4 to 10 hours, and the heating rate of the fifth liquid during the calcination treatment is 1 to 10°C / min.
[0015] The present invention proposes a method for preparing solid electrolytes using a supergravity method, which can reduce the demand for equipment in the production process and meet environmental protection requirements. The preparation method proposed in the present invention can effectively control the growth of crystals by controlling the support rotation speed of the filler in the supergravity reactor, thereby forming particles with a smaller initial size, and then obtaining a solid electrolyte with a smaller size (less than 1μm). Small-sized solid electrolytes will be able to effectively improve the electrical performance of lithium-ion batteries. In addition, the use of supergravity reactors to produce solid electrolytes can greatly increase the feed amount, thereby effectively increasing the reaction rate and reducing the size of the equipment. During the manufacturing process, the materials can be quickly and evenly mixed, increasing production efficiency and particle consistency. In addition, the energy consumption is low, the time is short, and the process is simple, which can meet the needs of large-scale production. BRIEF DESCRIPTION OF THE DRAWINGS
[0016] Figure 1 2 is a structural diagram of the high-gravity reactor used in an embodiment of the present invention.
[0017] Figure 2 Flowchart of a method for manufacturing a solid electrolyte according to an embodiment of the present invention.
[0018] Figure 3 The X-ray diffraction patterns of the solid electrolytes prepared in the examples and comparative examples of the present invention are shown. DETAILED DESCRIPTION
[0019] The following describes the specific embodiments of the present invention in detail with reference to the accompanying drawings. It should be understood that the specific embodiments described herein are only used to illustrate and explain the present invention and are not intended to limit the present invention.
[0020] The endpoints of the ranges and any values disclosed herein are not limited to the precise ranges or values, and these ranges or values should be understood to include values close to these ranges or values. For numerical ranges, the endpoints of each range, the endpoints of each range and individual point values, and the individual point values can be combined with each other to obtain one or more new numerical ranges, which should be considered to be specifically disclosed herein.
[0021] Please refer to Figure 1 , Figure 1 The following is a structural diagram of the high-gravity reactor used in an embodiment of the present invention. High-gravity reactor 100 comprises a chamber 1, a liquid conduit 2, internal packing supports 3, a rotating shaft 4, and a liquid outlet 5. The liquid conduit 2 enters the chamber 1 from above and connects to the internal packing supports 3 from below. The rotating shaft 4 enters the chamber 1 from below and connects to the internal packing supports 3. Rotation of the rotating shaft 4 drives the internal packing supports 3 to rotate. The liquid outlet 5 is located below the chamber 1, allowing the reacted liquid to be discharged from the chamber 1 through the liquid outlet 5.
[0022] This disclosure proposes a method for preparing a solid electrolyte using a high-gravity method, the steps of which are as follows.
[0023] Please refer to Figure 2 , Figure 2 This is a flow chart of a method for manufacturing a solid-state electrolyte according to an embodiment of the present invention. First, a lithium source and an aluminum source are dissolved in deionized water to obtain a first liquid. A titanium source and aqueous ammonia are dissolved in deionized water to slow the hydrolysis rate of the titanium source and obtain a second liquid. A phosphorus source is dissolved in deionized water to obtain a third liquid. The first and second liquids are mixed at a first flow rate to obtain a fourth liquid. The third and fourth liquids are mixed at the first flow rate to obtain a fifth liquid. The fifth liquid is then processed to obtain a solid-state electrolyte.
[0024] In the embodiments of this disclosure, the lithium source can be one or more compounds selected from lithium hydroxide (LiOH), lithium carbonate (Li2CO3), lithium acetate (C2H3LiO2), lithium nitrate (LiNO3), and their hydrates. The aluminum source can be one or more compounds selected from aluminum oxide (Al2O3), aluminum nitrate nonahydrate (Al(NO3)3·9(H2O)), aluminum nitrate (Al(NO3)3), aluminum chloride (AlCl3), aluminum hydroxide (Al(OH)3), aluminum acetate (C6H9AlO6), aluminum sulfate octahydrate (Al2(SO4)3·18H2O), and their hydrates. The titanium source can be one or more selected from tetrabutyl titanate (Ti(C4H9O)4), titanium tetrachloride (TiCl4), titanium dichloride (TiCl2), and titanate esters. The phosphorus source can be one or more selected from ammonium dihydrogen phosphate (NH4H2PO4), diammonium hydrogen phosphate ((NH4)2HPO4), and phosphoric acid (H3PO4). Preferably, the lithium source is lithium hydroxide, the aluminum source is aluminum nitrate, the titanium source is tetrabutyl titanate, and the phosphorus source is ammonium dihydrogen phosphate.
