Method for preparing yttrium-oxide-stabilized hafnium oxide vacuum coating material

A vacuum coating and hafnium oxide technology, applied in the field of yttrium oxide stabilized hafnium oxide vacuum coating materials, can solve problems such as unevenness and unstable refractive index, and achieve the effects of inhibiting phase transition, eliminating volume effect and reducing the probability of defects.

Inactive Publication Date: 2015-03-25
SHANDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a vacuum coating material of yttrium oxide stabilized hafnium oxide, which solves the problems of instability and r

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: After mixing hafnium oxide and yttrium oxide at a molar ratio of 98%: 2%, add polyvinyl alcohol binder, shape the mixed powder, and pre-calcine at a temperature of 1260°C, then vacuum sintering. The vacuum degree of vacuum sintering is 1×10 －4 Pa, the maximum sintering temperature is 1700°C, and the holding time is 150 minutes. After cooling down, a stable and dense yttrium oxide-stabilized hafnium oxide vacuum coating material is obtained. According to XRD analysis, a solid solution is formed, and hafnium oxide exists in a tetragonal crystal form. Use yttrium oxide-stabilized hafnium oxide vacuum coating material to vapor-deposit a single-layer film on the BK7 glass substrate, the refractive index is stable, and the beam current of the electron gun in the vacuum chamber is stable.

Embodiment 2

[0018] Example 2: After mixing hafnium oxide and yttrium oxide in a molar ratio of 98%: 2%, add polyvinyl alcohol binder, shape the mixed powder, pre-calcine, the pre-calcination temperature is 1260 ° C, and then vacuum sintering. The vacuum degree of vacuum sintering is 1×10 －4 Pa, the maximum sintering temperature is 2200°C, and the holding time is 150 minutes. After cooling down, a stable and dense yttrium oxide-stabilized hafnium oxide vacuum coating material is obtained. According to XRD analysis, a solid solution is formed, and hafnium oxide exists in a tetragonal crystal form. Use yttrium oxide-stabilized hafnium oxide vacuum coating material to vapor-deposit a single-layer film on the BK7 glass substrate, the refractive index is stable, and the beam current of the electron gun in the vacuum chamber is stable.

Embodiment 3

[0019] Example 3: After mixing hafnium oxide and yttrium oxide in a molar ratio of 98%: 2%, add polyvinyl alcohol binder, shape the mixed powder, pre-calcine, the pre-calcination temperature is 1260 ° C, and then vacuum sintering. The vacuum degree of vacuum sintering is 1×10 －4 Pa, the maximum sintering temperature is 2000°C, and the holding time is 150 minutes. After cooling down, a stable and dense yttrium oxide-stabilized hafnium oxide vacuum coating material is obtained. According to XRD analysis, a solid solution is formed, and hafnium oxide exists in a tetragonal crystal form. Use yttrium oxide-stabilized hafnium oxide vacuum coating material to vapor-deposit a single-layer film on the BK7 glass substrate, the refractive index is stable, and the beam current of the electron gun in the vacuum chamber is stable.

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Abstract

The invention relates to a method for preparing an yttrium-oxide-stabilized hafnium oxide vacuum coating material. The method is characterized by comprising the following steps: 1) evenly mixing raw materials (hafnium oxide and yttrium oxide powder), wherein a molar ratio of hafnium oxide to yttrium oxide is (73-98): (2-27); adding a polyvinyl alcohol binder so that the powder materials are agglomerated and granulating to obtain granular material; (2) pre-sintering the granular material at a pre-sintering temperature of 1260 DEG C; and (3) sintering in a vacuum sintering furnace at the vacuum degree of 1*10<-2>-1*10<-4> Pa and the heating speed of 3-8 DEG C/min; when the temperature reaches 1700-2280 DEG C, carrying out heat preservation for more than 150 minutes, and then naturally cooling to room temperature. By the method, the problems of instability and non-uniform refractive index during the coating of traditional hafnium oxide coating material can be solved and meanwhile, the damage threshold of a hafnium oxide film is increased.

Description

technical field [0001] The invention belongs to the technical field of vacuum coating, in particular to a method for preparing a yttrium oxide-stabilized hafnium oxide vacuum coating material. Background technique [0002] To prepare laser thin films with high damage threshold, in the visible and near-infrared bands, high refractive index materials have undergone a process from TiO 2 (n=2.4), Ta 2 o 5 (n=2.1) to ZrO 2 (n=2.1), HfO 2 (n=2.0) Changes in transformation. Therefore, when people design and manufacture high-performance optical thin film elements with high threshold requirements, they often tend to use HfO 2 / SiO 2 The combination. [0003] In the UV band, the current research on ultraviolet film materials is mainly focused on excimer laser wavelengths 351nm (XeF), 308nm (XeCl), 248nm (KrF), 193nm (ArF) and Nd‐YAG laser triple frequency and quadruple Frequency (355nm and 266nm), the shorter the wavelength, the less membrane material available. [0004] HfO ...

Claims

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Application Information

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IPC IPC(8): C04B35/48C04B35/622
Inventor 吴师岗
Owner SHANDONG UNIV OF TECH
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