CN113506918B - Preparation method of inorganic solid electrolyte - Google Patents
Preparation method of inorganic solid electrolyte Download PDFInfo
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- CN113506918B CN113506918B CN202110778702.2A CN202110778702A CN113506918B CN 113506918 B CN113506918 B CN 113506918B CN 202110778702 A CN202110778702 A CN 202110778702A CN 113506918 B CN113506918 B CN 113506918B
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- 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
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- H—ELECTRICITY
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- 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
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Abstract
The invention relates to a preparation method of an inorganic solid electrolyte, belonging to the technical field of solid electrolytes. The preparation method of the inorganic solid electrolyte comprises the following steps: preparing a mixture of an inorganic solid electrolyte raw material and a solvent under an anaerobic condition, removing the solvent in the mixture to obtain mixed powder, and performing heat treatment on the mixed powder to obtain the electrolyte; the solvent contains one or any combination of methanol, acetonitrile, dioxolane, N-heptane, ethylene glycol dimethyl ether, dimethyl pyrrolidone, N-N dimethylformamide, acetone, cyclohexane, methyl ether and cyclohexane. According to the preparation method of the inorganic solid electrolyte, the raw materials of the inorganic solid electrolyte are subjected to nanocrystallization under the action of the solvent, and then are separated out again after drying, so that a new unit body can be quickly formed, the preparation time of the solid electrolyte is shortened, the heat treatment temperature is reduced, the heat treatment time is shortened, and the effects of energy conservation, emission reduction and cost saving can be achieved.
Description
Technical Field
The invention relates to a preparation method of an inorganic solid electrolyte, belonging to the technical field of solid electrolytes.
Background
The inorganic solid electrolyte is used for replacing a liquid organic electrolyte, so that the potential safety hazard of flammability of the conventional lithium battery is expected to be fundamentally solved, and the problem of formation of lithium dendrite between the electrolyte and a metal lithium electrode interface is solved.
At present, inorganic solid electrolyte systems containing Li, P, oxygen elements and halogen elements comprise electrolyte systems such as LGPS, germanium phosphate ore, inverse perovskite and the like, and the inorganic solid electrolytes are widely considered to have the most application prospect. However, most inorganic solid electrolyte systems need to completely isolate water and oxygen in the preparation process, often adopt long-time mechanical ball milling of precursors, and then undergo long-time heat treatment process, and the mechanical ball milling method needs to consume a large amount of energy and time, so that the mass production of solid electrolyte materials is difficult to realize.
Disclosure of Invention
The invention aims to provide a preparation method of an inorganic solid electrolyte, which is low in energy consumption and short in time consumption.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for preparing an inorganic solid electrolyte, comprising the steps of: preparing a mixture of an inorganic solid electrolyte raw material and a solvent under an anaerobic condition, removing the solvent in the mixture to obtain mixed powder, and performing heat treatment on the mixed powder to obtain the electrolyte; the solvent contains one or any combination of methanol, acetonitrile, dioxolane, N-heptane, ethylene glycol dimethyl ether, dimethyl pyrrolidone, N-N dimethylformamide, acetone, cyclohexane, methyl ether and cyclohexane.
The preparation method of the inorganic solid electrolyte has simple process, and the raw materials of the inorganic solid electrolyte are subjected to nanocrystallization under the action of the solvent and then are separated out again after drying, so that a new unit body can be quickly formed, the preparation time of the solid electrolyte can be shortened, the heat treatment temperature can be reduced, the heat treatment time can be shortened, the effects of energy conservation, emission reduction and cost saving can be achieved, the preparation method is compatible with the coating process of the traditional battery preparation, the large-scale industrial production of the inorganic solid electrolyte and the large-scale application of the inorganic solid electrolyte can be facilitated, and the preparation method has important significance for the large-scale production of the inorganic solid electrolyte. The structure and electrochemical performance of the inorganic solid electrolyte prepared by the method of the invention are similar to those of the materials obtained by the traditional solid phase method.
The preparation method of the inorganic solid electrolyte can be used for preparing one or any combination of crystal, vitreous body and amorphous inorganic solid electrolyte.
The solvent selected by the invention is an aprotic organic solvent, and has the following advantages: the solvent does not react with the inorganic solid electrolyte raw material, (b) is volatile, and (c) can partially or completely dissolve the inorganic solid electrolyte raw material.