[0025] The high-gravity reactor 100 is started, and the rotational speed of the rotating shaft 4 is set. The rotation of the rotating shaft 4 drives the rotation of the support 3 within the packing. A pump is then used to flow the first and second liquids into the liquid conduit 2 through the opening of the liquid conduit 2 at a predetermined flow rate, rapidly mixing the first and second liquids within the chamber 1 to produce a fourth liquid. The mixed fourth liquid then flows out of the liquid outlet 5 at the bottom of the chamber 1.
[0026] In the embodiments of the present disclosure, the flow rate of the first liquid and the second liquid into the high-gravity reactor 100 is controlled at 0.1 L / min to 10 L / min, the rotation speed of the support 3 in the packing is controlled at 500 rpm to 5000 rpm, the reaction temperature in the cavity 1 is controlled at 80 to 100°C, and the pH value is controlled at 8 to 12.
[0027] Next, a pump is used to flow the third and fourth liquids into the liquid conduit 2 through the opening of the liquid conduit 2 at a preset flow rate, so that the third and fourth liquids are quickly mixed in the chamber 1 to obtain the fifth liquid. The mixed fifth liquid flows out of the liquid outlet 5 at the bottom of the chamber 1.
[0028] In the embodiments of this disclosure, the flow rate of the third liquid and the fourth liquid into the high-gravity reactor 100 is controlled at 0.1 L / min to 10 L / min, the rotation speed of the support 3 in the packing is controlled at 500 rpm to 5000 rpm, and the reaction temperature in the cavity 1 is controlled at 80 to 100°C.
[0029] The fifth liquid is then aged, and then subjected to precipitation, separation, drying, and finally calcination to obtain a solid electrolyte of lithium aluminum titanium phosphate (LATP). The molecular formula of the solid electrolyte is Li 1+x Al x Ti 2-x (PO4)3, where 0<x<0.5.
[0030] In the Examples of this disclosure, the aging treatment lasts for 6 to 18 hours at a temperature of 80 to 100° C. The calcination treatment lasts for 700 to 950° C. The heating rate of the fifth liquid during the calcination treatment is 1 to 10° C. / min, and the calcination treatment lasts for 4 to 10 hours.
[0031] In the embodiments of the present disclosure, the high-gravity reactor 100 can be vertical or horizontal, and the inner support 3 of the packing of the high-gravity reactor 100 can be columnar, mesh-shaped, or other types, but the present disclosure is not limited thereto.
[0032] The following examples illustrate the preparation method of the solid electrolyte disclosed in this disclosure.
[0033] Example 1:
[0034] (1) Dissolve 1.45 mol of lithium acetate and 0.3 mol of aluminum nitrate in 1 L of deionized water at a molar ratio of Li:Al = 1.45:0.3 to obtain the first liquid. Prepare 0.5 L of 0.5 mol / L ammonia solution and add 1.7 mol of tetrabutyl titanate to obtain the second liquid. Dissolve 3 mol of ammonium dihydrogen phosphate in 1 L of water to obtain the third liquid.
[0035] (2) The high-gravity reactor 100 was turned on, the rotation speed of the support 3 in the packing was set to 1500 rpm, and the first liquid and the second liquid were pumped into the high-gravity reactor 100 at a speed of 1 L / min by a peristaltic pump. The reaction temperature was controlled at 80°C and the pH value was controlled at 9. After the reaction was completed, the fourth liquid was obtained.
[0036] (3) The third liquid and the fourth liquid are pumped into the high-gravity reactor gas 100 at a speed of 1 L / min, and the support 3 in the packing rotates at a speed of 1500 rpm. After the reaction is completed, the fifth liquid is obtained.
[0037] (4) The fifth liquid is aged for 6 hours, and the aging temperature is controlled at 90°C.
