CN111377736A - Preparation method for synthesizing garnet structure material by solid phase method - Google Patents

Preparation method for synthesizing garnet structure material by solid phase method Download PDF

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CN111377736A
CN111377736A CN202010285379.0A CN202010285379A CN111377736A CN 111377736 A CN111377736 A CN 111377736A CN 202010285379 A CN202010285379 A CN 202010285379A CN 111377736 A CN111377736 A CN 111377736A
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solid phase
garnet structure
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刘国强
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Shanghai Dian Yang Industry Co ltd
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Abstract

The invention provides a preparation method for synthesizing garnet structure material by a solid phase method, which comprises the following steps: a preparation method for synthesizing garnet structure material by a solid phase method is characterized by comprising the following steps: the method comprises the following steps: step (1) according to LixLa3ZryTazO12Weighing equal and corresponding parts by weight of lithium carbonate, lanthanum oxide, zirconium oxide and tantalum pentoxide according to the stoichiometric ratio (x +4y +5z is 15), putting the weighed parts into a ball milling tank, and adding deionized water to obtain mixed slurry A; taking out the mixture slurry A, putting the mixture slurry A into an oven, drying the mixture slurry A to obtain a dried material B; taking the material B out, and putting the material B into a box-type furnace for pre-sintering; then cooling to obtain a material C; step (4), taking out the material C and putting the material C into a grinder; pressing under a pressure of 2kg to form a briquette D; the invention shortens the sintering time, does not lose lithium element at high temperature, and reduces the cost.

