CN110530206B - Preparation process of high-damage-threshold protective film for optical code disc of laser information field - Google Patents

Preparation process of high-damage-threshold protective film for optical code disc of laser information field Download PDF

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CN110530206B
CN110530206B CN201910964211.XA CN201910964211A CN110530206B CN 110530206 B CN110530206 B CN 110530206B CN 201910964211 A CN201910964211 A CN 201910964211A CN 110530206 B CN110530206 B CN 110530206B
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film
optical code
code disc
thickness
protective film
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CN110530206A (en
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张金豹
耿浩
史成浡
王明慧
田军
南勇
张勇
陈俊霞
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Henan Pingyuan Optical & Electronic Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02—Pretreatment of the material to be coated
    • C23C14/021—Cleaning or etching treatments
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/081—Oxides of aluminium, magnesium or beryllium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08—Oxides
    • C23C14/083—Oxides of refractory metals or yttrium
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/46—Sputtering by ion beam produced by an external ion source
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F41—WEAPONS
    • F41G—WEAPON SIGHTS; AIMING
    • F41G3/00—Aiming or laying means

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  • Engineering & Computer Science (AREA)
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  • Materials Engineering (AREA)
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  • Organic Chemistry (AREA)
  • General Engineering & Computer Science (AREA)
  • Optical Record Carriers And Manufacture Thereof (AREA)
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Abstract

The invention belongs to the technical field of optical film processing, and discloses a preparation process of a high-damage threshold protective film for an optical code disc of a laser information field, which comprises the following steps: 1) manufacturing an optical code disc: k9 optical glass is used as an optical code disc substrate, and an aluminum film and an aluminum oxide protective film are selected to manufacture an optical code disc pattern; 2) cleaning an optical coded disc: cleaning the optical code disc by using alcohol ether mixed liquid; 3) plating a protective film: the surface of the optical code disc is sequentially plated with an aluminum oxide film with the thickness of 46-52nm, a tantalum pentoxide film with the thickness of 42-48nm and a silicon dioxide film with the thickness of 227-233 nm. The reflectivity of the optical code disc protective film prepared by the invention is lower than 0.3% at the blank area with the thickness of 1.064 mu m, the reflectivity of the pattern area with the thickness of 1.064 mu m is higher than 88%, the electric field distribution at the interface of the film layer of the pattern area and the air is close to 0, and the laser damage resistance threshold level of the optical code disc is improved.

