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A kind of single crystal lead zirconate titanate thin film and its preparation and application

A technology of lead zirconate titanate and thin film, which is applied in the field of single crystal lead zirconate titanate thin film and its preparation, which can solve the problems affecting microstructure and performance, unable to thick thin film, and unable to obtain structurally controllable thin film.

Active Publication Date: 2022-05-10
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, lead zirconate titanate single crystal thin films can only be prepared by using vapor phase deposition methods such as pulsed laser deposition (PLD) with high experimental requirements and high cost. However, it is limited by the weak spatial diffusion ability and Higher cost, the PLD method cannot form a thicker film at a higher growth rate, and the thickness of the film is difficult to achieve a micron level; moreover, the reaction temperature (>600°C) of the PLD method and other vapor deposition methods is much higher than The Curie temperature of lead zirconate titanate (300-450°C), the unavoidable phase transition process from paraelectric phase to ferroelectric phase during the process of cooling down to room temperature during preparation, and the high volatility of Pb may all contribute to the The introduction of defects in the film affects the microstructure and properties, making it difficult to control the structure and properties of the film, so that it is impossible to obtain a film with a controllable structure or a specific structure

Method used

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  • A kind of single crystal lead zirconate titanate thin film and its preparation and application
  • A kind of single crystal lead zirconate titanate thin film and its preparation and application
  • A kind of single crystal lead zirconate titanate thin film and its preparation and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0074] 1) Weigh 0.3 mmol of zirconium oxychloride octahydrate and place it in a beaker, add 20 mL of ethylene glycol methyl ether to dissolve, and fully stir for 20 min to obtain a solution with a molar concentration of zirconium ions of 15 mmol / L;

[0075] 2) Under stirring, add 3.6mmol of lead nitrate to the solution prepared in step 1), and stir for 20 minutes until the solid is completely dissolved; then add 2.7mmol of tetra-n-butyl titanate, and stir for 10 minutes to obtain a mixed solution; , the molar ratio of the sum of zirconium and titanium elements to the lead element is 1:1.2, and the molar ratio of zirconium and titanium elements in the sum of zirconium and titanium elements is 0.1 (in terms of mole percentage, it is 10mol%);

[0076] 3) Add the mixed solution prepared in step 2) dropwise to 75ml of ammonia water (ammonia in excess), let it stand for 20min (complete precipitation); then, wash the precipitate with 50ml of deionized water, filter, repeat washing and...

Embodiment 2

[0091] 1) Weigh 0.10 mmol of zirconium oxychloride octahydrate and place it in a beaker, add 15 mL of ethylene glycol methyl ether to dissolve, and fully stir for 10 min to obtain a solution with a zirconium ion molar concentration of 6.67 mmol / L;

[0092] 2) Under stirring, add 2.4 mmol of lead nitrate to the solution prepared in step 1), fully stir for 10 minutes until the solid is completely dissolved, then add 1.90 mmol of tetra-n-butyl titanate, and stir for 10 minutes to obtain a mixed solution; Wherein, the molar ratio of the sum of zirconium and titanium elements to the lead element is 1:1.2, and the molar ratio of zirconium elements in the sum of zirconium and titanium elements is 0.05 (5mol% in mole percent);

[0093] 3) Add the mixed solution prepared in step 2) dropwise to 50ml ammonia water (excess ammonia water), let it stand for 20min (complete precipitation); then, wash the precipitate with 50ml deionized water, filter, repeat washing and filtering 5 times , to...

Embodiment 3

[0116] 1) Weigh 0.7 mmol of zirconium oxychloride octahydrate and place it in a beaker, add 20 mL of ethylene glycol methyl ether to dissolve, and fully stir for 20 min to obtain a solution with a molar concentration of zirconium ions of 35 mmol / L;

[0117] 2) Under stirring, add 5.25 mmol of lead nitrate to the solution prepared in step 1), fully stir for 20 minutes until the solid is completely dissolved, then add 2.8 mmol of tetra-n-butyl titanate, and stir for 10 minutes to obtain a mixed solution; Wherein, the molar ratio of the sum of zirconium and titanium elements to the lead element is 1:1.5, and the molar ratio of zirconium elements in the sum of zirconium and titanium elements is 0.2 (20mol% in mole percent);

[0118] 3) Add the mixed solution prepared in step 2) dropwise to 100ml ammonia water (ammonia water is excessive), let it stand for 20min (complete precipitation); then, wash the precipitate with 50ml deionized water, filter, repeat washing and filtering 5 tim...

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Abstract

The invention discloses a single crystal lead zirconate titanate film and its preparation and application. The film is a large-area high-quality lead zirconate titanate single crystal film epitaxially grown on a strontium niobate titanate substrate, with an area close to cm 2 The macro-level size, the thickness can reach the micron level, and the ratio of zirconium ions and titanium ions changes in a gradient in the direction of ferroelectric polarization. The single crystal lead zirconate titanate thin film is prepared by combining co-precipitation reaction and hydrothermal reaction in an environment far below the Curie temperature. The process is simple, controllable, low cost, and easy to scale production. Fields such as ferroelectric memory, pyroelectric sensor and electro-optic detector have broad potential application prospects.

Description

technical field [0001] The invention belongs to the field of functional materials and preparation, and in particular relates to a single crystal lead zirconate titanate film and its preparation. Background technique [0002] In the information age dominated by big data, micro-nano electronic devices pursue high-density, low-loss information storage, fast response, and low-interference information detection. The spontaneous polarization direction and physical and chemical properties regulated by external fields have broad application prospects in the fields of information storage and signal detection, and have become a hot spot in the development and research of functional thin film materials. [0003] Lead zirconate titanate (PbZr x Ti 1-x o 3 , PZT) is a tetragonal ferroelectric lead titanate (PbTiO 3 ) and rhombohedral opposite ferroelectric lead zirconate (PbZrO 3 ) is a perovskite ferroelectric oxide solid solution that is soluble in any ratio, and has excellent fer...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C30B29/32C30B19/00C30B19/12
CPCC30B29/32C30B19/00C30B19/12
Inventor 韩高荣林宸任召辉陈嘉璐周迪逵曹海文
Owner ZHEJIANG UNIV
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