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BCT/BZT-system lead-free monocrystal epitaxial multilayer energy storage film and preparation method thereof

A lead-free single crystal and thin film technology, applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc., can solve problems such as hazards and restricted use fields, and achieve breakdown suppression, enhanced hindrance, and huge energy storage effect of density

Inactive Publication Date: 2018-12-21
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among the thin film energy storage materials, the lead lanthanum zirconate titanate ceramic (PLZT) system has the highest energy storage density, and its energy storage density reaches 67J / cm 3 However, due to the harm of lead poisoning to the natural environment and human body in production, its application field is limited

Method used

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  • BCT/BZT-system lead-free monocrystal epitaxial multilayer energy storage film and preparation method thereof
  • BCT/BZT-system lead-free monocrystal epitaxial multilayer energy storage film and preparation method thereof
  • BCT/BZT-system lead-free monocrystal epitaxial multilayer energy storage film and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0052] (1) First according to Ba 0.7 Ca 0.3 TiO 3 (BCT) and BaZr 0.2 Ti 0. 8O 3 The stoichiometric ratio of (BZT) weighs 4-5N grade BaCO 3 High purity powder, ZrO 2 High purity powder, TiO 2 Synthesis of BaZr from High Purity Powder 0.2 Ti 0.8 o 3 (BZT) ceramic target mixture, weigh BaCO 3 High purity powder, CaCO 3 High purity powder and TiO 2 Synthetic Ba from High Purity Powder 0.7 Ca 0.3 TiO 3 (BCT) ceramic target mixture; each target mixture is sequentially subjected to ball milling, pre-sintering, secondary ball milling, granulation, molding and sintering processes to obtain sheet-shaped BCT and BZT ceramic targets. The process parameters of ball milling and secondary ball milling are the same, specifically: the mass ratio of ball stone, mixture and alcohol is 2:1:1, the ball milling speed is 400r / min, and the ball milling time is 6h; the pre-sintering temperature is 900℃, pre-sintering The sintering time is 4h; it is formed by a tablet press, the pressur...

Embodiment 2

[0059] In the present embodiment, in step 2, the ultrasonic cleaning time is 3min; -5 mbar, when the substrate temperature is 850°C, pump the air pressure in the cavity to 10 -5 mbar; in step (5), a film with N=4 is prepared, the growth time of the single-layer BCT layer is 46min, and the thickness is 7.5nm; the growth time of the BZT layer is 126min, and the thickness is 17.5nm; it is formed after 4 cycles of staggered preparation Process film; the rest of the steps are the same as in Example 1.

Embodiment 3

[0061] In the present embodiment, in step 2, the ultrasonic cleaning time is 4min; -4 mbar, when the substrate temperature is 850°C, pump the air pressure in the cavity to 10 -5 mbar; in step (5), the film of N=8 is prepared, the growth time of the single-layer BCT layer is 23min, and the thickness is 3.8nm; the growth time of the single-layer BZT layer is 63min, and the thickness is 8.8nm; 8 cycles of staggered preparation Afterwards, the process film is formed; the rest of the steps are the same as in Example 1.

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Abstract

The invention discloses a BCT / BZT-system lead-free monocrystal epitaxial multilayer energy storage film and a preparation method thereof. The preparation method has the advantages that the radio frequency magnetron sputtering technology is adopted, a BCT / BZT multilayer film is obtained on a substrate through plasma bombardment of target materials, films with different periods but same thicknessesare prepared through regulation of the sputtering time of the two target materials, the obtained films can have epitaxial multilayer heterostructures, part of the current paths can be stopped at the interfaces, and breakdown is effectively suppressed; as the interfaces increase, the hindrance effect of internal current branches on materials is enhanced, so that the energy storage film prepared bythe method has extremely high energy efficiency while the huge energy storage density is achieved; the energy efficiency of 8-cycle samples is more than 65%, most of them are more than 70%, and the efficiency of 4-cycle samples can be more than 80%.

Description

technical field [0001] The invention relates to the field of energy storage thin film materials, in particular to a BCT / BZT system lead-free single crystal epitaxial multilayer energy storage thin film and a preparation method thereof. Background technique [0002] BT-based dielectric materials have been widely used in electronic material components in various fields. By doping with different elements or compounding with other materials, BTO-based dielectric materials have become an important research direction in the field of materials today. Among the thin film energy storage materials, the lead lanthanum zirconate titanate ceramic (PLZT) system has the highest energy storage density, and its energy storage density reaches 67J / cm 3 However, due to the harm of lead poisoning to the natural environment and human body in production, its application field is limited. (Ba,Ca)(Zr,Ti)O 3 (BCZT) system ceramic materials are a non-negligible branch of BT-based materials. At the s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/32C30B23/02
CPCC30B23/02C30B29/32
Inventor 刘明孙梓雄
Owner XI AN JIAOTONG UNIV
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