[0038] (5) After aging, the filtered and separated precipitate was placed in a forced air oven at 80°C and dried for 12 hours to obtain an oxide solid electrolyte precursor.
[0039] (6) The oxide solid electrolyte precursor was placed in an alumina crucible, placed in a muffle furnace, heated at 3°C / min to 300°C, kept warm for 1 hour, then heated at 5°C / min to 700°C, kept warm for 4 hours, and the oxide solid electrolyte Li was obtained. 1.3 Al 0.3 Ti 1.7 (PO4)3.
[0040] Example 2:
[0041] (1) Dissolve 1.45 mol of lithium acetate and 0.3 mol of aluminum nitrate in 1 L of deionized water at a molar ratio of Li:Al = 1.45:0.3 to obtain the first liquid. Prepare 0.5 L of 0.5 mol / L ammonia solution and add 1.7 mol of tetrabutyl titanate to obtain the second liquid. Dissolve 3 mol of ammonium dihydrogen phosphate in 1 L of water to obtain the third liquid.
[0042] (2) The high-gravity reactor 100 was turned on, and the rotation speed of the support 3 in the packing was set to 2000 rpm. The first liquid and the second liquid were pumped into the high-gravity reactor 100 at a speed of 1.5 L / min by a peristaltic pump. The reaction temperature was controlled at 80°C and the pH value was controlled at 9. After the reaction was completed, the fourth liquid was obtained.
[0043] (3) The third liquid and the fourth liquid are pumped into the high-gravity reactor gas 100 at a speed of 1.5 L / min, and the support 3 in the packing rotates at a speed of 2000 rpm. After the reaction is completed, the fifth liquid is obtained.
[0044] (4) The fifth liquid is aged for 8 hours, and the aging temperature is controlled at 90°C.
[0045] (5) After aging, the filtered and separated precipitate was placed in a forced air oven at 80°C and dried for 12 hours to obtain an oxide solid electrolyte precursor.
[0046] (6) The oxide solid electrolyte precursor was placed in an alumina crucible, placed in a muffle furnace, heated at 3°C / min to 300°C, kept warm for 1 hour, then heated at 5°C / min to 700°C, kept warm for 4 hours, and the oxide solid electrolyte Li was obtained. 1.3 Al 0.3 Ti 1.7 (PO4)3.
[0047] Example 3:
[0048] (1) Dissolve 1.45 mol of lithium acetate and 0.3 mol of aluminum nitrate in 1 L of deionized water at a molar ratio of Li:Al = 1.45:0.3 to obtain the first liquid. Prepare 0.5 L of 0.5 mol / L ammonia solution and add 1.7 mol of tetrabutyl titanate to obtain the second liquid. Dissolve 3 mol of ammonium dihydrogen phosphate in 1 L of water to obtain the third liquid.
[0049] (2) The high-gravity reactor 100 was turned on, and the rotation speed of the support 3 in the packing was set to 3000 rpm. The first liquid and the second liquid were pumped into the high-gravity reactor 100 at a speed of 2 L / min by a peristaltic pump. The reaction temperature was controlled at 80°C and the pH value was controlled at 9. After the reaction was completed, the fourth liquid was obtained.
[0050] (3) The third liquid and the fourth liquid are pumped into the high-gravity reactor gas 100 at a speed of 2 L / min, and the support 3 in the packing rotates at a speed of 3000 rpm. After the reaction is completed, the fifth liquid is obtained.
[0051] (4) The fifth liquid is aged for 12 hours, and the aging temperature is controlled at 90°C.
[0052] (5) After aging, the filtered and separated precipitate was placed in a forced air oven at 80°C and dried for 12 hours to obtain an oxide solid electrolyte precursor.
[0053] (6) The oxide solid electrolyte precursor was placed in an alumina crucible, placed in a muffle furnace, heated at 3°C / min to 300°C, kept warm for 1 hour, then heated at 5°C / min to 700°C, kept warm for 4 hours, and the oxide solid electrolyte Li was obtained. 1.3 Al 0.3 Ti 1.7 (PO4)3.
