CN110983280A

CN110983280A - Preparation of W-doped ZrO by ion beam assisted deposition process2Method for making thin film

Info

Publication number: CN110983280A
Application number: CN201911353350.5A
Authority: CN
Inventors: 沈洪雪; 姚婷婷; 李刚; 彭塞奥; 杨扬
Original assignee: CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
Current assignee: CNBM Bengbu Design and Research Institute for Glass Industry Co Ltd
Priority date: 2019-12-25
Filing date: 2019-12-25
Publication date: 2020-04-10

Abstract

The invention discloses a method for preparing W-doped ZrO by an ion beam assisted deposition process₂A method of making a film comprising the steps of: a. cleaning a substrate by using a monocrystalline silicon wafer as the substrate, and removing dirt on the surface of the substrate; b. putting a substrate into a chamber of an ion beam assisted deposition system, wherein the ion beam assisted deposition system adopts a tungsten target and a zirconium target; c. starting an ion beam auxiliary deposition system, firstly using a tungsten target to deposit a tungsten oxide film on the surface of a substrate; then, depositing a zirconium oxide film on the surface of the tungsten oxide film by using a zirconium target; d. putting the substrate deposited with the film into an annealing furnace, and annealing for 3 hours in an oxygen atmosphere at 1000 ℃ to uniformly diffuse tungsten oxide in the zirconium oxide film; then cooling to normal temperature along with the furnace to obtain the W-doped ZrO₂A film; the method can be used for ZrO with any W doping amount₂The preparation of the film is realized, and the additional preparation of a mixed target material is not needed, so that the method is simple and has strong controllability.

Description

Preparation of W-doped ZrO by ion beam assisted deposition process2Method for making thin film

Technical Field

The invention relates to the technical field of sputtering deposition coating, in particular to a method for preparing W-doped ZrO by an ion beam assisted deposition process₂A method of making a thin film.

Background

ZrO₂Because of its characteristics of high hardness, high-temperature conductivity, high chemical stability, etc., it is widely used in the fields of electronic components, etc. There are studies showing that: a certain amount of W doping can be in ZrO₂Certain zirconium tungstate is formed in the film, and the doped zirconia film has a wider negative thermal expansion temperature range; higher coefficient, etc., to make the doped ZrO₂The film is more widely applied.

The traditional magnetron sputtering method for preparing the W-doped ZrO2 film utilizes a zirconium oxide target material containing a certain amount of tungsten oxide to carry out sputtering, the doping amount in the prepared doped film is a constant value, and the method has the defect of flexibly preparing zirconium oxide films with different doping amounts.

Disclosure of Invention

The invention aims to provide a method for preparing a W-doped ZrO2 thin film by an ion beam assisted deposition process, which can perform ZrO with any W doping amount₂The preparation of the film is realized, and the additional preparation of a mixed target material is not needed, so that the method is simple and has strong controllability.

The technical scheme adopted by the invention for solving the technical problems is as follows:

preparation of W-doped ZrO by ion beam assisted deposition process₂A method of making a film comprising the steps of:

a. cleaning a substrate by using a monocrystalline silicon wafer as the substrate, and removing dirt on the surface of the substrate;

b. putting a substrate into a chamber of an ion beam assisted deposition system, wherein the ion beam assisted deposition system adopts a tungsten target and a zirconium target;

c. starting an ion beam auxiliary deposition system, firstly using a tungsten target to deposit a tungsten oxide film on the surface of a substrate; then, depositing a zirconium oxide film on the surface of the tungsten oxide film by using a zirconium target;

d. placing the substrate with deposited film into annealing furnace, and introducing oxygen at 1000 deg.CAnnealing for 3 hours in the atmosphere to ensure that the tungsten oxide is uniformly diffused in the zirconium oxide film; then cooling to normal temperature along with the furnace to obtain the W-doped ZrO₂A film.

The invention has the beneficial effects that:

firstly, two independent targets are adopted, each target can be independently controlled, and the ion beam assisted deposition process is simple, high in efficiency and strong in controllability.

And secondly, the thickness of the film can be changed by only changing the technological parameters of the target material in the ion beam assisted deposition process, so that the doping amount of W is changed, and the preparation is flexible and convenient.

Thirdly, annealing in oxygen atmosphere at 1000 ℃ can redistribute and uniformly diffuse the tungsten oxide in the zirconium oxide film.

Fourthly, the tungsten and zirconium mixed target does not need to be manufactured independently.

Drawings

The invention is further illustrated with reference to the following figures and examples:

FIG. 1 is a schematic of the present invention.

Detailed Description

As shown in FIG. 1, the present invention provides an ion beam assisted deposition process for preparing W-doped ZrO₂A method of making a film comprising the steps of:

a. cleaning a substrate 1 by using a monocrystalline silicon wafer as the substrate 1, and removing dirt on the surface of the substrate; the substrate can be cleaned by ultrasonic waves such as acetone, alcohol, deionized water and the like to remove impurities and oil stains on the surface of the substrate, and the substrate is dried by hot air for later use;

b. putting the substrate 1 into a chamber of an ion beam assisted deposition system, wherein the ion beam assisted deposition system adopts a tungsten target and a zirconium target; the purity of the tungsten target and the purity of the zirconium target are both 99.99%:

c. starting the ion beam assisted deposition system, firstly using tungsten target, vacuumizing until the vacuum degree reaches 4.0 x 10^-5When Pa is needed, argon is introduced, argon ions bombard the tungsten target to achieve the purposes of removing oxides on the surface of the tungsten target and activating the target material, and then a tungsten oxide film 2 is deposited on the surface of the substrate 1;

then, the substrate 1 is turned to a zirconium target, and a zirconium oxide film 3 is deposited on the surface of the tungsten oxide film 2;

d. taking out the substrate 1 deposited with the film, putting the substrate into an annealing furnace, and annealing the substrate for 3 hours in an oxygen atmosphere at 1000 ℃ to uniformly diffuse tungsten oxide in the zirconium oxide film; then cooling to normal temperature along with the furnace to obtain the W-doped ZrO₂A film.

The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modification, equivalent replacement, equivalent change and modification made to the above embodiments according to the technical essence of the present invention are still within the scope of the protection of the technical solution of the present invention.

Claims

1. Preparation of W-doped ZrO by ion beam assisted deposition process₂A method of making a film, comprising the steps of:

d. putting the substrate deposited with the film into an annealing furnace, and annealing for 3 hours in an oxygen atmosphere at 1000 ℃ to uniformly diffuse tungsten oxide in the zirconium oxide film; then cooling to normal temperature along with the furnace to obtain the W-doped ZrO₂A film.