CN115117436A - Method and battery for reducing moisture content of nano ion conductor solid electrolyte - Google Patents

Method and battery for reducing moisture content of nano ion conductor solid electrolyte Download PDF

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CN115117436A
CN115117436A CN202210891817.7A CN202210891817A CN115117436A CN 115117436 A CN115117436 A CN 115117436A CN 202210891817 A CN202210891817 A CN 202210891817A CN 115117436 A CN115117436 A CN 115117436A
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solid electrolyte
nano
ion conductor
conductor solid
electrolyte
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沈德赟
申彤
张新华
周建飞
施雅玲
翁启东
李婷
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Nanmu Nanotechnology Beijing Co ltd
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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
    • 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
    • H01M10/052—Li-accumulators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0068—Solid electrolytes inorganic

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Abstract

The invention relates to a method and a battery for reducing the moisture content of a solid electrolyte of a nano ion conductor. The method comprises the following steps: dissolving a fluorine-containing silane coupling agent in a first organic solvent, and stirring for dissolving to obtain a first solution; dispersing the nano ion conductor solid electrolyte in a mixed solution of a second organic solvent and pure water, and performing ultrasonic dispersion uniformly to obtain a dispersion solution; mixing the first solution with the dispersion liquid, adjusting the pH value of the mixed solution, and heating and magnetically stirring the mixed solution after the pH value is adjusted to obtain a suspension; and performing centrifugal precipitation on the suspension, performing vacuum drying and grinding to obtain the nano ion conductor solid electrolyte with the surface subjected to hydrophobic modification, and reducing the water content of the nano ion conductor solid electrolyte by reducing the water absorption of the nano ion conductor solid electrolyte.