[0054] Comparative Example 1:
[0055] (1) Dissolve 1.45 mol of lithium acetate and 0.3 mol of aluminum nitrate in 1 L of deionized water at a molar ratio of Li:Al = 1.45:0.3 to obtain the first liquid. Prepare 0.5 L of 0.5 mol / L ammonia solution and add 1.7 mol of tetrabutyl titanate to obtain the second liquid. Dissolve 3 mol of ammonium dihydrogen phosphate in 1 L of water to obtain the third liquid.
[0056] (2) The second liquid was pumped into the first liquid at a rate of 0.01 L / min using a peristaltic pump to mix, thereby obtaining a fourth liquid. The third liquid was pumped into the fourth liquid at a rate of 0.01 L / min using a peristaltic pump. The reaction temperature was controlled at 80°C, the pH value was controlled at 9, and the stirring and mixing rate was controlled at 400 rpm. After the reaction was completed, a fifth liquid was obtained.
[0057] (3) The fifth liquid is aged for 12 hours, and the aging temperature is controlled at 90°C.
[0058] (4) After aging, the filtered and separated precipitate was placed in an 80°C forced air oven and dried for 12 hours to obtain an oxide solid electrolyte precursor.
[0059] (5) The oxide solid electrolyte precursor was placed in an alumina crucible, placed in a muffle furnace, heated at 3°C / min to 300°C, kept warm for 1 hour, then heated at 5°C / min to 700°C, kept warm for 4 hours, and the oxide solid electrolyte Li was obtained. 1.3 Al 0.3 Ti 1.7 (PO4)3.
[0060] Comparative Example 2:
[0061] (1) Dissolve 1.45 mol of lithium acetate and 0.3 mol of aluminum nitrate in 1 L of deionized water at a molar ratio of Li:Al = 1.45:0.3 to obtain the first liquid. Prepare 0.5 L of 0.5 mol / L ammonia solution and add 1.7 mol of tetrabutyl titanate to obtain the second liquid. Dissolve 3 mol of ammonium dihydrogen phosphate in 1 L of water to obtain the third liquid.
[0062] (2) The second liquid was pumped into the first liquid at a rate of 1.5 L / min using a peristaltic pump to mix, thereby obtaining a fourth liquid. The third liquid was pumped into the fourth liquid at a rate of 1.5 L / min using a peristaltic pump. The reaction temperature was controlled at 80°C, the pH value was controlled at 9, and the stirring and mixing rate was controlled at 800 rpm. After the reaction was completed, a fifth liquid was obtained.
[0063] (3) The fifth liquid is aged for 12 hours, and the aging temperature is controlled at 90°C.
[0064] (4) After aging, the filtered and separated precipitate was placed in an 80°C forced air oven and dried for 12 hours to obtain an oxide solid electrolyte precursor.
[0065] (5) The oxide solid electrolyte precursor was placed in an alumina crucible, placed in a muffle furnace, heated at 3°C / min to 300°C, kept warm for 1 hour, then heated at 5°C / min to 700°C, kept warm for 4 hours, and the oxide solid electrolyte Li was obtained. 1.3 Al 0.3 Ti 1.7 (PO4)3.
[0066] Table 1 below presents experimental data for Examples 1 to 3 and Comparative Examples 1 and 2. Table 1 illustrates the effects of the rotational speed of support 3 within the packing and the feed rate on particle size. The smallest particle size was achieved when the rotational speed of support 3 within the packing was set to 2000 rpm and the feed rates of the first, second, third, and fourth liquids were 1.5 L / min.
[0067] Table 1
[0068]
[0069] Please refer to Figure 3 , Figure 3 The X-ray diffraction patterns of the solid electrolytes prepared in Examples 1, 2, 3 and Comparative Examples 1 and 2 are shown in FIG. Figure 3 It can be seen that the solid electrolytes prepared by the methods of Examples 1, 2, and 3 of this disclosure are pure NASICON phases, free of impurity phases, and have good crystallinity, while the solid electrolyte prepared in Comparative Example 2 contains impurity phases.