It can be understood that the inorganic solid electrolyte raw material adopts the raw materials required when the inorganic solid electrolyte is prepared by the existing method. The mixture is obtained by mixing inorganic solid electrolyte raw materials and a solvent and then stirring the mixture to uniformly disperse the inorganic solid electrolyte raw materials in the solvent. The mixture is in the form of a stable suspension or a completely dissolved transparent solution.
Preferably, the inorganic solid electrolyte raw material comprises a raw material A and lithium halide;
the raw material A is selected from one or any combination of a raw material B, a raw material C and a raw material D; b is sulfur and/or lithium oxide, and the raw material C is P 2 O 5 And/or Li 3 PO 4 The raw material D is a combination of lithiated hydrogen and phosphorus; the lithium halide is selected from one or any combination of lithium chloride, lithium bromide and lithium iodide. Further preferably, the raw material A comprises one or any combination of B and C.
Preferably, the raw material A consists of a raw material B and a raw material C; the raw material B is lithium oxide. The raw material C can form a new unit body including P 2 O 7 4-- 、PO 4 3- And the like, which helps to shorten the preparation time of the inorganic solid electrolyte. For example, the raw material B is lithium oxide, the raw material C is lithium phosphate, and the molar ratio of the lithium oxide to the lithium phosphate to the lithium halide is 0.75-1.25. If the raw material A is lithium oxide, the molar ratio of the lithium oxide to the lithium halide is 1.
Preferably, the solvent in the mixture is removed by drying the mixed solvent in vacuum; the temperature of the vacuum drying is 55-65 ℃, and the time is 4-6h. For example, the temperature of the vacuum drying is 50 ℃ and the time is 5h.
Preferably, the temperature of the heat treatment is 230-580 ℃ and the time is 4-6h. The temperature of the heat treatment is preferably 350 to 580 ℃. The time of the heat treatment is preferably 5 hours.
When preparing the mixture, it is preferable that the volume of the solvent used is 6 to 10mL per 1g of the inorganic solid electrolyte raw material.
Drawings
FIG. 1 is an XRD pattern of the solid state electrolyte properties prepared in examples 1-4 of the present invention;
fig. 2 is an impedance spectrum of the solid electrolyte prepared in example 1 of the present invention;
FIG. 3 is an impedance diagram of a solid electrolyte prepared in examples 2 to 3 of the present invention;
fig. 4 is an impedance spectrum of the solid electrolyte prepared in example 4 of the present invention;
fig. 5 is an XRD contrast pattern of the inorganic solid electrolytes prepared in example 2 and comparative example.
Detailed Description
The technical solution of the present invention will be further described with reference to the following embodiments.
In the following examples and comparative preparation methods of inorganic solid electrolytes, all operations were performed in an argon, nitrogen or vacuum environment.
Example 1
The preparation method of the inorganic solid electrolyte of the embodiment includes the following steps:
1) Lithium oxide (Li) 2 O) powder, lithium chloride (LiCl) powder, lithium phosphate (Li) 3 PO 4 ) Respectively placing the powder, a clean sample bottle (10 mL) and a stirrer in a vacuum drying oven to dry for 24 hours under the vacuum condition;
2) Under the protection of argon atmosphere in a glove box, sucking 30mL of acetonitrile solution by using a suction pipe, dripping into a sample bottle with a stirrer, taking 3g of dried lithium oxide powder, lithium chloride powder and lithium phosphate powder according to the molar ratio of the lithium oxide to the lithium chloride to the lithium phosphate of 1;
3) Putting the liquid precursor in the sample bottle into a vacuum drying oven, and drying for 5 hours at 60 ℃ under a vacuum condition to obtain white powder;
4) Taking out the dried white powder, putting the white powder into a muffle furnace, and carrying out heat treatment for 5 hours at 580 ℃ in argon to obtain Li 6 PO 5 And Cl powder to obtain the catalyst.
Li prepared in this example 6 PO 5 The XRD pattern of the Cl solid electrolyte is shown in fig. 1, and the corresponding impedance pattern is shown in fig. 2.