Description

Method and battery for reducing moisture content of nano ion conductor solid electrolyte
Technical Field
The invention relates to the technical field of material treatment, in particular to a method and a battery for reducing the moisture content of a solid electrolyte of a nano ion conductor.
Background
Currently, commercial lithium ion batteries mainly use organic electrolyte and graphite carbon negative electrodes, and the energy density of the lithium ion batteries almost reaches a theoretical limit value, so that the lithium ion batteries are difficult to meet the increasing energy storage requirement. Metallic lithium is an ideal anode material with the highest specific energy and the lowest reduction potential. However, the problems of pulverization, dendritic crystal growth, volume expansion, continuous reaction with the electrolyte and the like of the metal lithium cathode in the repeated charge-discharge process are solved, and more importantly, the traditional liquid electrolyte has the characteristics of easy volatilization, easy leakage, easy combustion and the like, so that the lithium battery is easy to catch fire or even explode, and serious safety accidents can be caused.
The development of solid-state batteries using a solid electrolyte instead of a liquid electrolyte is a final solution that is considered to solve the above-mentioned problems. The solid electrolyte has high safety and reliability due to the advantages of no leakage, good thermal stability and the like. Most importantly, the solid electrolyte has high mechanical strength and can effectively inhibit the growth of dendrites during the cycling process of the battery. Meanwhile, the solid-state battery has a simple structure, and the electrodes and the electrolyte are solid, so that the battery is convenient to process and package. Therefore, the solid-state battery has the characteristics of high safety and high energy density, and is an ideal scheme for developing a new generation of energy storage battery.
The total ionic conductivity of the solid electrolyte is significantly reduced after contacting water, and microcracks, grain shape deformation, nanoparticle formation, chemical composition transformation, cell shrinkage, internal structure polyhedrons and strain changes can also occur when the solid electrolyte is arranged. The solid electrolyte is highly sensitive to water. The surface of the nano solid electrolyte contains polar hydrophilic groups which are easy to absorb water, and has extremely small particle size and extremely high specific surface area, and a pore structure exists among particles, so that the nano solid electrolyte is easy to absorb water, and the final performance of the solid battery is influenced.
Disclosure of Invention
The embodiment of the invention provides a method for reducing the moisture content of a nano ion conductor solid electrolyte and a battery.
In a first aspect, embodiments of the present invention provide a method for reducing the moisture content of a nano-ion conductor solid-state electrolyte, the method including:
dissolving a fluorine-containing silane coupling agent in a first organic solvent, and stirring for dissolving to obtain a first solution;
dispersing the nano ion conductor solid electrolyte in a mixed solution of a second organic solvent and pure water, and performing ultrasonic dispersion uniformly to obtain a dispersion solution;
mixing the first solution with the dispersion liquid, adjusting the pH value of the mixed solution, and heating and magnetically stirring the mixed solution after the pH value is adjusted to obtain a suspension;
and performing centrifugal precipitation on the suspension, performing vacuum drying and grinding to obtain the nano ion conductor solid electrolyte with the surface subjected to hydrophobic modification, and reducing the water content of the nano ion conductor solid electrolyte by reducing the water absorption of the nano ion conductor solid electrolyte.
Preferably, the nano-ion conductor solid-state electrolyte comprises: at least one of garnet-type solid electrolyte, sulfide-type solid electrolyte, NASICON-type solid electrolyte, LiPON-type solid electrolyte, and perovskite-type solid electrolyte;
the particle size of the nano ion conductor solid electrolyte is 10nm-3 um.
Preferably, the fluorine-containing silane coupling agent and the first organic solvent are as follows in parts by weight: 10-20: 80-90;
the fluorine-containing silane coupling agent includes: one or more of heptadecafluorodecyltriethoxysilane, heptadecafluorodecyltrimethoxysilane, tridecafluorooctyltriethoxysilane and tridecafluorooctyltrimethoxysilane;
the first organic solvent includes: one or more of n-butanol, acetone, ethylene glycol, isopropanol, and ethanol.
Preferably, the fluorine-containing silane coupling agent and the first organic solvent are as follows in parts by weight: 10-20: 80-90;
the fluorine-containing silane coupling agent includes: one or more of heptadecafluorodecyltriethoxysilane, heptadecafluorodecyltrimethoxysilane, tridecafluorooctyltriethoxysilane and tridecafluorooctyltrimethoxysilane;
the first organic solvent includes: one or more of n-butanol, acetone, ethylene glycol, isopropanol, and ethanol.
Preferably, the mass part ratio of the first solution to the mixed solution is as follows: 1/10-1/2.
Preferably, the pH of the mixed solution is specifically: adjusting the pH value range of the mixed solution to 3-6 by using an acid regulator;
the acidity regulator comprises: one or more of dilute hydrochloric acid, glacial acetic acid and citric acid.
Preferably, the heating magnetic stirring treatment specifically comprises: heating and magnetically stirring in a three-neck flask at 40-70 deg.c for 1-24 hr.
In a second aspect, the embodiment of the present invention provides a surface-hydrophobically modified nano-ion conductor solid-state electrolyte prepared by the method for reducing the moisture content of the nano-ion conductor solid-state electrolyte according to the first aspect.
Preferably, the surface hydrophobically modified nano ion conductor solid electrolyte has the structure: and a layer of coating material is arranged on the surface of the nano ion conductor solid electrolyte, and the coating material is used for reducing the surface energy of the nano ion conductor solid electrolyte.