[0070] This disclosure proposes a method for preparing oxide solid electrolytes using a high-gravity reactor. The high-gravity environment increases the ion diffusion rate during the reaction, making the raw materials more evenly mixed and effectively ensuring that the raw materials are fully reacted, thereby obtaining high-quality, high-purity precursor crystals and reducing by-products. High-temperature calcination is then performed to obtain a high-purity LATP solid electrolyte. The overall preparation process does not require complex grinding and screening, and there is no need to control the heating rate during calcination. The entire preparation process is simple and low-cost. The manufacturing method proposed in this disclosure can significantly improve the purity of the solid electrolyte, and the resulting particle size distribution is uniform, overcoming the shortcomings of traditional preparation methods such as insufficient reaction, uneven reaction degree, and excessive by-products.
[0071] The above contents involving common knowledge are not described in detail and can be understood by those skilled in the art.
[0072] The above descriptions are merely specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention. The technical scope of the present invention is not limited to the contents of the specification and must be determined according to the scope of the claims.
Claims
1. A method for manufacturing a solid electrolyte, wherein the chemical formula of the solid electrolyte is Li 1+x Al x Ti 2-x (PO4)3,0<x<0.5, characterized in that include: Dissolving a lithium source and an aluminum source in deionized water to obtain a first liquid; The titanium source and ammonia are dissolved in deionized water to obtain a second liquid; Dissolving a phosphorus source in deionized water to obtain a third liquid; The first liquid and the second liquid flow into the high-gravity reactor and are mixed in a high-gravity manner to obtain a fourth liquid. The first liquid and the second liquid flow into the high-gravity reactor at a flow rate of 0.1 L / min to 100 L / min. When synthesizing the fourth liquid, the rotation speed of the support inside the packing of the high-gravity reactor is 1500 rpm to 5000 rpm; The third liquid and the fourth liquid flow into the high-gravity reactor and are mixed in a high-gravity manner to obtain a fifth liquid. The flow rate of the third liquid and the fourth liquid into the high-gravity reactor is 0.1 L / min to 100 L / min. When synthesizing the fifth liquid, the rotation speed of the support inside the packing of the high-gravity reactor is 1500 rpm to 5000 rpm; The solid electrolyte is obtained by processing the fifth liquid.
2. The method for manufacturing a solid electrolyte according to claim 1, wherein: The lithium source includes one or more compounds selected from lithium hydroxide (LiOH), lithium carbonate (Li2CO3), lithium acetate (C2H3LiO2), and lithium nitrate (LiNO3), and hydrates thereof; the aluminum source includes one or more compounds selected from aluminum oxide (Al2O3), aluminum nitrate nonahydrate (Al(NO3)3·9(H2O)), aluminum chloride (AlCl3), aluminum hydroxide (Al(OH)3), aluminum acetate (C6H9AlO6), and aluminum sulfate 18hydrate (Al2(SO4)3·18H2O), and hydrates thereof.
3. The method for manufacturing a solid electrolyte according to claim 1, wherein: The titanium source includes one or more of tetrabutyl titanate (Ti(C4H9O)4), titanium tetrachloride (TiCl4), titanium dichloride (TiCl2), titanate esters and their derivatives; the phosphorus source includes one or more of ammonium dihydrogen phosphate (NH4H2PO4), diammonium hydrogen phosphate ((NH4)2HPO4), and phosphoric acid (H3PO4).
4. The method for manufacturing a solid electrolyte according to claim 1, wherein: When synthesizing the fourth liquid, the reaction temperature of the high-gravity reactor is 80 to 100° C., and the pH value is 8 to 12.
5. The method for manufacturing a solid electrolyte according to claim 1, wherein: When synthesizing the fifth liquid, the reaction temperature of the high-gravity reactor is 80 to 100°C.
6. The method for manufacturing a solid electrolyte according to claim 1, wherein: The inner support of the filler of the high-gravity reactor is columnar or mesh-shaped.
7. The method for manufacturing a solid electrolyte according to claim 1, wherein: The treatment includes aging treatment, precipitation treatment, separation treatment, drying treatment, and calcination treatment. The aging treatment time of the fifth liquid is 6 to 18 hours, the aging treatment temperature of the fifth liquid is 80 to 100°C, the calcination treatment temperature of the fifth liquid is 700 to 950°C, the calcination treatment time of the fifth liquid is 4 to 10 hours, and the heating rate of the fifth liquid during the calcination treatment is 1 to 10°C / min.
Citation Information
Patent Citations
Lithium titanium aluminum phosphate solid electrolyte as well as preparation method and application thereof
CN114914528A