Description

Preparation method for synthesizing garnet structure material by solid phase method
Technical Field
The invention relates to the technical field of lithium ion battery electrolyte materials, in particular to a preparation method for synthesizing a garnet structure material by a solid phase method.
Background
Li having garnet structure in recent years7La3Zr2O12Materials have attracted attention because of their conductivity of up to 10 at room temperature-4S cm-1 order of magnitude, is suitable for the practical application level of all-solid-state lithium batteries, has good contact stability with lithium electrodes, can be used as a solid electrolyte material of solid-state batteries, and avoids the problems of potential safety hazards, such as leakage, flammability and the like, of the existing liquid organic electrolyte so as to improve the existing technology. The preparation method has the advantages of simple preparation, easily obtained raw materials, low pollution and the like due to good chemical and electrochemical stability, so that the method gradually becomes a research hotspot and has wide application prospect. LixLa3ZryTazO12The doping of (x +4y +5z 15) can be such that Li7La3Zr2O12The material has lower synthesis temperature, longer crystallization time and better crystal form, so that the material has higher conductivity.
At present LixLa3ZryTazO12The preparation method of the (x +4y +5z ═ 15) material mainly comprises the traditional solid phase method and liquid phase method.
Compared with a solid phase method for large-scale industrial production, the solid phase method is more environment-friendly, low in cost and easy to operate, but the traditional solid phase method has longer roasting time and can easily cause a large amount of Li element to run off at high temperature, so that the production and processing costs are obviously increased.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method for synthesizing a garnet structure material by a solid phase method, which solves the problems of incomplete filtration and low preparation efficiency.
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method for synthesizing garnet structure material by a solid phase method comprises the following steps:
step (1) according to LixLa3ZryTazO12Weighing equal parts by weight of lithium carbonate, lanthanum oxide, zirconium oxide and tantalum pentoxide according to the stoichiometric ratio (x +4y +5z ═ 15), and putting the lithium carbonate, the lanthanum oxide, the zirconium oxide and the tantalum pentoxide into ballsAdding deionized water into a grinding tank to obtain mixed slurry A;
taking out the mixture slurry A, putting the mixture slurry A into an oven, drying the mixture slurry A to obtain a dried material B;
taking the material B out, putting the material B into a box-type furnace for pre-sintering, and then cooling to obtain a material C;
step (4), taking out the material C and putting the material C into a grinder; pressing under a pressure of 2kg to form a briquette D;
step (5), treating the sagger at high temperature in advance, adopting the sagger made of zirconia, uniformly scattering lithium carbonate powder at the bottom, then pretreating at high temperature in an air atmosphere, wherein the temperature is 1300 ℃ for 4 hours, placing the briquette D into a specially treated closed sagger for secondary sintering, and then cooling to obtain a briquette E;
and (6) ball-milling and crushing the compact E to obtain a final product, namely a garnet structure LixLa3ZryTazO12(x +4y +5z 15) powder.
Further, the ball milling time in the step (1) is 6-12 hours.
Further, the sintering temperature in the step (3) is 600-800 ℃, and the time is 2-4 hours.
Further, the temperature of the secondary sintering in the step (5) is 1000-1200 ℃, and the time is 6-12 hours.
Advantageous effects
The invention provides a preparation method for synthesizing a garnet structure material by a solid phase method. Compared with the prior art, the method has the following beneficial effects: the invention has short sintering time, does not lose lithium element at high temperature, and reduces the cost.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method for synthesizing garnet structure material by a solid phase method comprises the following steps:
step (1) according to LixLa3ZryTazO12Weighing equal and corresponding parts by weight of lithium carbonate, lanthanum oxide, zirconium oxide and tantalum pentoxide according to the stoichiometric ratio (x +4y +5z is 15), putting the weighed materials into a ball milling tank, adding deionized water, and carrying out ball milling for 6 hours to obtain mixed slurry A;
taking out the mixture slurry A, putting the mixture slurry A into an oven, drying the mixture slurry A for 2 hours to obtain a dried material B;
taking the material B out, putting the material B into a box-type furnace, presintering the material B for 2 hours at 600 ℃, and then cooling the material B to obtain a material C;
step (4), taking out the material C, putting the material C into a grinder, and pressing the material C into a billet D under the pressure of 2 kg;
step (5), treating the sagger at high temperature in advance, adopting a zirconia sagger, uniformly scattering lithium carbonate powder at the bottom, then pretreating at high temperature in an air atmosphere, wherein the temperature is 1300 ℃ for 4 hours, placing the briquette D into a specially treated closed sagger, sintering for 6 hours at 1000 ℃, and then cooling to obtain a briquette E;
and (6) ball-milling and crushing the compact E to obtain a final product, namely a garnet structure LixLa3ZryTazO12(x +4y +5z 15) powder.
Example 2
A preparation method for synthesizing garnet structure material by a solid phase method comprises the following steps:
step (1) according to LixLa3ZryTazO12Weighing equal and corresponding parts by weight of lithium carbonate, lanthanum oxide, zirconium oxide and tantalum pentoxide according to the stoichiometric ratio (x +4y +5z is 15), putting the weighed materials into a ball milling tank, adding deionized water, and carrying out ball milling for 9 hours to obtain mixed slurry A;
taking out the mixture slurry A, putting the mixture slurry A into an oven, drying the mixture slurry A for 2 hours to obtain a dried material B;
taking the material B out, putting the material B into a box-type furnace, pre-sintering the material B for 3 hours at 750 ℃, and then cooling the material B to obtain a material C;
step (4), taking out the material C and putting the material C into a grinder; pressing under a pressure of 2kg to form a briquette D;
step (5), treating the sagger at high temperature in advance, adopting the sagger made of zirconia, uniformly scattering lithium carbonate powder at the bottom, then pretreating at high temperature in an air atmosphere, wherein the temperature is 1300 ℃ for 4 hours, placing the briquette D into a specially-treated closed sagger, and sintering for 10 hours at 1100 ℃; then cooling to obtain a billet E;
and (6) ball-milling and crushing the compact E to obtain a final product, namely a garnet structure LixLa3ZryTazO12(x +4y +5z 15) powder.
Example 3
A preparation method for synthesizing garnet structure material by a solid phase method comprises the following steps:
step (1) according to LixLa3ZryTazO12Weighing equal and corresponding parts by weight of lithium carbonate, lanthanum oxide, zirconium oxide and tantalum pentoxide according to the stoichiometric ratio (x +4y +5z is 15), putting the weighed materials into a ball milling tank, adding deionized water, and carrying out ball milling for 12 hours to obtain mixed slurry A;
taking out the mixture slurry A, putting the mixture slurry A into an oven, drying the mixture slurry A for 2 hours to obtain a dried material B;
taking the material B out, putting the material B into a box-type furnace, pre-sintering the material B for 2 hours at 800 ℃, and then cooling the material B to obtain a material C;
step (4), taking out the material C, putting the material C into a grinder, and pressing the material C into a billet D under the pressure of 2 kg;
step (5), treating the sagger at high temperature in advance, adopting a zirconia sagger, uniformly scattering lithium carbonate powder at the bottom, then pretreating at high temperature in an air atmosphere, wherein the temperature is 1300 ℃ for 4 hours, then placing the briquette D into a specially-treated closed sagger, and sintering for 12 hours at 1200 ℃; then cooling to obtain a billet E;
and (6) ball-milling and crushing the compact E to obtain a final product, namely a garnet structure LixLa3ZryTazO12(x +4y +5z 15) powder.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (4)