In a third aspect, an embodiment of the present invention provides a lithium battery, including the surface hydrophobically modified nano-ion conductor solid-state electrolyte prepared by the method for reducing the moisture content of the nano-ion conductor solid-state electrolyte according to the first aspect.
According to the method for reducing the moisture content of the nano ion conductor solid electrolyte provided by the embodiment of the invention, the fluorine-containing silane coupling agent is dissolved in the first organic solvent, the first solution is obtained by stirring and dissolving, the nano ion conductor solid electrolyte is dispersed in the mixed solution of the second organic solvent and pure water, and the dispersion liquid is obtained by uniformly dispersing through ultrasonic; and then mixing the first solution with the dispersion liquid, adjusting the pH value of the mixed solution, heating and magnetically stirring the mixed solution after the pH value is adjusted to obtain turbid liquid, and finally performing centrifugal drying to form a low-surface-energy material coating on the surface of the nano ion conductor solid electrolyte, so that the hydrophobicity of the material is enhanced, the adsorption of the nano ion conductor solid electrolyte material to water in the environment is prevented, and the stability of the nano ion conductor solid electrolyte is improved.
Drawings
The technical solutions of the embodiments of the present invention are further described in detail with reference to the accompanying drawings and embodiments.
FIG. 1 is a flow chart of a method of reducing the moisture content of a nano-ionic conductor solid-state electrolyte according to an embodiment of the present invention;
fig. 2 is an X-ray diffraction (XRD) pattern of the surface hydrophobically modified nano ion conductor solid electrolyte particle prepared in example 1 of the present invention and an XRD pattern of the nano ion conductor solid electrolyte particle.
Detailed Description
The invention is further illustrated by the following figures and specific examples, but it should be understood that these examples are for the purpose of illustration only and are not to be construed as in any way limiting the present invention, i.e., as in no way limiting its scope.
The invention provides a method for reducing the moisture content of a solid electrolyte of a nano ion conductor, which mainly comprises the following steps of:
110, dissolving a fluorine-containing silane coupling agent in a first organic solvent, and stirring for dissolving to obtain a first solution;
wherein the fluorine-containing silane coupling agent and the first organic solvent are as follows in parts by weight: 10-20: 80-90; the fluorine-containing silane coupling agent comprises: one or more of heptadecafluorodecyltriethoxysilane, heptadecafluorodecyltrimethoxysilane, tridecafluorooctyltriethoxysilane and tridecafluorooctyltrimethoxysilane; the first organic solvent includes: one or more of n-butanol, acetone, ethylene glycol, isopropanol, and ethanol.
Step 120, dispersing the nano ion conductor solid electrolyte in a mixed solution of a second organic solvent and pure water, and performing ultrasonic dispersion uniformly to obtain a dispersion solution;
the nano-ion conductor solid electrolyte, the second organic solvent and the pure water are as follows according to the parts by weight: 1-5: 75-90: 5-20 parts of; the second organic solvent comprises one or more of n-butanol, acetone, ethylene glycol, isopropanol, and ethanol. The nano ion conductor solid electrolyte suitable for the present invention comprises: at least one of garnet-type solid electrolyte, sulfide-type solid electrolyte, NASICON-type solid electrolyte, LiPON-type solid electrolyte, and perovskite-type solid electrolyte; the particle diameter of the nano ion conductor solid electrolyte is 10nm-3 um.
In the invention, the second organic solvent and pure water are used as mutual solvents, and the fluorine-containing silane coupling agent in the first solvent is subjected to hydrolysis reaction through the pure water.
Step 130, mixing the first solution with the dispersion liquid, adjusting the pH value of the mixed solution, and heating and magnetically stirring the mixed solution after the pH value is adjusted to obtain a suspension;
specifically, the mass part ratio of the first solution to the mixed solution is as follows: 1/10-1/2.
And adjusting the pH value range of the mixed solution to 3-6 by using an acidity regulator, and accelerating the reaction of the first solution and the mixed solution by using the acidity regulator to generate a catalytic effect. The acidity regulator comprises: one or more of dilute hydrochloric acid, glacial acetic acid and citric acid.
The heating magnetic stirring treatment specifically comprises the following steps: heating and magnetically stirring in a three-neck flask at 40-70 deg.c for 1-24 hr.
And 140, performing centrifugal precipitation on the suspension, performing vacuum drying and grinding to obtain the nano ion conductor solid electrolyte with the surface subjected to hydrophobic modification, and reducing the water content of the nano ion conductor solid electrolyte by reducing the water absorbability of the nano ion conductor solid electrolyte.
The fluorine-containing silane coupling agent is subjected to hydrolysis reaction, low molecular alcohol is released after hydrolysis, active silanol generated by the hydrolysis reaction is chemically bonded with active hydroxyl oxygen-containing groups on the surface of the solid electrolyte, and a self-assembled monomolecular fluorine-silicon film layer is formed on the surface of the solid electrolyte, so that surface hydrophobic modification is realized.
The structure of the surface hydrophobically modified nano ion conductor solid electrolyte obtained by the method is as follows: the surface of the nano ion conductor solid electrolyte is coated with a layer of monomolecular fluorine-silicon film layer material, and the coating material has low surface energy, so that the surface energy of the nano ion conductor solid electrolyte can be reduced.
