CN102540282B - Preparation method of dual-waveband high-efficiency anti-reflection film - Google Patents

Preparation method of dual-waveband high-efficiency anti-reflection film Download PDF

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CN102540282B
CN102540282B CN201210033571.6A CN201210033571A CN102540282B CN 102540282 B CN102540282 B CN 102540282B CN 201210033571 A CN201210033571 A CN 201210033571A CN 102540282 B CN102540282 B CN 102540282B
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magnesium fluoride
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CN102540282A (en
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张锡涛
张双文
王长明
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DONGGUAN HUAQING OPTICAL TECHNOLOGY Co.,Ltd.
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DONGGUAN HUAQING OPTICAL TECHNOLOGY Co Ltd
Janus Dongguan Precision Components Co Ltd
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Abstract

The invention discloses a dual-waveband high-efficiency anti-reflection film and a preparation method thereof. Dual wave bands comprise a visible light waveband and a 1064 nanometer light waveband; and the high-efficiency anti-reflection film takes K9 glass as a base material, is formed by alternatively stacking thin film forming materials of MgF2, HfO2 and TiO2 with three different refractive indexes and sequentially comprises an MgF2 film layer, an HfO2 film layer, an MgF2 film layer, a TiO2 film layer, an HfO2 film layer and an MgF2 film layer from one side of the anti-reflection film close to the glass to outside. The preparation method of the dual-waveband high-efficiency anti-reflection film is carried out on an evaporation film plating machine with an electronic gun, a film thickness monitoring apparatus and an oxygen supplying system; the average reflectivity of the dual-waveband high-efficiency anti-reflection film in the visible light spectrum region is lower than 0.5%, and the reflectivity at the 1064 nanometer laser position is lower than 0.5%; and simultaneously, the dual-waveband high-efficiency anti-reflection film has the advantages of simple designed film-system structure, common selected materials, easy implementation of a process and capability of realizing industrial production.