Description

Preparation process of high-damage-threshold protective film for optical code disc of laser information field
Technical Field
The invention belongs to the technical field of optical film processing, and particularly relates to a preparation process of a high-damage threshold protective film for an optical code disc of a laser information field.
Background
With the development of science and technology, the precise striking weapon becomes a killer mace for defeating and defeating on a battlefield, wherein laser guidance is one of the main implementation modes for implementing precise striking in modern war. The principle of laser beam steering guidance is that a ground transmitting system transmits scanned coded laser beams to a target, a missile flies in the laser beams, and a missile tail receiving device receives laser coded information to form a control instruction, so that the missile flies along the axis of the light beams all the time until the missile hits the target. The optoelectronic system for encoding and decoding the laser information field is the key of laser guidance, and the optical code disc is an important component. The optical code disc is mainly manufactured by obtaining information patterns through the post-photographing etching treatment of metal and metal protective films deposited on an optical glass substrate, and is a reference scale component for aiming, observing, adjusting, guiding and image information analysis of an optoelectronic system.
In recent years, laser technology is rapidly developed, and high-power lasers are more and more widely applied to optoelectronic systems, which puts forward a new performance index requirement, namely laser damage resistance threshold performance, for manufacturing optical code discs in laser information field systems. The laser damage resistance threshold of the optical code disc without the plated protective film is very low, which is mainly characterized in that standing wave fields among a substrate, a metal film, the metal protective film and an air interface are very strong, under laser irradiation, the film generates electron avalanche ionization similar to dielectric breakdown under the action of a high-frequency electromagnetic field, and thermoelastic pressure and thermal force waves are generated at local hot spots due to the rapid change of a temperature field, so that the final damage of the film is caused. In the preparation of the high laser damage threshold optical code disc protective film, the thickness of the protective film needs to be designed from a source for improving the damage threshold, so that the strong laser damage resistance of the film is obtained. When laser is incident to the film, one part of the laser enters the film to be continuously transmitted, the other part of the laser is reflected back through the film and the substrate, standing wave fields are formed in the film by the two beams of light transmitted in the forward direction and the reverse direction, and different electric field intensities exist at different positions in the film. The larger the electric field intensity in the film is, the more easily the damage is caused, and the air/film interlayer interface, the film/film interlayer interface and the film/substrate interface are weak links of the whole film system, especially the air/film interlayer interface is the most easily caused position of laser damage. Therefore, the protective film reduces the electric field intensity at these positions as much as possible. Meanwhile, in order to weaken the absorption of the metal film layer, the protective film improves the reflectivity of laser wavelength as much as possible, the higher the reflectivity of the metal film layer is, the smaller the film layer absorption is, and the less damage is. Therefore, the high laser damage threshold protective film of the prepared optical code disc can reach the advanced level of the industry.
Disclosure of Invention
In view of the above situation, an object of the present invention is to provide a process for preparing a high damage threshold protection film for an optical code disc of a laser information field, wherein three high damage threshold dielectric film materials are used to plate three layers of dielectric protection films on the premise that an optical code disc substrate material, a pattern film material and a thickness are selected in a 1.064 μm laser information field, the reflectivity of the prepared optical code disc protection film in a blank area of 1.064 μm is lower than 0.3%, the reflectivity of a pattern area of 1.064 μm is higher than 88%, the electric field distribution at an interface between the film layer of the pattern area and air is close to 0, and the laser damage resistance threshold level of the optical code disc is improved.
The invention provides a preparation process of a high-damage threshold protective film for an optical code disc of a laser information field, which comprises the following steps:
1) manufacturing an optical code disc: k9 optical glass is used as an optical code disc substrate, and an aluminum film and an aluminum oxide protective film are selected to manufacture an optical code disc pattern;
2) cleaning an optical coded disc: cleaning the optical code disc by using alcohol ether mixed liquid;
3) plating a protective film: the surface of the optical code disc is sequentially plated with an aluminum oxide film with the thickness of 46-52nm, a tantalum pentoxide film with the thickness of 42-48nm and a silicon dioxide film with the thickness of 227-233 nm.
In the invention, the optical code disc substrate applied to the 1.064 mu m laser information field is made of K9 optical glass produced by Chengdu Guangming in China, the spectrum absorption is small, the chemical stability is good, and the film layer for manufacturing the code disc pattern is made of aluminum (Al) film and aluminum oxide (Al)2O3) The 1.064-micron laser reflectivity of the aluminum film is higher and close to 90%, so that the heat absorption is smaller, the laser damage resistance is better, and the aluminum oxide protective film can prevent the aluminum film from being too soft and damaging the surface quality of the aluminum film in the process of manufacturing coded disc patterns. The surface roughness of the optical code disc is smaller than 1nm, the surface of the optical code disc has no broken points or broken roads, the smaller the surface roughness of the optical code disc is, the better the surface quality is, the higher the film forming quality is, and the stronger the resistance of the optical code disc to laser is. The optical code disc is divided into a blank area and a pattern area, the thickness of the aluminum film of the pattern is more than 100nm, which can ensure the sufficient reflectivity of the aluminum film at 1.064 μm, the thickness of the aluminum oxide protective film is 325-335nm, preferably 328nm,the reflectivity of the aluminum film can not be influenced under the condition of protecting the surface of the aluminum film. The parameters can be realized in the process of manufacturing the optical code disc, and the optical code disc is manufactured by adopting a conventional method in the field.
According to the present invention, the protective film is made of a wide variety of materials, such as magnesium fluoride (MgF)2) Silicon dioxide (SiO)2) Alumina (Al)2O3) Tantalum pentoxide (Ta)2O5) Titanium dioxide (TiO)2) And the invention preferably selects silicon dioxide, aluminum oxide and tantalum pentoxide with high laser damage resistance to be used for manufacturing the protective film, and the three film materials of aluminum oxide, tantalum pentoxide and silicon dioxide have strong mechanical property, stable chemical property and high laser damage resistance threshold.
In order to ensure that the optical code disc applied to a 1.064 μm laser information field has better performance, the three-layer protective film is preferably formed by sequentially plating a 49nm aluminum oxide film, a 45nm tantalum pentoxide film and a 230nm silicon dioxide film on the surface of the optical code disc.
