CN113943151A - Sagger for preparing lithium aluminum titanium phosphate solid electrolyte material and preparation method thereof - Google Patents

Sagger for preparing lithium aluminum titanium phosphate solid electrolyte material and preparation method thereof Download PDF

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CN113943151A
CN113943151A CN202111198363.7A CN202111198363A CN113943151A CN 113943151 A CN113943151 A CN 113943151A CN 202111198363 A CN202111198363 A CN 202111198363A CN 113943151 A CN113943151 A CN 113943151A
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sagger
solid electrolyte
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protective layer
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CN113943151B (en
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彭家兴
刘兴亮
汪伟伟
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Gotion High Tech Co Ltd
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Abstract

The invention discloses a sagger for preparing a lithium aluminum titanium phosphate solid electrolyte material and a preparation method thereof, and relates to the technical field of solid electrolytes, the sagger comprises a sagger substrate and a protective layer coated on the inner surface of the sagger substrate, and the sagger substrate is prepared from the following raw materials in parts by weight: 50-60 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 20-25 parts of clay, 2.5-5 parts of zirconia micro powder, 2.5-5 parts of alumina micro powder, 5-10 parts of binder and 10-15 parts of water; the protective layer is prepared from the following raw materials in parts by weight: 20-35 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 10-15 parts of carrageenan, 2.5-5 parts of nano zirconia, 2.5-5 parts of nano alumina, 5-10 parts of talcum powder, 1-5 parts of graphene and 25-35 parts of water. The sagger effectively prevents the reaction between the raw materials of the lithium titanium aluminum phosphate and the sagger during firing, is easier to separate the fired materials in the sagger from the sagger body, and prolongs the service life of the sagger.

Description

Sagger for preparing lithium aluminum titanium phosphate solid electrolyte material and preparation method thereof
Technical Field
The invention relates to the technical field of solid electrolytes, in particular to a sagger for preparing a lithium aluminum titanium phosphate solid electrolyte material and a preparation method thereof.
Background
With the progress of science and technology and humanityThe improvement of the activity level, the development of electronic industries such as electric automobiles, portable electronic equipment, large-scale energy storage networks and the like is changing day by day, and the traditional commercial graphite cathode material of the lithium ion battery tends to the theoretical capacity (372mAh g)-1) The method reaches the development bottleneck and is difficult to meet the requirements of human society on high-endurance and high-power energy storage devices. Therefore, the vigorous development of battery energy storage materials with excellent performance has great significance for promoting the development of sustainable society. The lithium cathode in the lithium metal battery has high theoretical specific capacity (3860mAh/g), low electrochemical potential (-3.04V vs. standard hydrogen electrode) and small density (0.534 g/cm)3) However, although the lithium metal battery has many advantages, the battery has a series of problems of low coulombic efficiency, short cycle life and the like due to the violent volume change of the lithium metal, the instability of the SEI film and the uneven growth of lithium dendrites during continuous charge and discharge cycles, and the growth of the lithium dendrites even pierces the diaphragm to cause potential safety hazards, thereby causing short circuit and explosion of the lithium metal battery. Therefore, the inhibition of the growth of lithium dendrites becomes one of the research hotspots of the current battery energy storage materials, and researchers have conducted a great deal of research, and the inhibition of the growth of lithium dendrites is mainly achieved through the following research ideas: (1) a solid electrolyte; (2) a gel polymer electrolyte; (3) establishing electrode/electrolyte interface stability; (4) adding an electrolyte additive; (5) constructing an artificial SEI film; (6) and modifying the functional electrode.
Li of NASICON structure1.4Al0.4Ti1.6(PO4)3(LATP) has a relatively high electrical conductivity, about 7X 10 at ambient temperature-4S/cm, high melting point, good safety and stability at high temperature, high mechanical strength, and capability of well inhibiting the growth of lithium dendrites so as to avoid short circuit, however, LATP is very easy to chemically react with a sagger material in the firing process, and is tightly bonded with the inner surface of the sagger so as to be difficult to fall off.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte material and the preparation method thereof.
The sagger for preparing the lithium titanium aluminum phosphate solid electrolyte material comprises a sagger substrate and a protective layer coated on the inner surface of the sagger substrate, and is characterized in that the sagger substrate is prepared from the following raw materials in parts by weight: 50-60 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 20-25 parts of clay, 2.5-5 parts of zirconia micro powder, 2.5-5 parts of alumina micro powder, 5-10 parts of binder and 10-15 parts of water;
the protective layer is prepared from the following raw materials in parts by weight: 20-35 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 10-15 parts of carrageenan, 2.5-5 parts of nano zirconia, 2.5-5 parts of nano alumina, 5-10 parts of talcum powder, 1-5 parts of graphene and 25-35 parts of water.