Example 2
The preparation method of the inorganic solid electrolyte of the embodiment includes the following steps:
1) Lithium oxide (Li) 2 O) powder, lithium chloride (LiCl) powder, lithium phosphate (Li) 3 PO 4 ) Respectively putting the powder, a clean sample bottle (10 mL) and a stirrer in a vacuum drying oven to dry for 24h under a vacuum condition;
2) Under the protection of argon atmosphere in a glove box, sucking 30mL of acetonitrile solution by using a suction pipe, dripping the acetonitrile solution into a sample bottle with a stirrer, then respectively taking 3g of dried lithium oxide powder, lithium chloride powder and lithium phosphate powder according to the molar ratio of lithium oxide, lithium chloride and lithium phosphate being 5;
3) Placing the liquid precursor in the sample bottle in a vacuum drying oven, and drying for 5 hours at 60 ℃ under a vacuum condition to obtain white powder;
4) Taking out the dried white powder, putting the white powder into a muffle furnace, and carrying out heat treatment for 5 hours at 580 ℃ in a nitrogen atmosphere to obtain Li 6.25 PO 5.25 Cl 0.75 And (5) obtaining the powder.
Li prepared in this example 6.25 PO 5.25 Cl 0.75 The XRD spectrum of the solid electrolyte is shown in figure 1, the symmetry characteristics of the silver-germanium ore are still kept, the impedance spectrum is shown in figure 3, and the impedance ratio Li 6 PO 5 The Cl was reduced by 50%.
Example 3
The preparation method of the inorganic solid electrolyte of the embodiment includes the following steps:
1) Lithium oxide (Li) 2 O) powder, lithium chloride (LiCl) powder, lithium phosphate (Li) 3 PO 4 ) Powder, clean sample bottle (10 mL), stirrer, place separatelyDrying for 24h in a vacuum drying oven under vacuum condition;
2) Under the protection of argon atmosphere in a glove box, sucking 30mL of acetonitrile solution by using a suction pipe, dripping into a sample bottle with a stirrer, then respectively taking 3g of lithium oxide powder, lithium chloride powder and lithium phosphate powder according to the molar ratio of lithium oxide, lithium chloride and lithium phosphate being 3;
3) Putting the liquid precursor in the sample bottle into a vacuum drying oven, and drying for 5 hours at 60 ℃ under a vacuum condition to obtain white powder;
4) Taking out the dried white powder, putting the white powder into a muffle furnace, and carrying out heat treatment for 5 hours at 580 ℃ in a nitrogen atmosphere to obtain Li 5.75 PO 4.75 Cl 1.25 And (5) obtaining the powder.
Solid Li prepared in this example 5.75 PO 4.75 Cl 1.25 The XRD pattern of the electrolyte is shown in figure 1, and the impedance pattern is shown in figure 3. FIG. 3 shows that Li 5.75 PO 4.75 Cl 1.25 The ionic conductivity of (a) is higher.
Example 4
The preparation method of the inorganic solid electrolyte of the embodiment comprises the following steps:
1) Lithium oxide (Li) 2 O) powder, lithium chloride (LiCl) powder, a clean sample bottle (10 mL) and a stirrer are respectively placed in a vacuum drying oven to be dried for 24 hours under the vacuum condition;
2) Under the protection of argon atmosphere in a glove box, sucking 30mL of acetonitrile solution by using a suction pipe, dripping the acetonitrile solution into a sample bottle with a stirrer, then respectively taking 5g of dried lithium oxide powder and lithium chloride powder according to the molar ratio of lithium oxide to lithium chloride being 1, then slowly pouring the taken lithium oxide powder and lithium chloride powder into the sample bottle one by one in the process of continuously stirring the acetonitrile in the sample bottle, and transferring the sample bottle into a closed environment for stirring for 2-5h after the lithium oxide powder and the lithium chloride powder are completely added until the solution becomes a white transparent liquid precursor;
3) Putting the liquid precursor in the sample bottle into a vacuum drying oven, and drying for 5 hours at 60 ℃ under a vacuum condition to obtain white powder;
4) Taking out the dried white powder, putting the white powder into a muffle furnace, and carrying out heat treatment for 5 hours at 350 ℃ in a nitrogen atmosphere to obtain Li 3 And (5) obtaining the OCl powder.
Li prepared in this example 3 The XRD pattern of the OCl solid electrolyte is shown in figure 1, and the impedance pattern is shown in figure 4. As can be seen from FIG. 4, successfully synthesized Li 3 The OCl electrolyte has high ionic conductivity.
