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A preparation method of zirconium dioxide film with controllable crystal form and thickness

A zirconia and zirconia technology, applied in metal material coating process, vacuum evaporation coating, coating and other directions, can solve the problem of long sample preparation time, and achieve short sample preparation cycle, simple experimental operation and shortening. effect of time

Active Publication Date: 2021-10-26
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional zirconia thin film preparation method generally only obtains one crystal form in one sample preparation, but the number of samples required for systematic research on zirconia thin film materials is relatively large, so the sample preparation time required is longer

Method used

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  • A preparation method of zirconium dioxide film with controllable crystal form and thickness
  • A preparation method of zirconium dioxide film with controllable crystal form and thickness
  • A preparation method of zirconium dioxide film with controllable crystal form and thickness

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] (1) Cleaning the glass substrate: Put the glass substrate into a beaker, use isopropanol, deionized water, deionized water, and isopropanol to sonicate for 15 minutes in sequence, put it in an oven for drying, and then take it out.

[0022] (2) Pulsed laser deposition of zirconia thin film: choose a zirconia target with a purity of 99.99%, and place a glass substrate according to figure 1 The position is fixed on the substrate and put into the vacuum chamber, and the vacuum chamber is pumped to 5×10 -4 Pa, adjust the distance between the target and the substrate to be 7cm, set the pulse frequency to 5Hz, and the laser energy to be 300mJ, and use a diamond-shaped laser spot with a vertical diagonal longer than a horizontal diagonal to irradiate the target (the shape of the laser spot and the base The placement of the chip on the substrate is as follows figure 1 shown), and after 2 minutes of pre-deposition, set the number of pulses to 27000 for deposition.

[0023] (3)...

Embodiment 2

[0027] (1) Cleaning the glass substrate: Put the glass substrate into a beaker, use isopropanol, deionized water, deionized water, and isopropanol to sonicate for 15 minutes in sequence, put it in an oven for drying, and then take it out.

[0028] (2) Pulsed laser deposition of zirconia thin film: choose a zirconia target with a purity of 99.99%, and place a glass substrate according to figure 1 The position is fixed on the substrate and put into the vacuum chamber, and the vacuum chamber is pumped to 5×10 -4 Pa, adjust the distance between the target and the substrate to 4.5cm, set the pulse frequency to 5Hz, and the laser energy to 300mJ, irradiate the target with a diamond-shaped laser spot whose vertical diagonal is longer than the horizontal diagonal, and set after 2 minutes of pre-deposition The number of pulses was 12000 for deposition.

[0029] (3) Annealing treatment: place the deposited zirconia film in an air environment for thermal annealing, the annealing tempera...

Embodiment 3

[0033] (1) Cleaning the glass substrate: Put the glass substrate into a beaker, use isopropanol, deionized water, deionized water, and isopropanol to sonicate for 15 minutes in sequence, put it in an oven for drying, and then take it out.

[0034] (2) Pulsed laser deposition of zirconia thin film: choose a zirconia target with a purity of 99.99%, and place a glass substrate according to figure 1 The position is fixed on the substrate and put into the vacuum chamber, and the vacuum chamber is pumped to 5×10 -4 Pa, adjust the distance between the target and the substrate to 5cm, set the pulse frequency to 5Hz, and the laser energy to 200mJ, use a diamond-shaped laser spot with a vertical diagonal longer than the horizontal diagonal to irradiate the target, and set the pulse after pre-deposition for 2 minutes The number is 18000 to be deposited.

[0035] (3) Annealing treatment: place the deposited zirconia film in an air environment for thermal annealing, the annealing temperat...

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Abstract

The invention belongs to the technical field of film material preparation, and discloses a preparation method of a zirconium dioxide film with controllable crystal form and thickness. With zirconia as the target material, place the glass substrate on the substrate, and pump the vacuum chamber to 2×10 ‑4 ~5×10 ‑4 Pa, adjust the distance between the target and the substrate, set the pulse frequency to 4-6Hz, the laser energy to 150-350mJ, use a non-circular laser spot to irradiate the target, and set the pulse number to 10000 after pre-deposition for 1-3min ~30,000 times of continuous deposition, and then thermal annealing in the air environment, the annealing temperature is 300-400 ° C, to obtain a zirconia film with controllable crystal form and thickness. The invention regulates the crystal form of the thin film through the shape of the laser spot and the position of the substrate, and adjusts the thickness through the number of pulses during deposition and the distance between the target and the substrate, so that zirconia films with different crystal forms and thicknesses can be obtained in one sample preparation.

Description

technical field [0001] The invention belongs to the technical field of film material preparation, and in particular relates to a method for preparing a zirconium dioxide film with controllable crystal form and thickness. Background technique [0002] Zirconia (ZrO 2 ) is a dielectric material with superior performance, and its dielectric constant is much higher than that of traditional silicon oxide (SiO 2 ), which is expected to replace silicon oxide as the gate dielectric material of transistors. Under normal conditions, zirconia has two crystal forms, monoclinic and tetragonal, and the dielectric properties of zirconia films with different crystal forms are also different. The existing methods for preparing tetragonal zirconia films generally require high-temperature heat treatment, but tetragonal zirconia films will undergo martensitic transformation into monoclinic zirconia films at high temperatures (>800°C). The traditional zirconia thin film preparation method ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/28C23C14/08C23C14/58
CPCC23C14/083C23C14/28C23C14/5806
Inventor 姚日晖黎群杰宁洪龙邱斌符晓陈俊龙张观广袁炜键周尚雄彭俊彪
Owner SOUTH CHINA UNIV OF TECH
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