ZrOx for plating optical film and preparation method of ZrOx

An optical film and block technology, applied in the direction of zirconia, coatings, etc., can solve the problems of explosion, high technical requirements for reaction equipment and operation control, easy combustion and other problems, and achieve stable chemical properties, stability and consistency Good, stable evaporation effect

Active Publication Date: 2020-12-04
有研资源环境技术研究院(北京)有限公司
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  • Description
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Problems solved by technology

However, the metal zirconium powder used in the raw materials is a flammable, explosive and dangerous chemical, which is extremely prone to combustion or even explosion. The zirconium powder should be kept in water (not less than 25% water-wet passivation) during transportation and storage. When this process is used in batch preparation, it needs to solve the problems of the safety of raw materials and the stability of proportioning and metering.
Beijing Henglong Technology Co., Ltd. in its patent (201410841672.5) "a conductive zirconia rotating target and its preparation method", after mixing 93-98% zirconia powder with 2-7% carbon powder, at 1500-1700 Sintering in a hydrogen atmosphere at ℃ for 6-10 hours to prepare a conductive ZrOx rotating target, but the requirements for reaction equipment and operation control technology are relatively high when firing in a hydrogen atmosphere

Method used

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  • ZrOx for plating optical film and preparation method of ZrOx
  • ZrOx for plating optical film and preparation method of ZrOx
  • ZrOx for plating optical film and preparation method of ZrOx

Examples

Experimental program
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Effect test

Embodiment 1

[0035] use as figure 1 The process shown in the preparation of ZrO x : ZrH 2 Powder and ZrO 2 The powder is weighed according to the ratio of 2:5 by weight, and the mixing machine is used for mechanical mixing for 6 hours, and the mixed powder is mixed at 300 N / cm 2 The block is pressed under a certain pressure, and then the block material is crushed and sieved to make particles with a particle size of 1-3mm. -1 The solid-phase synthesis reaction was carried out under the condition of Pa for 6 hours, and cooled to room temperature under vacuum.

[0036] The material prepared by this method is a dark gray material (such as figure 2 shown), the density of the material tested by the drainage method is 5.0g / cm 3 , XRD analysis showed that the material was composed of a new compound Zr 3 O and some ZrO 2 composition. When in use, the ZrOx material is fully pre-melted first, and pre-melted in a water-cooled oxygen-free copper crucible. The pre-melting temperature is about 230...

Embodiment 2

[0038] use as figure 1 The process shown in the preparation of ZrO x : ZrH 2 Powder and ZrO 2 The powder is weighed according to the ratio of 2:3 by weight, and the ball mill is used for mechanical mixing for 4 hours, and the mixed powder is mixed by a hydraulic machine at 600N / cm 2 The block is pressed under a certain pressure, and the block material is crushed and sieved to make particles with a particle size of 1-3mm. -2 The solid-phase synthesis reaction was carried out under the condition of Pa for 8 hours, and cooled to room temperature under vacuum.

[0039] The material prepared by this method is a dark gray material (such as image 3 shown), the density of the material tested by the drainage method is 5.2g / cm 3 , XRD analysis showed that the material was composed of a new compound Zr 3 O and some ZrO 2 composition (such as Figure 4 shown). When in use, the ZrOx material is fully pre-melted first, and pre-melted in a water-cooled oxygen-free copper crucible. ...

Embodiment 3

[0041] use as figure 1 The process shown in the preparation of ZrO x : ZrH 2 Powder and ZrO 2 The powder is weighed according to the ratio of 3:2 by weight, and the mixing machine is used for mechanical mixing for 8 hours, and the mixed powder is mixed by a hydraulic press at 500N / cm 2 briquetting under a certain pressure, and then the material is crushed and sieved to make particles with a particle size of 1-5mm. -3 The solid-phase synthesis reaction was carried out under the condition of Pa for 10 hours, and cooled to room temperature under vacuum.

[0042] The material prepared by this method is a dark gray material (such as Figure 6 shown), the density of the material tested by the drainage method is 5.4g / cm 3 , XRD analysis showed that the material was composed of a new compound Zr 3 O and some ZrO 2 composition. When in use, the ZrOx material is fully pre-melted first, and pre-melted in a water-cooled oxygen-free copper crucible. The pre-melting temperature is a...

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Abstract

The invention provides ZrOx for plating an optical film and a preparation method of the ZrOx. The preparation method mainly comprises the following steps: by taking ZrO2 and ZrH2 powder as raw materials, uniformly mixing according to a certain ratio, briquetting or granulating, carrying out solid-phase synthesis under high-temperature vacuum, and cooling to room temperature under a vacuum state togenerate a new compound ZrOx. The melting point of the compound is lower than that of zirconium dioxide, stable chemical composition of the material is kept in the evaporation process, and process control over the coating process is facilitated. An optical film layer plated by the material is good in stability and consistency, has high transmittance from a near ultraviolet band to a near infraredband, is compact, firm and stable in chemical property, and can be used as a high-quality high-refractive-index material to be applied to optical film system design and batch film plating production.

Description

technical field [0001] The invention belongs to the field of optical thin film materials, and relates to a high-quality high-refractive index optical thin film evaporation material and a preparation method thereof, in particular to a ZrO coating for optical thin films x and its preparation method. Background technique [0002] Zirconium dioxide has a high refractive index and is easy to coat low-absorption optical films. The film is firm, dense and stable, and its extinction coefficient is 0.001 at a short wavelength of 0.25 μm, so it is also used for optical coatings in the ultraviolet band. The methods for preparing zirconium dioxide optical thin films include: direct evaporation of zirconium dioxide evaporation materials, ZrO2 x Reactive evaporation and reactive sputtering of zirconium. However, as far as electron beam evaporation is concerned, due to the high melting point of zirconia, about 2700 ° C, the material is partially melted during evaporation, which is easy t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G25/02C03C17/245
CPCC01G25/02C03C17/245C01P2006/10C01P2006/34C01P2002/72C01P2004/01C03C2217/22C03C2217/70C03C2218/151
Inventor 张碧田彭程石志霞孙静段华英张恒
Owner 有研资源环境技术研究院(北京)有限公司
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