Description

A kind of preparation method of Dual-waveband high-efficiency anti-reflection film
Technical field
The present invention relates to a kind of thin film fabrication technology of precision optical instrument industry, particularly relate to a kind of preparation method of Dual-waveband high-efficiency anti-reflection film.
Background technology
Along with the development of microbial technique, the more and more meticulousr and robotization of the micro-processing technology of cell cutting, botany section etc., simultaneously also more and more higher to the requirement of various technology.Yet, when the relevant instrument of Design and manufacture, run into a series of technical matters: first, the high-definition image of realizing microorganism shows, the pixel of optical system and enlargement factor require high, the optical system structure designing is like this complicated, and lens set number is more, and image definition is affected.Secondly, realize automatic laser processing, because lens group number is many, after multiple reflections, the energy loss that light finally arrives microorganism surface through light path system is serious, is unfavorable for processing.Therefore, need to, by be coated with visible range (380-760nm) and 1064 nanometer Dual-waveband high-efficiency anti-reflection films on camera lens surface, increase the high definition of picture element and the energy loss of minimizing 1064 nano wave length laser.
As No. 03156715.0 disclosed optical anti-reflective film of patent documentation of People's Republic of China's patented claim and film plating process, this optical anti-reflective film is that plating is on the substrate of synthetic resin, be by the layers of material of different refractivity time plating on synthetic resin, make this multilayer film there is antireflective properties useful.Patent documentation CN1576894A is the immediate prior art of the present invention.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of Dual-waveband high-efficiency anti-reflection film is provided, can effectively change the optical characteristics on camera lens surface, solve the fuzzy and laser ability attenuation problem of the figure running in the optical system of precision optical instrument.
In order to achieve the above object, the technical solution used in the present invention is: a kind of Dual-waveband high-efficiency anti-reflection film, described two waveband is visible light wave range and 1064 nanometer optical wave sections, described high-efficiency anti-reflection film be take K9 glass as base material, and this high-efficiency anti-reflection film becomes material magnesium fluoride (MgF by the film-shaped of three kinds of different refractivities 2), hafnium oxide (HfO 2) and titania (TiO 2) alternately stack form, described anti-reflection film from the side near glass to comprise successively MgF 2rete, HfO 2rete, MgF 2rete, TiO 2rete, HfO 2rete and MgF 2rete.
A preparation method for described Dual-waveband high-efficiency anti-reflection film, described preparation method's step is as follows:
This preparation method is based on following condition, vacuum chamber, the evaporation coating machine of electron gun, thickness monitoring instrument and oxygen air supply system is housed,
Step 1, the vacuum tightness of vacuum chamber is extracted into lower than 5.0 * 10 -3handkerchief, substrate of glass temperature is heated to 145~155 degree, to K9 substrate of glass Ions Bombardment 2 minutes, increases the activity of substrate of glass;
Step 2, evaporation the first tunic MgF 2, vacuum tightness is 4.8 * 10 -3~5.2 * 10 -3handkerchief, substrate of glass temperature 145~155 degree, MgF 2thicknesses of layers is 201.2 nanometers, and rate of film build is 0.6 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 3, at ground floor MgF 2evaporation the second tunic HfO on rete 2, the vacuum tightness after filling oxygen is 1.8 * 10 -2~2.0 * 10 -2handkerchief, substrate of glass temperature 145~155 degree, HfO 2thicknesses of layers is 37.7 nanometers, and rate of film build is 0.3 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 4, at second layer HfO 2evaporation trilamellar membrane MgF on rete 2, vacuum tightness is 4.8 * 10 -3~5.2 * 10 -3handkerchief, substrate of glass temperature is 145~155 degree, MgF 2thicknesses of layers is 20.96 nanometers, and rate of film build is 0.6 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 5, on the 3rd layer of magnesium fluoride rete evaporation the 4th tunic TiO 2, the vacuum tightness after filling oxygen is 1.8 * 10 -2~2.0 * 10 -2, substrate of glass temperature is 145~155 degree, TiO 2thicknesses of layers is 126 nanometers, and rate of film build is 0.3 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 6, at the 4th layer of TiO 2evaporation layer 5 film HfO on rete 2, the vacuum tightness after filling oxygen is 1.8 * 10 -2~2.0 * 10 -2, substrate of glass temperature is 145~155 degree, HfO 2thicknesses of layers is 75.4 nanometers, and rate of film build is 0.3 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 7, at layer 5 HfO 2evaporation layer 6 film MgF on rete 2, vacuum tightness is 4.8 * 10 -3~5.2 * 10 -3handkerchief, substrate of glass temperature is 145~155 degree, MgF 2thicknesses of layers is 100.6 nanometers, and rate of film build is 0.6 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 8, treat that substrate of glass temperature naturally cools to below 100 degree, take out product, obtain visible range and 1064 nanometer Dual-waveband high-efficiency anti-reflection films.
Compared with prior art, the invention has the beneficial effects as follows: this Dual-waveband high-efficiency anti-reflection film in visible spectrum region the average reflectance of (400 nanometer-700 nanometer) lower than 0.5%, the reflectivity of laser 1064 nanometers is lower than 0.5%, therefore, light is after being coated with the camera lens of this rete, transmitance (one side) at visible spectrum region and 1064 places can reach more than 99.5%, the needed image high-resolution of the optical instruments such as biological microscope that has met microfabrication, laser energy loses little requirement.Meanwhile, the designed film structure of this anti-reflection film is simple, and the material of selecting is common, and technique easily realizes, and can realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is the reflectance spectrum curve of visible region of the present invention;
