Preparing method for high laser damage threshold ZrO2 thin-membrane

A laser damage threshold and thin film technology, applied in optics, optical components, instruments, etc., can solve the problems of complex preparation process, low damage threshold, unsafe, etc., and achieve the effect of simple preparation process and easy operation.

Inactive Publication Date: 2004-12-08
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

THO 2 and HfO 2 The optical properties and damage threshold of TiO can meet the requirements, but the preparation process is complicated and unsafe; TiO 2 The refractive index is high and the optical performance is good, but the damage threshold is low; AlOOH can meet the requirements of the damage threshold, but the AlOOH refractive index is only 1.44

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 10g of zirconium oxychloride and 100ml of deionized water were mixed and stirred for 10 minutes, then 10g of deionized resin (produced by ROHMAND HAAM France S.A company, model: AMBERLITE IRA96RF 63279 LOT 621AG40, the same below) was stirred for 10 minutes, and then filtered out resin. Put the solution into an airtight container (container filling degree≤70%), then place the container in an oven at 165° C. to heat for 1 hour, and cool down rapidly to obtain a zirconium dioxide hydrosol. Mix ethylene glycol methyl ether 110ml into zirconium dioxide hydrosol, replace water with ethylene glycol methyl ether by fractional distillation to obtain zirconium dioxide alcohol sol, add polyvinylpyrrolidone (PVP) in a ratio of 3% by weight to obtain ZrO 2 - PVP alcohol sol, a single-layer zirconia film is deposited on a glass substrate by spin coating. Anti-laser damage threshold is 10J / cm 2 (1064nm, 1ns); the refractive index of the film is 1.57.

Embodiment 2

[0020] 15g of zirconium oxychloride and 130ml of deionized water were mixed and stirred for 12 minutes, then 15g of deionized resin was added and stirred for 7 minutes, and then the resin was filtered off. Put the solution into an airtight container (container filling degree ≤ 70%), then place the container in an oven at 180°C and heat for 50 minutes, then quench and cool down to obtain a zirconium dioxide hydrosol. 140ml of ethylene glycol methyl ether was mixed into the zirconium dioxide hydrosol, and water was replaced by ethylene glycol methyl ether by fractional distillation to obtain the zirconium dioxide alcohol sol. Add polyvinylpyrrolidone (PVP) in the proportion of 5% by weight, fully stir to obtain ZrO 2 - PVP Alcohol Sol. A single-layer zirconia film was deposited on a glass substrate by spin coating. Anti-laser damage threshold is 15J / cm 2 (1064nm, 1ns); the refractive index of the film is 1.60.

Embodiment 3

[0022] 12g of zirconium oxychloride and 100ml of deionized water were mixed and stirred for 12 minutes, then 12g of deionized resin was added and stirred for 10 minutes, and then the resin was filtered off. Put the solution into an airtight container (container filling degree≤70%), then place the container in an oven at 165° C. to heat for 1 hour, and cool down rapidly to obtain a zirconium dioxide hydrosol. Mix 100ml of ethylene glycol methyl ether into the zirconium dioxide hydrosol, and replace water with ethylene glycol methyl ether by fractional distillation to obtain the zirconium dioxide alcohol sol. Add polyvinylpyrrolidone (PVP) in the proportion of 10% by weight, fully stir to obtain ZrO 2 - PVP Alcohol Sol. A single-layer zirconia film was deposited on a glass substrate by spin coating. Anti-laser damage threshold is 19J / cm 2 (1064nm, 1ns); the refractive index of the film is 1.65.

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Abstract

The preparing method is as the follows, agueous solution of ZrOC1.8H2O is prepared first and hydrothermal composition is carried out for the aqueous solution is sealed container for obtaining ZrO2 water soliquid, then athylene glycol dimethyl ether is used to replace water contained in ZrO2 water soliquid to form Zro2 alcohol soliquid and finally uniform and stable ZrO2-PVP soliquid can be formed by agitating when proper quantity of PVP is added into the alcohol soliquid.

Description

technical field [0001] The invention belongs to the technical field of optical thin films, in particular to a high laser damage threshold ZrO 2 The method of film preparation. Background technique [0002] The preparation of anti-laser damage thin films is usually divided into physical coating method and sol-gel chemical coating method. [0003] Most of the traditional optical thin film methods are physical coating methods (PVD), such as vacuum evaporation, magnetron sputtering, electron beam evaporation, etc. Although these methods are relatively mature, they are difficult to produce large-scale anti-reflection coatings, reflective coatings and Polarizing films and coatings on curved surfaces have encountered serious problems such as high cost, increased technical difficulty, and especially insufficient resistance to strong laser damage. However, the chemical coating method represented by the sol-gel method has opened up attractive prospects in this respect: the price is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C17/23G02B1/10
Inventor 沈军杨帆孙骐王珊张勤远吴广明倪星元周斌
Owner TONGJI UNIV
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