The surface hydrophobic modified nano ion conductor solid electrolyte prepared by the method for reducing the moisture content of the nano ion conductor solid electrolyte can be used for lithium batteries, particularly lithium ion batteries.
In order to better understand the technical scheme provided by the present invention, the following description uses specific examples to illustrate the specific processes and properties for preparing the surface-hydrophobically modified nano-ion conductor solid-state electrolyte by using the method for reducing the moisture content of the nano-ion conductor solid-state electrolyte provided by the above embodiments of the present invention.
Example 1
3g of heptadecafluorodecyltrimethoxysilane was dissolved in 20g of acetone, and dissolved with stirring by an electromagnetic stirrer to obtain a first solution.
3g of NASICON type solid electrolyte lithium titanium aluminum phosphate (LATP) was dispersed in 70g of acetone and 10g of pure water with an ultrasonic disperser for 10 minutes to obtain a dispersion.
Mixing the first solution and the dispersion, adding 0.6g of glacial acetic acid to adjust the pH value to about 4.5, pouring the mixed solution into a three-neck flask, setting the temperature at 45 ℃ and the rotating speed at 600r/min, and heating and magnetically stirring for 6 hours.
And performing 10000r/min high-speed centrifugal precipitation on the obtained suspension, washing the suspension for three times by using ethanol, performing vacuum drying on the final precipitate at 80 ℃ for 12 hours to obtain surface hydrophobically modified LATP, and grinding the LATP for 0.5 hour to obtain the low-water-content nano ion conductor solid electrolyte.
Comparative tests of the properties were carried out with the material prepared in example 1, using the NASICON type solid electrolyte lithium titanium aluminium phosphate (LATP) used in example 1 as comparative example 1.
The X-ray diffraction (XRD) pattern of the surface hydrophobically modified nano ion conductor solid electrolyte particle prepared in example 1 of the present invention and the XRD pattern of the nano ion conductor solid electrolyte particle are shown in fig. 2. It can be seen that the diffraction peak of the material is not obviously changed, so that the method provided by the invention can be used for surface modification without changing the chemical property of the solid electrolyte.
The measured moisture content and contact angle are shown in tables 1 and 2 below.
Example 1 Comparative example 1
Moisture content/ppm 1749 19851
TABLE 1
Example 1 Comparative example 1
Contact Angle/° 30 143
TABLE 2
Therefore, the modified LATP material obtained in example 1 of the present invention has a much lower moisture content than the original LATP material, and the contact angle is significantly reduced, which indicates that the hydrophobic property of the material is significantly improved.
Example 2
4g of tridecafluorooctyltriethoxysilane was dissolved in 20g of ethylene glycol and dissolved by stirring with an electromagnetic stirrer to obtain a first solution.
4g of garnet-type solid electrolyte Li 7 La 3 Zr 2 O 12 (LLZO) was dispersed in 80g of acetone and 10g of pure water with an ultrasonic disperser for 10 minutes to obtain a dispersion.
Mixing the first solution and the dispersion, adding 0.8g of citric acid to adjust the pH value to about 5, pouring the mixed solution into a three-neck flask, setting the temperature at 50 ℃ and the rotating speed at 800r/min, and heating and magnetically stirring for 8 hours.
And performing 10000r/min high-speed centrifugal precipitation on the obtained suspension, washing the suspension for three times by using ethanol, taking the final precipitate, performing vacuum drying on the final precipitate at 80 ℃ for 12 hours to obtain LLZO with the surface subjected to hydrophobic modification, and grinding the LLZO for 0.5 hour to obtain the nano ion conductor solid electrolyte with low water content.
Example 3
5g of heptadecafluorodecyltriethoxysilane was dissolved in 40g of isopropyl alcohol, and dissolved with stirring by a magnetic stirrer to obtain a first solution.
5g of sulfide solid electrolyte Li 6 PS 5 The Cl was dispersed in 80g of isopropanol and 15g of pure water with an ultrasonic disperser for 10 minutes to obtain a dispersion.
Mixing the first solution and the dispersion liquid, adding 0.5g of dilute hydrochloric acid to adjust the pH value to about 4, pouring the mixed solution into a three-neck flask, setting the temperature at 60 ℃ and the rotating speed at 800r/min, and heating and magnetically stirring for 6 hours.
Performing 10000r/min high-speed centrifugal precipitation on the obtained suspension, washing the suspension for three times by using ethanol, and performing vacuum drying on the final precipitate at 80 ℃ for 12 hours to obtain Li with surface subjected to hydrophobic modification 6 PS 5 And (4) Cl, and grinding for 0.5 hour to obtain the nano ion conductor solid electrolyte with low water content.
According to the method for reducing the moisture content of the nano ion conductor solid electrolyte provided by the embodiment of the invention, the fluorine-containing silane coupling agent is dissolved in the first organic solvent, the first solution is obtained by stirring and dissolving, the nano ion conductor solid electrolyte is dispersed in the mixed solution of the second organic solvent and pure water, and the dispersion liquid is obtained by uniformly dispersing through ultrasonic; and then mixing the first solution with the dispersion liquid, adjusting the pH value of the mixed solution, heating and magnetically stirring the mixed solution after the pH value is adjusted to obtain turbid liquid, and finally performing centrifugal drying to form a low-surface-energy material coating on the surface of the nano ion conductor solid electrolyte, so that the hydrophobicity of the material is enhanced, the adsorption of the nano ion conductor solid electrolyte material to water in the environment is prevented, and the stability of the nano ion conductor solid electrolyte is improved.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are merely exemplary embodiments of the present invention, and are not intended to limit the scope of the present invention, and any modifications, equivalent substitutions, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (10)