The preparation method of the inorganic solid electrolyte of example 5 is different from that of example 1 only in that: the lithium chloride powder of example 1 was replaced with lithium bromide powder and acetonitrile with dioxolane. The lithium ion conductivity of the inorganic solid electrolyte prepared in example 5 was 6.5X 10 -4 mS/cm。
The preparation method of the inorganic solid electrolyte of example 6 differs from that of example 1 only in that: the lithium chloride powder of example 1 was replaced with lithium iodide powder and acetonitrile with n-heptane. The lithium ion conductivity of the inorganic solid electrolyte obtained in example 6 was 3.8X 10 -4 mS/cm。
The preparation method of the inorganic solid electrolyte of example 7 differs from that of example 2 only in that: the lithium chloride powder of example 2 was replaced with lithium bromide powder and acetonitrile with ethylene glycol dimethyl ether. The lithium ion conductivity of the inorganic solid electrolyte obtained in example 7 was 5X 10 -4 mS/cm。
The preparation method of the inorganic solid electrolyte of example 8 is different from that of example 2 only in that: the lithium chloride powder of example 2 was replaced with lithium iodide powder and acetonitrile was replaced with N, N dimethylformamide. The lithium ion conductivity of the inorganic solid electrolyte prepared in example 8 was 6.0X 10 -4 mS/cm。
Comparative example
Inorganic solid electrolyte Li of this comparative example 6.25 PO 5.25 Cl 0.75 The preparation method comprises the following steps:
1) Lithium oxide (Li) 2 O) powder, lithium chloride (Li)Cl) powder, lithium phosphate (Li) 3 PO 4 ) Respectively putting the powder, a clean sample bottle (10 mL) and a stirrer in a vacuum drying oven to dry for 24h under a vacuum condition;
2) Under the protection of argon atmosphere in a glove box, sucking 30mL of acetonitrile solution by using a suction pipe, dripping the acetonitrile solution into a sample bottle with a stirrer, then respectively taking 3g of lithium oxide powder, lithium chloride powder and lithium phosphate powder according to the molar ratio of lithium oxide, lithium chloride and lithium phosphate being 3.25;
3) Putting the liquid precursor in the sample bottle into a vacuum drying oven, and drying for 5 hours at 60 ℃ under a vacuum condition to obtain white powder;
4) Taking out the dried white powder, putting the white powder into a muffle furnace, and carrying out heat treatment for 5 hours at 580 ℃ in a nitrogen atmosphere to obtain Li 5.75 PO 4.75 Cl 1.25 And (5) obtaining the powder.
As shown in FIG. 5, when the XRD patterns of the inorganic solid electrolyte prepared in this comparative example were compared with those of the inorganic solid electrolyte prepared in example 2, it can be seen from FIG. 5 that Li, which is an inorganic solid electrolyte, was successfully prepared by the liquid phase method 6.25 PO 5.25 Cl 0.75 And is consistent with XRD of the electrolyte prepared by the solid-phase sintering method.
Claims (5)
1. A method for preparing an inorganic solid electrolyte is characterized by comprising the following steps: the inorganic solid electrolyte is Li 6 PO 5 X or Li 6.25 PO 5.25 X 0.75 Type solid electrolyte, X is Cl, br, I, or Li 5.75 PO 4.75 Cl 1.25 A type solid electrolyte; the method comprises the following steps: preparing a mixture of an inorganic solid electrolyte raw material and a solvent under an anaerobic condition, removing the solvent in the mixture to obtain mixed powder, and performing heat treatment on the mixed powder to obtain the electrolyte; the solvent contains methanol, acetonitrile, dioxolane, n-heptane and ethylene glycolOne or any combination of methyl ether, dimethyl pyrrolidone, N-N dimethylformamide, acetone, cyclohexane, methyl ether and cyclohexane;
the inorganic solid electrolyte raw material comprises lithium oxide and Li 3 PO 4 And a lithium halide;
the lithium halide is selected from one or any combination of lithium chloride, lithium bromide and lithium iodide.
2. The method for producing an inorganic solid electrolyte according to claim 1, characterized in that: the molar ratio of the lithium oxide, the lithium phosphate and the lithium halide is 0.75-1.25.
3. The method for producing an inorganic solid electrolyte according to claim 2, characterized in that: removing the solvent from the mixture by vacuum drying the mixed solvent; the temperature of the vacuum drying is 55-65 ℃, and the time is 4-6h.
4. The method of producing an inorganic solid electrolyte according to claim 1, characterized in that: the temperature of the heat treatment is 230-580 ℃, and the time is 4-6h.
5. The method of producing an inorganic solid electrolyte according to claim 1, characterized in that: the volume of the solvent adopted for each 1g of the inorganic solid electrolyte raw material is 6-10mL.
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