Sandwich-structured dielectric materials for pulse energy storage as well as preparation method and application thereof

Patent metadata

Field	Value
Publication number	US-11735360-B2
Application number	US-202117203230-A
Country	US
Kind code	B2
Filing date	Mar 16, 2021
Priority date	Mar 17, 2020
Publication date	Aug 22, 2023
Grant date	Aug 22, 2023

Abstract

A sandwich-structured dielectric material for pulse energy storage is provided as well as a preparation method thereof. Employing a sandwich structure and combining the properties of ceramic-glass materials prepares a high performance dielectric material for pulse energy storage, in which the ceramic dielectric is core-shell structured powder of BaxSr1-xTiO3 coated with SiO2, and the glass material is alkali-free glass AF45, of which the chemical composition is 63% SiO2-12% BaO-16% B2O3-9% Al2O3. AF45 alkali-free glass paste is spin-coated on both sides of the ceramic and calcined to get a layer-structured material of glass-ceramic-glass.

First claim

What is claimed is:

1. A method of preparing a sandwich-structured dielectric material for pulse energy storage, wherein, comprising the following steps:
(1) dispersing Ba x Sr 1-x TiO 3 powder in ethyl alcohol, adding glacial acetic acid and polyvinylpyrrolidone, mixing uniformly, then adding ethyl orthosilicate to adjust pH, reacting at 30-60° C. with stirring for 12-24 hours, getting a suspension, which is filtered and dried to get BST@SiO 2 powder;
wherein x represents the molar fraction of Ba, 0.2≤x≤0.6, and BST@SiO 2 identifies a core-shell structure with BST as a core of the core-shell structure and SiO 2 as a shell of the core-shell structure;
(2) mixing the BST@SiO 2 powder with a binder uniformly, molding at 150-200 MPa, discharging, and finally calcining at 1100-1200° C. to get ceramic blocks;
(3) mixing SiO 2 , BaCO 3 , B 2 O 3 and Al 2 O 3 , ball-milling uniformly, then sieving, drying, melting at 1400-1500° C. for 2-4 hours, quenching, to get frits; adding water into the frits and then ball-milling and drying again, to get AF45 glass; wherein the chemical composition of the AF45 glass in molar contents is 63% SiO 2 -12% BaO-16% B 2 O 3 -9% Al 2 O 3 ;
(4) adding the AF45 glass and carboxymethyl cellulose into water, to get AF45 glass paste, which is spin-coated onto both sides of ceramic blocks, dried and then calcined, to get a sandwich-structured material of glass-ceramic-glass.

2. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 1 , wherein, the weight of ethyl alcohol in step (1) is 100-200 times that of Ba x Sr 1-x TiO 3 powder; the weight of glacial acetic acid is 4-6 times that of Ba x Sr 1-x TiO 3 powder; the weight of polyvinylpyrrolidone is 50-100% that of Ba x Sr 1-x TiO 3 powder; and the weight of ethyl orthosilicate is 2-8% that of Ba x Sr 1-x TiO 3 powder.

3. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 1 , wherein, the conditions for calcination in step (4) are: calcination at 800-1000° C. for 10-30 min.

4. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 2 , wherein, the conditions for calcination in step (4) are: calcination at 800-1000° C. for 10-30 min.

5. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 1 , wherein, the adjustment of pH in step (1) means adjusting the pH to 9-11 with aqueous ammonia; and the time for calcination in step (2) is 2-4 hours.

6. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 2 , wherein, the adjustment of pH in step (1) means adjusting the pH to 9-11 with aqueous ammonia; and the time for calcination in step (2) is 2-4 hours.

7. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 1 , wherein, the binder in step (2) is PVA; the weight of the binder is 1-3% that of the BST@SiO 2 powder; the discharging conditions are: holding at 500-600° C. for 4-8 hours.

8. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 2 , wherein, the binder in step (2) is PVA; the weight of the binder is 1-3% that of BST@SiO 2 powder; the discharging conditions are: holding at 500-600° C. for 4-8 hours.

9. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 1 , wherein, the Ba x Sr 1-x TiO 3 powder in step (1) is prepared by the method below:
mixing BaCO 3 , SrCO 3 and TiO 2 uniformly at a molar ratio of x:(1−x):1, adding NaCl and mixing uniformly, and ball-milling, sieving, drying, then calcining at 1000-1200° C. for 2-4 hours, filtering and drying to get Ba x Sr 1-x TiO 3 powder; wherein the weight of NaCl is 5-15 times the total weight of BaCO 3 , SrCO 3 and TiO 2 ;
absolute ethyl alcohol is used as the medium for ball-milling, wherein the added amount of the absolute ethyl alcohol is 1-2 times the total weight of BaCO 3 , SrCO 3 and TiO 2 ; the ball-milling conditions are: ball-milling at 400-500 r/min for 4-8 hours; and the sieving mesh count is 100-200 meshes.

10. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 2 , wherein, the Ba x Sr 1-x TiO 3 powder in step (1) is prepared by the method below:
mixing BaCO 3 , SrCO 3 and TiO 2 uniformly at a molar ratio of x:(1−x): 1 , adding NaCl and mixing uniformly, and ball-milling, sieving, drying, then calcining at 1000-1200° C. for 2-4 hours, filtering and drying to get Ba x Sr 1-x TiO 3 powder; wherein the weight of NaCl is 5-15 times the total weight of BaCO 3 , SrCO 3 and TiO 2 ;
absolute ethyl alcohol is used as the medium for ball-milling, wherein the added amount of the absolute ethyl alcohol is 1-2 times the total weight of BaCO 3 , SrCO 3 and TiO 2 ; the ball-milling conditions are: ball-milling at 400-500 r/min for 4-8 hours; and the sieving mesh count is 100-200 meshes.

11. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 1 , wherein, the density of AF45 glass in the AF45 glass paste of step (4) is 1-1.5 g/cm 3 ; the spin-coating conditions are: the rotation rate is 100-200 rpm, and the duration time is 10-30 s; the weight of carboxymethyl cellulose is 1-2% that of AF45 glass.

12. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 2 , wherein, the density of AF45 glass in the AF45 glass paste of step (4) is 1-1.5 g/cm 3 ; the spin-coating conditions are: the rotation rate is 100-200 rpm, and the duration time is 10-30 s; the weight of carboxymethyl cellulose is 1-2% that of AF45 glass.

13. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 1 , wherein, the conditions for uniform ball-milling of SiO 2 , BaCO 3 , B 2 O 3 and Al 2 O 3 in step (3) are: using absolute ethyl alcohol as the medium, and ball-milling at 400-500 r/min for 4-8 hours, wherein the weight of the absolute ethyl alcohol is 1-2 times the total weight of SiO 2 , BaCO 3 , B 2 O 3 and Al 2 O 3 ; the conditions for ball-milling again after adding water into the frits are: ball-milling at 400-500 r/min for 4-8 hours; the sieving mesh count is 100-200 meshes.

14. The method of preparing a sandwich-structured dielectric material for pulse energy storage according to claim 2 , wherein, the conditions for uniform ball-milling of SiO 2 , BaCO 3 , B 2 O 3 and Al 2 O 3 in step (3) are: using absolute ethyl alcohol as the medium, and ball-milling at 400-500 r/min for 4-8 hours, wherein the weight of the absolute ethyl alcohol is 1-2 times the total weight of SiO 2 , BaCO 3 , B 2 O 3 and Al 2 O 3 ; the conditions for ball-milling again after adding water into the frits are: ball-milling at 400-500 r/min for 4-8 hours; the sieving mesh count is 100-200 meshes.

Assignees

• Univ South China Tech
• South China Univ Of Techology

Inventors

• Lv Ming
• Li Ruqiang
• Wei Yani
• Lai Qiutan

Classifications

• H01G4/1227 Primary

  based on alkaline earth titanates · CPC title

• C03C10/0018

  containing SiO2, Al2O3 and monovalent metal oxide as main constituents · CPC title

• C03C12/00

  Powdered glass (C03C8/02 takes precedence); Bead compositions · CPC title

• C04B35/465

  based on alkaline earth metal titanates · CPC title

• C04B35/468 Primary

  based on barium titanates · CPC title