1. A preparation method for synthesizing garnet structure material by a solid phase method is characterized by comprising the following steps: the method comprises the following steps:
step (1) according to LixLa3ZryTazO12Weighing equal and corresponding parts by weight of lithium carbonate, lanthanum oxide, zirconium oxide and tantalum pentoxide according to the stoichiometric ratio (x +4y +5z is 15), putting the weighed parts into a ball milling tank, and adding deionized water to obtain mixed slurry A;
taking out the mixture slurry A, putting the mixture slurry A into an oven, drying the mixture slurry A to obtain a dried material B;
taking the material B out, putting the material B into a box-type furnace for pre-sintering, and then cooling to obtain a material C;
step (4), taking out the material C and putting the material C into a grinder; pressing under a pressure of 2kg to form a briquette D;
step (5), treating the sagger at high temperature in advance, adopting the sagger made of zirconia, uniformly scattering lithium carbonate powder at the bottom, then pretreating at high temperature in an air atmosphere, wherein the temperature is 1300 ℃ for 4 hours, placing the briquette D into a specially treated closed sagger for secondary sintering, and then cooling to obtain a briquette E;
and (6) ball-milling and crushing the compact E to obtain a final product, namely a garnet structure LixLa3ZryTazO12(x +4y +5z 15) powder.
2. The method of claim 1, wherein the garnet structure is synthesized by a solid phase method, and the method comprises the following steps: the ball milling time in the step (1) is 6-12 hours.
3. The method of claim 1, wherein the garnet structure is synthesized by a solid phase method, and the method comprises the following steps: the sintering temperature in the step (3) is 600-800 ℃, and the time is 2-4 hours.
4. The method of claim 1, wherein the garnet structure is synthesized by a solid phase method, and the method comprises the following steps: the temperature of the secondary sintering in the step (5) is 1000-1200 ℃, and the time is 6-12 hours.
CN202010285379.0A 2020-04-13 2020-04-13 Preparation method for synthesizing garnet structure material by solid phase method Pending CN111377736A (en)

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CN105336980A (en) * 2015-10-21 2016-02-17 上海动力储能电池***工程技术有限公司 Tantalum-doped cubic garnet structured Li7La3Zr<2-x>TaxO12 material synthesized via intermediate phase, and synthesis method thereof
CN107787529A (en) * 2015-04-14 2018-03-09 康宁股份有限公司 Oxidate for lithium garnet batch composition and its solid electrolyte diaphragm
CN108727025A (en) * 2017-04-17 2018-11-02 中国科学院上海硅酸盐研究所 Lithium garnet composite ceramics, Its Preparation Method And Use
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CN107787529A (en) * 2015-04-14 2018-03-09 康宁股份有限公司 Oxidate for lithium garnet batch composition and its solid electrolyte diaphragm
CN105244536A (en) * 2015-10-21 2016-01-13 上海动力储能电池***工程技术有限公司 Tantalum-doped cubic garnet structure Li7La3Zr2-xTaxO12 material and preparation method thereof
CN105336980A (en) * 2015-10-21 2016-02-17 上海动力储能电池***工程技术有限公司 Tantalum-doped cubic garnet structured Li7La3Zr<2-x>TaxO12 material synthesized via intermediate phase, and synthesis method thereof
CN108727025A (en) * 2017-04-17 2018-11-02 中国科学院上海硅酸盐研究所 Lithium garnet composite ceramics, Its Preparation Method And Use
CN108899581A (en) * 2018-07-26 2018-11-27 上海电力学院 A kind of preparation method of high-compactness carbuncle type inorganic solid electrolyte material

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