Fig. 3 is the reflectance spectrum curve of 1064 nano-area of the present invention;
Fig. 4 is the reflectance spectrum curve of two waveband of the present invention.
Embodiment
Below in conjunction with embodiment, with reference to accompanying drawing, be elaborated, to technical characterictic of the present invention and advantage are interpretated more in-depth.
Structural representation of the present invention as shown in Figure 1, a kind of Dual-waveband high-efficiency anti-reflection film, described two waveband is visible light wave range and 1064 nanometer optical wave sections, and described high-efficiency anti-reflection film be take K9 glass as base material, and this high-efficiency anti-reflection film becomes material MgF by the film-shaped of three kinds of different refractivities 2, HfO 2and TiO 2alternately stack forms, described anti-reflection film from the side near glass to comprise successively MgF 2rete, HfO 2rete, MgF 2rete, TiO 2rete, HfO 2rete and MgF 2rete.
A preparation method for described Dual-waveband high-efficiency anti-reflection film, described preparation method's step is as follows:
This preparation method is based on following condition, vacuum chamber, the evaporation coating machine of electron gun, thickness monitoring instrument and oxygen air supply system is housed,
Step 1, the vacuum tightness of vacuum chamber is extracted into lower than 5.0 * 10 -3handkerchief, substrate of glass temperature is heated to 145~155 degree, to K9 substrate of glass Ions Bombardment 2 minutes, increases the activity of substrate of glass;
Step 2, evaporation the first tunic MgF 2, vacuum tightness is 4.8 * 10 -3~5.2 * 10 -3handkerchief, substrate of glass temperature 145~155 degree, MgF 2thicknesses of layers is 201.2 nanometers, and rate of film build is 0.6 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 3, at ground floor MgF 2evaporation the second tunic HfO on rete 2, the vacuum tightness after filling oxygen is 1.8 * 10 -2~2.0 * 10 -2handkerchief, substrate of glass temperature 145~155 degree, HfO 2thicknesses of layers is 37.7 nanometers, and rate of film build is 0.3 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 4, at second layer HfO 2evaporation trilamellar membrane MgF on rete 2, vacuum tightness is 4.8 * 10 -3~5.2 * 10 -3handkerchief, substrate of glass temperature is 145~155 degree, MgF 2thicknesses of layers is 20.96 nanometers, and rate of film build is 0.6 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 5, at the 3rd layer of MgF 2evaporation the 4th tunic TiO on rete 2, the vacuum tightness after filling oxygen is 1.8 * 10 -2~2.0 * 10 -2, substrate of glass temperature is 145~155 degree, TiO 2thicknesses of layers is 126 nanometers, and rate of film build is 0.3 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 6, at the 4th layer of TiO 2evaporation layer 5 film HfO on rete 2, the vacuum tightness after filling oxygen is 1.8 * 10 -2~2.0 * 10 -2, substrate of glass temperature is 145~155 degree, HfO 2thicknesses of layers is 75.4 nanometers, and rate of film build is 0.3 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 7, at layer 5 HfO 2evaporation layer 6 film MgF on rete 2, vacuum tightness is 4.8 * 10 -3~5.2 * 10 -3handkerchief, substrate of glass temperature is 145~155 degree, MgF 2thicknesses of layers is 100.6 nanometers, and rate of film build is 0.6 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 8, treat that substrate of glass temperature naturally cools to below 100 degree, take out product, obtain visible range and 1064 nanometer Dual-waveband high-efficiency anti-reflection films.
Visible range and 1064 nanometer Dual-waveband high-efficiency anti-reflection films are to take K9 glass as base material, select the common materials MgF of three kinds of different refractivities 2, HfO 2and TiO 2alternately stack forms, according to the ABC of Film Optics and analytical approach, then by software optimization, the film finally obtaining be basic structure be Glass LHLUHL Air, L is MgF 2, H is HfO 2, U refers to TiO 2, incident medium is air, and incident angle is 0 degree. and refractive index and the thickness of various materials see the following form:
In above table, QWOT is a kind of method for expressing of optical thickness, and its computing formula is:
QWOT=4nd/λ 0
Wherein, λ 0be reference wavelength, n is the real part of refractive index, and d is the physical thickness of film.
The film material using in this film system, also can substitute with the close other materials of refractive index, suitably revises thickness; When base material changes, the thickness that can adjust rete reaches requirement, and the preparation method of this Dual-waveband high-efficiency anti-reflection film is that the method by vacuum vapor plating realizes.
Reflectance spectrum curve is as shown in Figure 2,3, 4, and the average reflectance of (380 nanometer-780 nanometer) is lower than 0.5% in visible spectrum region for this Dual-waveband high-efficiency anti-reflection film, and the reflectivity of laser 1064 nanometers is lower than 0.5%.Therefore, light is after being coated with the camera lens of this rete, transmitance (one side) in visible spectrum region and 1064 nanometers can reach more than 99.5%, has met the needed image high-resolution of the optical instruments such as biological microscope of microfabrication, and laser energy loses little requirement.Meanwhile, the designed film structure of this anti-reflection film is simple, and the material of selecting is common, and technique easily realizes, and can realize suitability for industrialized production.
By the technical scheme in above embodiment, the present invention is carried out to clear, complete description; the embodiment that obvious described embodiment is a part of the present invention; rather than whole embodiment; embodiment based in the present invention; those of ordinary skills, not making the every other embodiment obtaining under creative work prerequisite, belong to the scope of protection of the invention.