Preferably, the alcohol ether mixed liquid is a mixed liquid of ethanol and diethyl ether with the volume ratio of 1: 1.
The conventional protective film plating equipment comprises a thermal evaporation mode, an ion source auxiliary evaporation mode, an ion beam sputtering mode and the like, wherein the ion beam sputtering mode is selected to plate the protective film on the surface of the optical code disc, so that the ion beam sputtering plated film has the advantages of few film forming defects, high film compactness, strong film mechanical strength, good film flatness, small absorption coefficient and extremely low scattering loss, and is more favorable for improving the laser damage resistance threshold.
Preferably, the ion beam sputtering is performed by using a dual ion beam sputter coater.
According to the invention, step 3) comprises: loading the cleaned optical code disc on a dual-ion beam sputtering film plating machine, vacuumizing until the vacuum degree of the dual-ion beam sputtering film plating machine is 6 multiplied by 10-2Pa-9×10-2When Pa is needed, baking the optical code disc at 100-120 ℃, keeping the temperature for 30-40 min, and continuously vacuumizing; when the vacuum degree is 2 x 10-3Pa-3×10-3Pa, 16cm ion source to Ta2O5、Al2O3、SiO2And cleaning the target material, cleaning the optical code disc by a 12cm ion source, and plating a protective film after cleaning.
Preferably, when the aluminum oxide film, the tantalum pentoxide film and the silicon dioxide film are plated, the process parameters comprise: the argon flow rate of the 16cm ion source was 18sccm, the argon flow rate of the radio frequency neutralizer was 5sccm, the argon flow rate of the 12cm ion source was 3sccm, the oxygen flow rate of the 12cm ion source was 25sccm, the beam current of the 12cm ion source was 200mA, the beam current of the 16cm ion source was 600mA, and the sputtering rate of the aluminum oxide film was 0.25nm/s, the sputtering rate of the tantalum pentoxide film was 0.24nm/s, and the sputtering rate of the silicon dioxide film was 0.22 nm/s.
The technological parameters which are not limited in the invention are all carried out by adopting the conventional mode in the field, for example, the other parameters in the manufacture of the optical code disc, the coating of the protective film and the like can all adopt the conventional operation in the field.
Compared with the prior art, the invention has the following beneficial effects:
the invention mainly aims at plating the protective film on the optical code disc element applied to the laser photoelectric system and improving the capability of the optical code disc element for bearing laser radiation. The reflectivity of the protective film plated by the preparation process is lower than 0.3% in a blank area 1.064 mu m of an optical code disc, the lower the reflection of the blank area is, the smaller the laser energy loss is, the reflectivity of a pattern area 1.064 mu m is higher than 88%, the higher the reflection of the pattern area is, the smaller the absorption is, the smaller the heat effect of the code disc is, the electric field distribution at the interface between the film layer of the pattern area and the air is close to 0, the smaller the electric field at the interface between the film layer of the pattern area and the air is, and the lower the possibility that the film layer is damaged by laser due to the absorption caused by surface pollution is. And the preparation process is easy to operate and popularize.
Drawings
FIG. 1: the structure schematic diagram of the optical code disc.
FIG. 2: the structure of the pattern area in fig. 1 is schematically illustrated.
FIG. 3: the structure schematic diagram of the blank area of the optical code disc after the coating of the protective film.
FIG. 4: the structure schematic diagram of the optical code disc pattern area after the protective film is plated.
FIG. 5: schematic diagram of dual ion beam sputter coating.
FIG. 6: the spectrum characteristic diagram of the blank area of the optical code disc after the coating of the protective film.
FIG. 7: and (5) coating a spectral characteristic diagram of the pattern area of the optical code disc after the protective film is coated.
FIG. 8: and (5) electric field distribution diagram of the optical code disc pattern area after the protective film is plated.
Description of reference numerals: a blank area; b pattern area; k9: a K9 substrate; 1, aluminum film; 2, an aluminum oxide protective film; 3, aluminum oxide film; 4 tantalum pentoxide film; 5 a silicon dioxide film; a 16cm ion source (sputtering); b12 cm ion source (assist); a-1 and B-1 radio frequency neutralizers; c, target material; d, optical code disc.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
The reference standards for the scrubbing reagents, film materials, equipment, optical software, spectrometer, ellipsometer used in the following examples are as follows:
alcohol ether mixed liquid: GB/T678 chemical reagent ethanol (absolute ethanol)
GB/T12591 CHEMICAL AGENT ETHYL ETHER
Film material of the film: SiO 22: purity over 99.99 percent
Al2O3: purity over 99.99 percent
Ta2O5: purity over 99.99 percent
Coating machine: U.S. Veeco double-ion-beam sputter coating machine
A spectrometer: american Agilent Cary 7000 UV-VIS-NIR full-automatic spectrometer
An ellipsometer: US Angstrom Advanced PHE-101 ellipsometer
Electric field analysis software: TFC optical thin film software
Film layer testing basis: JB/T8226.1-1999
Examples
The embodiment is used for explaining the preparation process of the high damage threshold protection film for the laser information field optical code disc, and comprises the following steps:
firstly, an optical code disc is manufactured and tested, the code disc is required to be in accordance with the condition that a substrate is K9 optical glass, a pattern is an aluminum film, the thickness is 160nm, the thickness of an aluminum oxide protective film is 328nm, the surface roughness is less than 1nm, and no broken points or particles exist on the surface. A specific optical code disc is shown in FIGS. 1-2.
Secondly, cleaning the code disc by using alcohol ether mixed liquid in a ratio of 1: 1, loading the code disc into a U.S. Veeco dual-ion beam sputter coating machine after cleaning, vacuumizing, and sputter coating as shown in FIG. 5.
Thirdly, when the vacuum degree of the dual-ion beam sputter coating machine is 7 multiplied by 10-2When Pa is needed, baking the optical code disc at 110 ℃, keeping the temperature for 35min, and continuously vacuumizing; when the vacuum degree is 2 x 10-3Pa, 16cm ion source to Ta2O5、Al2O3、SiO2Cleaning a target material, and cleaning an optical code disc by a 12cm ion source; after the cleaning, 49nm of aluminum oxide (Al) is sequentially sputtered and deposited according to the process parameters in the table 12O3) 45nm tantalum pentoxide (Ta)2O5) 230nm silicon dioxide (SiO)2) And the optical code disc structure is shown in FIGS. 3-4 until the film layer is finished.
TABLE 1
Figure GDA0003153351380000061
Figure GDA0003153351380000071
The surface of the optical code disc obtained in the embodiment is plated with a 1.064 mu m high laser damage threshold protection film, and a spectrometer is used for detecting the spectral characteristics of the optical code disc protection film, wherein the spectral characteristics are shown in FIGS. 6-7, the blank area of the optical code disc is 1.064 mu m, and R is less than 0.3%; the pattern area of the optical code disc is 1.064 mu m, R is more than 88 percent, the thickness of the protective film is measured by an ellipsometer, and the error of the thickness of the protective film is less than 3 nm; analyzing the electric field distribution by using TFC optical software, wherein the electric field distribution is as shown in FIG. 8, and the electric field distribution at the interface between the film layer of the pattern area and the air is close to 0; the film layer characteristics meet the JB/T8226.1-1999 standard.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the illustrated embodiments.

