Method used for increasing silicon dioxide antireflection film hole stability

A technology of silicon dioxide and anti-reflection coatings, which is applied in the field of improving the stability of the pores of silica anti-reflection coatings. It can solve the problems that the anti-reflection coatings cannot achieve the expected effect, the density of the film increases, and the film cracks, etc., so as to prevent the holes from collapsing. And cracking, reducing internal stress, reducing the effect of pressure

Inactive Publication Date: 2015-05-13
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

In the process of heat treatment, in addition to the evaporation and decomposition of the liquid in the gel, there is also a polymerization reaction between the colloidal particles, that is, shrinkage or acetalization reaction, and the condensed water or alcohol is also evaporated. When the meniscus is generated in the medium, the surface tension of the liquid in the gel pores on the gas-liquid interface will cause the nanopores in the gel film to have a strong capillary contraction, that is, capillary phenomenon or capillary force, strong Capillary force will lead to the collapse of the nano-sized pores of the gel, making the pores disappear and increasing the density of the film, and what's more, it will cause the film to crack, so that the anti-reflection coating cannot achieve the expected effect

Method used

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  • Method used for increasing silicon dioxide antireflection film hole stability
  • Method used for increasing silicon dioxide antireflection film hole stability
  • Method used for increasing silicon dioxide antireflection film hole stability

Examples

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Embodiment 1

[0034] This embodiment provides a method for improving the hole stability of a silica antireflection film, which includes the following steps:

[0035] Step 1: Prepare the ready-to-use sol, the organosiloxane added in the sol is methyltriethoxysilane;

[0036] Add ethyl orthosilicate, deionized water, methyltriethoxysilane, Triton X-100 at a molar ratio of 1:4.53:0.25:0.2 to absolute ethanol, use hydrochloric acid as a catalyst, and prepare 100mL sol , Wherein the molar concentration of methyltriethoxysilane is 0.075mol / L, the sol is treated in a water bath, the temperature of the water bath is 55°C, and the time is 2 hours, and then the sol is sealed and left standing at room temperature In 2 days, the preparation of the sol to be used was completed.

[0037] Step 2: Cleaning and surface treatment of high borosilicate glass;

[0038] Use deionized water, acetone and absolute ethanol to ultrasonically clean the high borosilicate wafers. The cleaning time for each step is 15 minutes. ...

Embodiment 2

[0048] This embodiment provides a method for improving the hole stability of a silica antireflection film, which includes the following steps:

[0049] Step 1': It is basically the same as Step 1 of Example 1, except that the organosiloxane added in the sol is trimethylethoxysilane, and the concentration of trimethylethoxysilane is 0.03mol / L.

[0050] Step 2'and step 3'are the same as step 2 and step 3 of the first embodiment.

[0051] Step 4': Heat treatment of the film;

[0052] Put the high borosilicate silicon wafer with gel film prepared in step 3'into the muffle furnace, start from room temperature, heat the film at a heating rate of 0.5°C / min, at 130°C, 200°C, 250°C The four temperatures of 300℃ and 300℃ each stay for 10 minutes, and then the temperature is raised to 500℃ for heat treatment for 15 minutes, the muffle furnace is turned off, and the film is cooled to room temperature along with the furnace.

[0053] Step 5'is the same as step 5 in the first embodiment.

[0054] The...

Embodiment 3

[0056] This embodiment provides a method for improving the hole stability of a silica antireflection film, which includes the following steps:

[0057] Step 1'': It is basically the same as Step 1 of Example 1, except that the organosiloxane added in the sol is methyltriacetoxysilane, and the concentration of methyltriacetoxysilane is 0.2mol / L.

[0058] Step 2'' and step 3'' are the same as step 2 and step 3 of the first embodiment.

[0059] Step 4’’: Thin film heat treatment;

[0060] Put the high borosilicate silicon wafer with gel film prepared in step 3'' into the muffle furnace, start from room temperature, heat the film at a heating rate of 1℃ / min, at 145℃, 200℃, 250 The four temperatures of ℃ and 300℃ each stay for 40 minutes, and then the temperature is raised to 500℃ for heat treatment for 15 minutes, the muffle furnace is turned off, and the film is cooled to room temperature along with the furnace.

[0061] Step 5'is the same as step 5 in the first embodiment.

[0062] The su...

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Abstract

The invention relates to a method used for increasing silicon dioxide antireflection film hole stability, and belongs to the technical field of optical thin film preparation. Sol-gel method is adopted for preparing a silicon dioxide antireflection film, and comprises following steps: a sol is prepared firstly; high borosilicate glass is subjected to cleaning and surface treatment; film preparation is carried out through pulling; and thin film heat treatment and thin film surface hydrophobic treatment are carried out; wherein 1) organic siloxane R'xSi(OR)4-x is added into the sol so as to modify the sol; and 2) in thin film heat treatment processes, a gel thin film is subjected to step thermal insulation heat processing at 90 to 350 DEG C. The method is capable of increasing film forming rate of porous silicon dioxide thin films, and ensuring transmittance of workpieces provided with antireflection films.

Description

Technical field [0001] The invention relates to a method for improving the hole stability of a silica antireflection film, and belongs to the technical field of optical film preparation. Background technique [0002] Anti-reflection coating is also called anti-reflection coating, which means that optical film is coated on the surface of optical elements to reduce the reflection on the surface of optical elements and increase the transmittance of light, thereby improving the performance of optical elements in the working wavelength or wavelength band. It is very necessary to add anti-reflection coating on optical components. [0003] At present, the coating materials used for antireflection mainly include titanium dioxide, silicon nitride, magnesium fluoride, silicon dioxide, tantalum pentoxide, zinc sulfide, zirconium dioxide, cerium oxide, etc. For silicon dioxide, due to its low cost , Moderate refractive index, high surface strength, etc., has become the first choice for prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C17/25
Inventor 王吉宁杨海龄郝雷刘晓鹏蒋利军王树茂
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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