Claims (1)

1. the preparation method of a Dual-waveband high-efficiency anti-reflection film, described two waveband is visible light wave range and 1064 nanometer optical wave sections, it is characterized in that: described high-efficiency anti-reflection film be take glass as base material, this high-efficiency anti-reflection film becomes material magnesium fluoride, hafnium oxide and titania alternately to superpose and form by the film-shaped of three kinds of different refractivities, described anti-reflection film near a side of glass to comprise successively magnesium fluoride rete, hafnium oxide rete, magnesium fluoride rete, titanium oxide film layer, hafnium oxide rete and magnesium fluoride rete, described preparation method's step is as follows:
This preparation method is based on following condition, vacuum chamber, the evaporation coating machine of electron gun, thickness monitoring instrument and oxygen air supply system is housed,
Step 1, the vacuum tightness of vacuum chamber is extracted into lower than 5.0 * 10 -3handkerchief, substrate of glass temperature is heated to 145~155 degree, to substrate of glass Ions Bombardment 2 minutes, increases the activity of substrate of glass;
Step 2, evaporation the first tunic magnesium fluoride, vacuum tightness is 4.8 * 10 -3~5.2 * 10 -3handkerchief, substrate of glass temperature 145~155 degree, magnesium fluoride thicknesses of layers is 201.2 nanometers, and rate of film build is 0.6 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 3, on ground floor magnesium fluoride rete evaporation the second tunic hafnium oxide, the vacuum tightness after filling oxygen is 1.8 * 10 -2~2.0 * 10 -2handkerchief, substrate of glass temperature 145~155 degree, hafnium oxide thicknesses of layers is 37.7 nanometers, and rate of film build is 0.3 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 4, on the second layer hafnium oxide rete evaporation trilamellar membrane magnesium fluoride, vacuum tightness is 4.8 * 10 -3~5.2 * 10 -3handkerchief, substrate of glass temperature is 145~155 degree, and magnesium fluoride thicknesses of layers is 20.96 nanometers, and rate of film build is 0.6 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 5, on the 3rd layer of magnesium fluoride rete evaporation the 4th tunic titania, the vacuum tightness after filling oxygen is 1.8 * 10 -2~2.0 * 10 -2, substrate of glass temperature is 145~155 degree, and titanium dioxide film layer thickness is 126 nanometers, and rate of film build is 0.3 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 6, in the 4th layer of titanium oxide film layer evaporation layer 5 film hafnium oxide, the vacuum tightness after filling oxygen is 1.8 * 10 -2~2.0 * 10 -2, substrate of glass temperature is 145~155 degree, and hafnium oxide thicknesses of layers is 75.4 nanometers, and rate of film build is 0.3 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 7, on layer 5 hafnium oxide rete evaporation layer 6 film magnesium fluoride, vacuum tightness is 4.8 * 10 -3~5.2 * 10 -3handkerchief, substrate of glass temperature is 145~155 degree, and magnesium fluoride thicknesses of layers is 100.6 nanometers, and rate of film build is 0.6 nanometer/s, and the electric current of electron gun is adjusted according to rate of film build;
Step 8, treat that substrate of glass temperature naturally cools to below 100 degree, take out product, obtain visible range and 1064 nanometer Dual-waveband high-efficiency anti-reflection films.
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Address after: Changan town in Guangdong province Dongguan City Zhen'an 523878 corner management section

Co-patentee after: Dongguan Huaqing Optical Technology Co., Ltd.

Patentee after: Guangdong wins smart group Limited by Share Ltd

Address before: Changan town in Guangdong province Dongguan City Zhen'an 523878 corner management section

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Patentee before: Dongguan Janus Precision Components Co., Ltd.

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Effective date of registration: 20200713

Address after: 523000, Guangdong, Dongguan province Changan Town, South District Industrial Zone

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Address before: Changan town in Guangdong province Dongguan City Zhen'an 523878 corner management section

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Patentee before: GUANGDONG JANUS INTELLIGENT GROUP Corp.,Ltd.