Claims (5)

1. The preparation process of the high damage threshold protection film for the laser information field optical code disc is characterized by comprising the following steps of:
1) manufacturing an optical code disc: k9 optical glass is used as an optical code disc substrate, and an aluminum film and an aluminum oxide protective film are selected to manufacture an optical code disc pattern;
2) cleaning an optical coded disc: cleaning the optical code disc by using alcohol ether mixed liquid;
3) plating a protective film: plating an alumina film with the thickness of 46-52nm, a tantalum pentoxide film with the thickness of 42-48nm and a silicon dioxide film with the thickness of 227-233nm on the surface of the optical code disc in sequence;
in the step 3), a protective film is coated on the surface of the optical code disc in an ion beam sputtering mode, wherein the ion beam sputtering is carried out by adopting a dual-ion beam sputtering coating machine;
the step 3) comprises the following steps: loading the cleaned optical code disc on a dual-ion beam sputtering film plating machine, vacuumizing until the vacuum degree of the dual-ion beam sputtering film plating machine is 6 multiplied by 10-2Pa-9×10-2When Pa is needed, baking the optical code disc at 100-120 ℃, keeping the temperature for 30-40 min, and continuously vacuumizing; when the vacuum degree is 2 x 10-3Pa-3×10-3Pa, 16cm ion source to Ta2O5、Al2O3、SiO2Cleaning a target material, cleaning an optical code disc by a 12cm ion source, and plating a protective film after cleaning;
when the aluminum oxide film, the tantalum pentoxide film and the silicon dioxide film are plated, the technological parameters comprise: the argon flow rate of the 16cm ion source was 18sccm, the argon flow rate of the radio frequency neutralizer was 5sccm, the argon flow rate of the 12cm ion source was 3sccm, the oxygen flow rate of the 12cm ion source was 25sccm, the beam current of the 12cm ion source was 200mA, the beam current of the 16cm ion source was 600mA, and the sputtering rate of the aluminum oxide film was 0.25nm/s, the sputtering rate of the tantalum pentoxide film was 0.24nm/s, and the sputtering rate of the silicon dioxide film was 0.22 nm/s.
2. The preparation process of the high damage threshold protection film for the optical code disc of the laser information field as claimed in claim 1, wherein: the thickness of the aluminum film of the optical code disc pattern is more than 100nm, the thickness of the aluminum oxide protective film is 325-335nm, the surface roughness of the optical code disc is less than 1nm, and the surface of the optical code disc is free of broken points and broken paths.
3. The preparation process of the high damage threshold protection film for the optical code disc of the laser information field as claimed in claim 2, wherein: the thickness of the alumina protective film is 328 nm.
4. The preparation process of the high damage threshold protection film for the optical code disc of the laser information field as claimed in claim 1, wherein: the alcohol ether mixed liquid is a mixed liquid of ethanol and ether with the volume ratio of 1: 1.
5. The preparation process of the high damage threshold protection film for the optical code disc of the laser information field as claimed in claim 1, wherein: an aluminum oxide film with the thickness of 49nm, a tantalum pentoxide film with the thickness of 45nm and a silicon dioxide film with the thickness of 230nm are sequentially plated on the surface of the optical code disc.
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