Preferably, the aluminosilicate mineral powder is mullite or cordierite or a mixed powder of the mullite and the cordierite.
Preferably, in the sagger substrate raw material, the aluminosilicate mineral powder and the boron nitride powder have the particle size D50 of 10-50 mm.
Preferably, in the raw material of the protective layer, the particle size D50 of the aluminosilicate mineral powder and the boron nitride powder is 0.5-5 mm.
Preferably, the binder is one or more of alkaline silica sol, water glass and carboxymethyl cellulose.
Preferably, the thickness of the protective layer is 1-5 mm.
The invention also provides a preparation method of the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte material, which comprises the following steps:
s1, taking aluminosilicate mineral powder, boron nitride, clay, zirconia micro powder, alumina micro powder and a binder as raw materials of the sagger substrate according to parts by weight, mixing, adding water, stirring, and performing compression molding to obtain the sagger substrate;
s2, mixing the aluminosilicate mineral powder, the boron nitride, the carrageenan, the nano-zirconia, the nano-alumina, the talcum powder and the graphene according to the weight part, and adding water to stir to obtain protective layer slurry;
and S3, coating the protective layer slurry on the inner surface of the sagger substrate, pre-drying, mechanically pressing, drying, sintering and cooling to obtain the sagger substrate.
In S2, the coating may be performed by a dip coating method, a spray coating method, or a brush coating method.
Preferably, in S3, the pre-drying temperature is 60-80 ℃, and the drying time is 1-5 h; the drying temperature after machine pressing is 80-100 ℃, and the drying time is 3-8 h.
Preferably, in S3, the sintering temperature is 1200-1400 ℃, and the sintering time is 1-5 h.
Has the advantages that: the sagger consists of a sagger substrate and a protective layer on the surface of the sagger substrate, so that the reaction between raw materials of lithium titanium aluminum phosphate and the sagger during firing is effectively prevented, and the fired materials in the sagger are easier to separate from the sagger body; boron nitride, aluminum oxide and graphene are added into the protective layer, and the synergistic effect of the boron nitride, the aluminum oxide and the graphene effectively improves the corrosion resistance and the wear resistance of the sagger and prolongs the service life of the sagger. The method adopts a mode of directly coating on the surface of the sagger, and effectively improves the bonding performance of the sagger substrate and the protective layer through high-temperature sintering, thereby prolonging the service life of the sagger.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 50 parts of mullite (10 mm in terms of D50), 10 parts of boron nitride (10 mm in terms of D50), 20 parts of clay, 2.5 parts of zirconia micro powder, 2.5 parts of alumina micro powder and 5 parts of binder alkaline silica sol in parts by weight, adding 10 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 20 parts of mullite (D50 is 0.5mm), 10 parts of boron nitride (D50 is 0.5mm), 10 parts of carrageenan, 2.5 parts of nano zirconia, 2.5 parts of nano alumina, 5 parts of talcum powder and 1 part of graphene according to parts by weight, adding 25 parts of water, and stirring and mixing uniformly to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a dip coating method, pre-drying for 5 hours at 60 ℃, then performing mechanical pressing, and drying for 8 hours at 80 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 1 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 5 hours at 1200 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 2
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 50 parts of mullite (50 mm in terms of D50), 10 parts of boron nitride (50 mm in terms of D50), 20 parts of clay, 2.5 parts of zirconia micro powder, 2.5 parts of alumina micro powder and 5 parts of binder alkaline silica sol in parts by weight, adding 10 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 35 parts of mullite (5 mm in terms of D50), 15 parts of boron nitride (5 mm in terms of D50), 15 parts of carrageenan, 5 parts of nano-zirconia, 5 parts of nano-alumina, 10 parts of talcum powder and 5 parts of graphene in parts by weight, adding 35 parts of water, and uniformly stirring and mixing to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a dip coating method, pre-drying for 5 hours at 60 ℃, then performing mechanical pressing, and drying for 8 hours at 80 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 5 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 5 hours at 1200 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 3
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 50 parts of mullite (10 mm in terms of D50), 10 parts of boron nitride (10 mm in terms of D50), 20 parts of clay, 2.5 parts of zirconia micro powder, 2.5 parts of alumina micro powder and 5 parts of binder alkaline silica sol in parts by weight, adding 10 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 20 parts of mullite (D50 is 0.5mm), 10 parts of boron nitride (D50 is 0.5mm), 10 parts of carrageenan, 2.5 parts of nano zirconia, 2.5 parts of nano alumina, 5 parts of talcum powder and 1 part of graphene according to parts by weight, adding 25 parts of water, and stirring and mixing uniformly to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a dip coating method, pre-drying for 1h at 80 ℃, then performing mechanical pressing, and drying for 3h at 100 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 1 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 1h at 1400 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 4