1. A method of reducing the moisture content of a nano-ionic conductor solid-state electrolyte, the method comprising:
dissolving a fluorine-containing silane coupling agent in a first organic solvent, and stirring for dissolving to obtain a first solution;
dispersing the nano ion conductor solid electrolyte in a mixed solution of a second organic solvent and pure water, and performing ultrasonic dispersion uniformly to obtain a dispersion solution;
mixing the first solution with the dispersion liquid, adjusting the pH value of the mixed solution, and heating and magnetically stirring the mixed solution after the pH value is adjusted to obtain a suspension;
and performing centrifugal precipitation on the suspension, performing vacuum drying and grinding to obtain the nano ion conductor solid electrolyte with the surface subjected to hydrophobic modification, and reducing the water content of the nano ion conductor solid electrolyte by reducing the water absorption of the nano ion conductor solid electrolyte.
2. The method of claim 1, wherein the nano-ionic conductor solid-state electrolyte comprises: at least one of garnet type solid electrolyte, sulfide solid electrolyte, NASI CON type solid electrolyte, LiPON type solid electrolyte, and perovskite type solid electrolyte;
the particle size of the nano ion conductor solid electrolyte is 10nm-3 um.
3. The method according to claim 1, wherein the fluorine-containing silane coupling agent and the first organic solvent are in parts by weight: 10-20: 80-90;
the fluorine-containing silane coupling agent includes: one or more of heptadecafluorodecyltriethoxysilane, heptadecafluorodecyltrimethoxysilane, tridecafluorooctyltriethoxysilane and tridecafluorooctyltrimethoxysilane;
the first organic solvent includes: one or more of n-butanol, acetone, ethylene glycol, isopropanol, and ethanol.
4. The method according to claim 1, wherein the nano-ion conductor solid electrolyte, the second organic solvent and pure water are prepared from the following components in parts by weight: 1-5: 75-90: 5-20 parts of;
the second organic solvent comprises one or more of n-butanol, acetone, ethylene glycol, isopropanol and ethanol.
5. The method according to claim 1, wherein the mass parts ratio of the first solution to the mixed solution is as follows: 1/10-1/2.
6. The method according to claim 1, wherein the adjusting the pH of the mixed solution is specifically: adjusting the pH value range of the mixed solution to 3-6 by using an acid regulator;
the acidity regulator comprises: one or more of dilute hydrochloric acid, glacial acetic acid and citric acid.
7. The method according to claim 1, wherein the heating magnetic stirring treatment is specifically: heating and magnetically stirring in a three-neck flask at 40-70 deg.c for 1-24 hr.
8. A surface hydrophobically modified nano-ionic conductor solid-state electrolyte prepared by the method for reducing the moisture content of the nano-ionic conductor solid-state electrolyte as claimed in any one of claims 1 to 7.
9. The surface hydrophobically modified nano-ionic conductor solid-state electrolyte of claim 8, wherein the surface hydrophobically modified nano-ionic conductor solid-state electrolyte has a structure of: and a layer of coating material is arranged on the surface of the nano ion conductor solid electrolyte, and the coating material is used for reducing the surface energy of the nano ion conductor solid electrolyte.
10. A lithium battery comprising the surface hydrophobically modified nano-ion conductor solid-state electrolyte prepared by the method for reducing the moisture content of the nano-ion conductor solid-state electrolyte according to any one of claims 1 to 7.
CN202210891817.7A 2022-07-27 2022-07-27 Method and battery for reducing moisture content of nano ion conductor solid electrolyte Pending CN115117436A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117174988A (en) * 2023-09-01 2023-12-05 哈尔滨工业大学 Preparation method of lithium/sodium ion battery material and application of lithium/sodium ion battery material in lithium/sodium ion battery

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117174988A (en) * 2023-09-01 2023-12-05 哈尔滨工业大学 Preparation method of lithium/sodium ion battery material and application of lithium/sodium ion battery material in lithium/sodium ion battery
CN117174988B (en) * 2023-09-01 2024-04-30 哈尔滨工业大学 Preparation method of lithium/sodium ion battery material and application of lithium/sodium ion battery material in lithium/sodium ion battery

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