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PbHfO3-based anti-ferroelectric material based on film rolling process, preparation method and applications thereof

An antiferroelectric and hafnium acid technology, applied in circuits, capacitors, electrical components, etc., can solve the problems of high saturation polarization, low breakdown field strength, and poor compactness, so as to improve breakdown resistance and energy storage Density, preparation method is simple and easy, and the effect of good application value

Inactive Publication Date: 2019-11-19
TONGJI UNIV
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AI Technical Summary

Problems solved by technology

At present, the energy storage density of reported antiferroelectric ceramic blocks is generally low. Due to the large volume of solid-phase synthesized ceramic blocks, the probability of internal defects increases, resulting in low breakdown field strength, and the energy storage performance cannot be improved.
Compared with other preparation processes, tape casting process and screen printing process can also prepare antiferroelectric materials, but more binders are added. During the paper burning process, due to the more volatilization holes of the binders, the compactness is poor, and it is harmful to the process. higher environmental requirements
[0004] At present, the research on antiferroelectrics mainly focuses on lanthanum-modified lead zirconate titanate-based antiferroelectric materials with mature preparation technology and excellent energy storage performance, but similar lead hafnate (PbHfO 3 )-based antiferroelectric materials have rarely been reported on their energy storage properties.
Although as early as 1953 PbHfO 3 was confirmed as an antiferroelectric, but about PbHfO 3 Literature reports on antiferroelectrics are still scarce
PbHfO 3 Ceramics have high AFE-FE phase change switching field (EF>200kV / cm), high saturation polarization (P max Up to 45μC / cm 2 ), high breakdown field strength (Eb up to 270kV / cm), and relatively small hysteresis (ΔE~46kV / cm), about PbHfO 3 There are relatively few introductions to the preparation process of ceramics. At present, most of them use the traditional solid-phase synthesis method, but the samples prepared by the solid-phase synthesis method have low energy storage density, which limits the further application of antiferroelectric materials.

Method used

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Examples

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Embodiment 1

[0033] Use the purity of analytically pure PbO, HfO 2 , according to PbHfO 3 The stoichiometric ratio of Pb and Hf in the mixture is weighed and batched, and the prepared material is put into a ball mill tank, and the ratio of ball to material to medium is 2:1:1. The ball milling time is 24 hours. After ball milling, take it out and dry it, pre-burn it at 850°C for 2 hours, then ball mill it again for 12 hours, dry it and sieve it. Then add 25% binder, firstly rough roll repeatedly for 1 hour on the film rolling machine, and finally finish roll to 0.26mm, and cut into green sheets of 10mm*10mm. Finally, place the debonded biscuit in a closed aluminum oxide dry pot, and place a thin aluminum oxide plate on top of the sample to avoid bending, and sprinkle an appropriate amount of lead oxide powder around it to avoid the loss of lead. Put the alumina crucible containing the biscuit into the muffle furnace, debond at 600°C for 4 hours, the heating rate is 1°C per minute, and the...

Embodiment 2

[0035] The purity is analytically pure PbO, La 2 o 3 , HfO 2 , SnO 2 According to (Pb 0.97 La 0.02 )(Hf 0.45 sn 0.55 ) 0.995 o 3 The stoichiometric ratio of Pb, La, Hf and Sn in the medium is weighed and batched, and the prepared materials are put into the ball mill tank, and the ratio of ball to material to medium is 2:1:1. The ball milling time is 24 hours. After ball milling, take it out and dry it, pre-burn it at 850°C for 2 hours, then ball mill it again for 12 hours, dry it and sieve it. Then add 25% binder, firstly rough roll repeatedly for 1 hour on the film rolling machine, and finally finish roll to 0.26mm, and cut into green sheets of 10mm*10mm. Finally, place the debonded biscuit in a closed aluminum oxide dry pot, and place a thin aluminum oxide plate on top of the sample to avoid bending, and sprinkle raw materials of the same composition around it to further prevent lead from being exposed to high temperatures. When the volatilization. Put the alumina...

Embodiment 3

[0037] A lead hafnate-based antiferroelectric material based on rolling film technology, with (Pb 0.04 La 0.04 )(Hf 0.26 sn 0.68 Ti 0.06 )O 3 As the substrate, the preparation method is as follows:

[0038] 1) lead oxide, hafnium oxide, lanthanum oxide, tin oxide and titanium oxide according to (Pb 0.04 La 0.04 )(Hf 0.26 sn 0.68 Ti 0.06 )O 3 The corresponding stoichiometric ratio of Pb, Hf, La, Sn, Ti in the mixture is mixed to obtain the mixed material, and a ball milling process is carried out in a ball mill tank;

[0039] 2) Dry the primary ground material at 130°C, and keep the temperature at 850°C for 2 hours for pre-calcination;

[0040] 3) The pre-calcined material is first crushed by a mortar, and then ball milled for a second time in a ball mill tank, and dried at 130°C;

[0041] 4) Mix the dried material with the binder at a mass ratio of 0.2:1, firstly carry out rough rolling on a film rolling machine for 1 hour, then finish rolling to the required thick...

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Abstract

The invention relates to a PbHfO3-based anti-ferroelectric material based on a film rolling process, a preparation method and applications thereof, wherein the PbHfO3-based anti-ferroelectric materialhas a chemical general formula of (Pb1-3z / 2Laz)(Hf1-x-ySnxTiy)O3, z is more than 0 and is less than or equal to 0.04, x is more than 0 and is less than or equal to 1.0, and y is more than 0 and is less than 1.0. The preparation method comprises: 1) carrying out mixing grinding on corresponding metal oxides according to the corresponding stoichiometric ratio of (Pb1-3z / 2Laz)(Hf1-x-ySnxTiy)O3; 2) drying, and pre-firing; 3) carrying out secondary grinding, and drying; 4) mixing with a binder, and carrying out rough rolling, finish rolling and cutting; and 5) carrying out binder discharge treatment and sintering treatment to prepare the PbHfO3-based anti-ferroelectric material. According to the present invention, the prepared PbHfO3-based anti-ferroelectric material can be used for preparingpulse power capacitors, energy storage capacitors and transducers; compared with the method in the prior art, the preparation method of the present invention has characteristics of simpleness, easy performing and convenient operation, and is suitable for batch production; and the sample of the present invention has characteristics of adjustable size, wide application range, strong breakdown resistance, high energy storage density and good application value.

Description

technical field [0001] The invention belongs to the technical field of electronic materials, and relates to a lead hafnate-based antiferroelectric material based on a rolled film process, a preparation method and an application thereof. Background technique [0002] In recent years, pulse power technology has been widely used in the fields of medical care, laser technology and pollution control, and energy storage capacitors, as the core component of pulse power systems, are the research focus of scientific researchers. Common dielectric materials for energy storage capacitors include ferroelectric materials, antiferroelectric materials, and linear dielectric materials. Compared with ferroelectrics and linear dielectric materials, antiferroelectrics are considered to be excellent energy storage materials due to their unique AFE-FE phase transition and better energy storage and charge-discharge characteristics. [0003] In terms of energy storage applications, in order to in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B35/48C04B35/622C04B35/626H01G4/12
CPCC04B35/48C04B35/622C04B35/62645C04B35/62675C04B2235/3227C04B2235/3232C04B2235/3293C04B2235/3296C04B2235/6562C04B2235/6567H01G4/1209
Inventor 杨同青晁雯娜
Owner TONGJI UNIV
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