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 60 parts of mullite and cordierite mixture powder (1: 1 mass ratio, 10mm for D50), 15 parts of boron nitride (10 mm for D50), 25 parts of clay, 5 parts of zirconia micro powder, 5 parts of alumina micro powder, 5 parts of alkaline silica sol and 5 parts of carboxymethyl cellulose according to parts by weight, adding 15 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 20 parts of mullite and cordierite mixture powder (1: 1 mass ratio, D50 is 0.5mm), 10 parts of boron nitride (D50 is 0.5mm), 10 parts of carrageenan, 2.5 parts of nano zirconia, 2.5 parts of nano alumina, 5 parts of talcum powder and 1 part of graphene according to parts by weight, adding 25 parts of water, and uniformly stirring and mixing to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a brush coating method, pre-drying for 5 hours at the temperature of 60 ℃, then performing mechanical pressing, and drying for 8 hours at the temperature of 80 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 1 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 5 hours at 1200 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 5
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 60 parts of mullite and cordierite mixture powder (1: 1 mass ratio, 50mm D50), 15 parts of boron nitride (50 mm D50), 25 parts of clay, 5 parts of zirconia micro powder, 5 parts of alumina micro powder, 5 parts of alkaline silica sol and 5 parts of carboxymethyl cellulose according to parts by weight, adding 15 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 35 parts of mullite and cordierite mixture powder (1: 1 mass ratio, 5mm D50), 15 parts of boron nitride (5 mm D50), 15 parts of carrageenan, 5 parts of nano zirconia, 5 parts of nano alumina, 10 parts of talcum powder and 5 parts of graphene according to parts by weight, adding 35 parts of water, and uniformly stirring and mixing to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a brush coating method, pre-drying for 5 hours at the temperature of 60 ℃, then performing mechanical pressing, and drying for 8 hours at the temperature of 80 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 5 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 5 hours at 1200 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 6
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 60 parts of mullite and cordierite mixture powder (1: 1 mass ratio, 10mm for D50), 15 parts of boron nitride (10 mm for D50), 25 parts of clay, 5 parts of zirconia micro powder, 5 parts of alumina micro powder, 5 parts of alkaline silica sol and 5 parts of carboxymethyl cellulose in parts by weight, adding 15 parts of water, uniformly stirring and mixing, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 20 parts of mullite and cordierite mixture powder (1: 1 mass ratio, D50 is 0.5mm), 10 parts of boron nitride (D50 is 0.5mm), 10 parts of carrageenan, 2.5 parts of nano zirconia, 2.5 parts of nano alumina, 5 parts of talcum powder and 1 part of graphene, adding 25 parts of water, and uniformly stirring and mixing to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a brush coating method, pre-drying for 1 hour at 80 ℃, then performing mechanical pressing, and drying for 3 hours at 100 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 1 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 1h at 1400 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Example 7
A sagger for preparing lithium aluminum titanium phosphate solid electrolyte material comprises a sagger base body and a protective layer, wherein the protective layer at least covers the inner surface of the sagger base body;
the preparation method comprises the following steps:
(1) mixing 55 parts of mullite and cordierite mixture powder (1: 1 mass ratio, D50 is 30mm), 13 parts of boron nitride (D50 is 30mm), 22 parts of clay, 3 parts of zirconia micropowder, 3 parts of alumina micropowder and 8 parts of binder carboxymethyl cellulose according to the parts by weight, adding 12 parts of water, stirring and mixing uniformly, and then carrying out compression molding by compression molding equipment to obtain a sagger substrate preliminarily;
(2) mixing 30 parts of mullite (D50 is 2mm), 12 parts of boron nitride (D50 is 2mm), 13 parts of carrageenan, 3.5 parts of nano zirconia, 3 parts of nano alumina, 7 parts of talcum powder and 2 parts of graphene according to parts by weight, adding 30 parts of water, and stirring and mixing uniformly to obtain a protective layer slurry;
(3) coating the protective layer slurry on the inner surface of the sagger substrate by adopting a brush coating method, pre-drying for 3 hours at 75 ℃, then performing mechanical pressing, and drying for 4 hours at 95 ℃, wherein the thickness of a material layer of the protective layer is controlled to be 2 mm;
(4) and (4) placing the sagger dried in the step (3) into a high-temperature kiln, sintering for 1.5h at 1360 ℃, and cooling to room temperature to obtain the sagger for preparing the lithium titanium aluminum phosphate solid electrolyte.
Comparative example
A sagger for preparing a lithium aluminum titanium phosphate solid electrolyte material comprises the following steps:
(1) 55 parts of mullite and cordierite mixed powder (1: 1 mass ratio, D50 is 30mm), 22 parts of clay and 8 parts of binder carboxymethyl cellulose are mixed according to the parts by weight, 12 parts of water is added, and the mixture is uniformly stirred and then is pressed and molded by pressing and molding equipment to obtain a sagger substrate;
(2) mixing 30 parts of mullite and 13 parts of carrageenan according to parts by weight, adding 30 parts of water, uniformly stirring, coating on the inner surface of the sagger substrate prepared in the step (1), controlling the thickness of a material layer of a coating layer to be 2mm, pre-drying for 3 hours at 75 ℃, then carrying out mechanical pressing, drying for 4 hours at 95 ℃, drying twice, and sintering for 1.5 hours at 1360 ℃ in a high-temperature kiln to prepare the common sagger.
Application tests show that when the saggars prepared in the embodiments 1-7 of the invention are fired with lithium aluminum titanium phosphate, the fired materials and the saggars are not bonded together, and the saggars are still normal after being recycled for a plurality of times; the conventional sagger prepared in the comparative example reacts with the sagger when firing the lithium titanium aluminum phosphate solid electrolyte, and is tightly combined with the sagger, so that the sagger is difficult to separate.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (9)

1. A sagger for preparing a lithium aluminum titanium phosphate solid electrolyte material comprises a sagger substrate and a protective layer coated on the inner surface of the sagger substrate, and is characterized in that the sagger substrate is prepared from the following raw materials in parts by weight: 50-60 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 20-25 parts of clay, 2.5-5 parts of zirconia micro powder, 2.5-5 parts of alumina micro powder, 5-10 parts of binder and 10-15 parts of water;
the protective layer is prepared from the following raw materials in parts by weight: 20-35 parts of aluminosilicate mineral powder, 10-15 parts of boron nitride, 10-15 parts of carrageenan, 2.5-5 parts of nano zirconia, 2.5-5 parts of nano alumina, 5-10 parts of talcum powder, 1-5 parts of graphene and 25-35 parts of water.
2. The sagger for producing lithium aluminum titanium phosphate solid electrolyte material according to claim 1, wherein the aluminosilicate mineral powder is a mixed powder of mullite or cordierite or both.
3. The sagger for preparing lithium aluminum titanium phosphate solid electrolyte material according to claim 1, wherein in the raw material of the sagger substrate, the powder particle diameter D50 of aluminosilicate mineral powder and boron nitride is 10-50 mm.
4. The sagger for preparing lithium aluminum titanium phosphate solid electrolyte material according to claim 1, wherein the particle size D50 of the aluminosilicate mineral powder and the boron nitride in the raw material of the protective layer is 0.5-5 mm.
5. The sagger for preparing lithium aluminum titanium phosphate solid electrolyte material according to claim 1, wherein the binder is one or more of alkaline silica sol, water glass, and carboxymethyl cellulose.
6. The sagger for producing lithium aluminum titanium phosphate solid electrolyte material according to claim 1, wherein the thickness of the protective layer is 1 to 5 mm.
7. A method for producing a sagger for producing a lithium aluminum titanium phosphate solid electrolyte material according to any one of claims 1 to 6, comprising the steps of:
s1, taking aluminosilicate mineral powder, boron nitride, clay, zirconia micro powder, alumina micro powder and a binder as raw materials of the sagger substrate according to parts by weight, mixing, adding water, stirring, and performing compression molding to obtain the sagger substrate;
s2, mixing the aluminosilicate mineral powder, the boron nitride, the carrageenan, the nano-zirconia, the nano-alumina, the talcum powder and the graphene according to the weight part, and adding water to stir to obtain protective layer slurry;
and S3, coating the protective layer slurry on the inner surface of the sagger substrate, pre-drying, mechanically pressing, drying, sintering and cooling to obtain the sagger substrate.
8. The method for producing a sagger for producing a lithium titanium aluminum phosphate solid electrolyte material according to claim 7, wherein in S3, the pre-drying temperature is 60 to 80 ℃, and the drying time is 1 to 5 hours; the drying temperature after machine pressing is 80-100 ℃, and the drying time is 3-8 h.
9. The method for preparing a sagger for preparing lithium aluminum titanium phosphate solid electrolyte material as claimed in claim 7, wherein in S3, the sintering temperature is 1200-1400 ℃, and the sintering time is 1-5 h.
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