CN108409153B - Preparation method of multifunctional three-dimensional nanostructure surface anti-reflection membrane for electrons - Google Patents
Preparation method of multifunctional three-dimensional nanostructure surface anti-reflection membrane for electrons Download PDFInfo
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- CN108409153B CN108409153B CN201810208889.0A CN201810208889A CN108409153B CN 108409153 B CN108409153 B CN 108409153B CN 201810208889 A CN201810208889 A CN 201810208889A CN 108409153 B CN108409153 B CN 108409153B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/11—Anti-reflection coatings
- G02B1/118—Anti-reflection coatings having sub-optical wavelength surface structures designed to provide an enhanced transmittance, e.g. moth-eye structures
Abstract
A preparation method of a three-dimensional nanostructure surface antireflection film for electrons comprises the following steps: use of C4F8Preparing polytetrafluoroethylene by gas coating; heating the prepared polytetrafluoroethylene film to 280-350 ℃, and preserving heat for 10-20 min to prepare a polytetrafluoroethylene ball mask layer; etching quartz glass serving as a substrate by adopting a plasma etching method; and (5) cleaning. The invention overcomes the defect of poor film adhesion force prepared by the traditional film coating method, and the three-dimensional nano structure can resist high temperature and damp and heat environments. The anti-reflection film prepared by the invention has a three-dimensional nano convex structure on the surface, so that the transmitted light is enhanced, the transmissivity is increased, and the anti-reflection effect of 96 percent can be achieved.
Description
Technical Field
The invention relates to the technical field of optical devices, in particular to a preparation method of a three-dimensional nanostructure surface anti-reflection membrane for electrons.
Background
In an optical element, light energy is lost due to reflection on the surface of the element, and in order to reduce the reflection loss on the surface of the element, a transparent dielectric film is often coated on the surface of the optical element, and such a film is called an antireflection film. If the transmittance of each of the three glasses is 0.90, 0.96 and 0.98, the transmittance becomes 0.34, 0.66 and 0.81 respectively after 10 times of accumulation, and the algorithm is as follows: 0.9010=0.34，0.9610=0.66，0.9810In the case where the index film is provided with a thickness of =0.81, it can be seen that after 10 stacks, the loss is very large, and in this case, the advantage of the antireflection film is more easily obtained. The thickness of the film coated on the glass surface was 1/4, which is the wavelength of light, so that the two reflected lights cancel each other out, and it can be seen that the thickness d of the antireflection film is λ/4n, where: n is the refractive index of the film and λ is the wavelength of light in air.
The application of the antireflection film relates to various industries such as medicine, military, space exploration and the like. At present, the commonly used coating methods include vacuum evaporation, chemical phase-starting deposition, sol-gel coating and the like. The coated glass is composed of two or more layers of structures, and the film layers belong to two-dimensional film layers. How to improve the mechanical properties such as strength, frictional wear and bonding force between film layers is an important subject, and the development of the coating industry is restricted by the difficult problems.
Corning corporation prepares a glass antireflection film, a Cu mask is prepared by Rapid Thermal Annealing (RTA), and fig. 1 and fig. 2 are a cross-sectional view and a top view of the prepared Cu mask etching, respectively. However, the Cu mask made by Rapid Thermal Annealing (RTA) is not uniform in size and sometimes the masks are connected, which seriously affects the subsequent process, as shown in fig. 2, the etched surfaces are connected together in large pieces. The mask is not uniform, which causes the etching depth to be correspondingly inconsistent, the cross section of the etching is shown in fig. 1, and the heights of the Cu masks in fig. 1 are uneven. Meanwhile, the Cu metal mask is easy to generate metal splashing phenomenon in the etching process, so that the bottom of the glass has the phenomenon of growing grass, the roughness is increased, and the anti-reflection performance of the glass film is further influenced. By adopting an electron beam exposure mode, a uniform and stable photoresist mask can be prepared on the surface of the glass, but the electron beam exposure is expensive.
Disclosure of Invention
The invention aims to overcome the defect of poor adhesion of a film prepared by the existing film coating method, and provides a preparation method of a three-dimensional nanostructure surface anti-reflection film for electrons, which can resist high temperature and damp-heat environments.
The technical scheme adopted by the invention for solving the problems is as follows:
a preparation method of a three-dimensional nanostructure surface antireflection film for electrons comprises the following steps:
step one, coating a film: taking quartz glass as a substrate, and growing a polytetrafluoroethylene film with the thickness of 100-200 nm on the substrate;
step two, mask preparation: preparing a polytetrafluoroethylene ball mask layer;
step three, etching: etching quartz glass serving as a substrate by adopting a plasma etching method;
step four, cleaning: and (3) heating the mixed solution of concentrated sulfuric acid and hydrogen peroxide at 80-100 ℃ for 10-15 min to remove un-etched polytetrafluoroethylene and other residues in the quartz tank.
Wherein the coating process in the first step comprises the following steps: using a plasma enhanced chemical vapor deposition apparatus, and depositing a layer of a material on a substrate with C4F8The gas is a reaction gas, and a polytetrafluoroethylene film grows on the surface of the substrate.
Further, the pressure of a cavity in the plasma enhanced chemical vapor deposition equipment is 10-20 Pa, the power is 200-300W, and C is4F8The flow rate of the gas is 40-80 sccm.
The mask preparation process in the second step comprises the following steps: and (3) heating the polytetrafluoroethylene film prepared in the step one to 280-350 ℃, and preserving heat for 10-20 min.
The etching process of the third step comprises the following steps: etching quartz glass by using an inductively coupled plasma etching machine, wherein the pressure of a cavity is 1-5 Pa, the power of an upper electrode is 400-600W, the power of a lower electrode is 200-300W, and CHF (CHF) is adopted3As an etching gas, CHF3The flow rate is 40-80 sccm.
Further, the etching depth of the quartz glass is more than 200nm, and the depth-to-width ratio is more than 2: 1.
in the fourth step, the mass percent concentration of the concentrated sulfuric acid is 98%, the mass percent concentration of the hydrogen peroxide is 30%, and the mass percent concentration of the concentrated sulfuric acid and the hydrogen peroxide is 3: 1 or 1.8: 1 to obtain a mixed solution.
In the invention, the vacuum degree of the step two and the step three is less than 5.0 multiplied by 10-4Pa, and the like.
According to the second step of the invention, polytetrafluoroethylene micro-nano spheres with the diameter of 80-120 nm are prepared. Polytetrafluoroethylene is used as a mask, and a plasma etching method is adopted to prepare a nano columnar structure with uniform distribution, consistent size, diameter of 100nm and height of 300nm on the surface of quartz glass, so that the surface of the anti-reflection membrane has a three-dimensional nano convex structure.
The preparation process of the polytetrafluoroethylene micro-nano spheres comprises the following steps: by PECVD chemical vapor deposition coating machines, using C4F8The polytetrafluoroethylene is prepared by gas coating, and the coating process of the polytetrafluoroethylene comprises the following steps: the pressure of the cavity is 10-20 Pa, and the power is 200-300W, C4F8And (3) rapidly heating at the flow rate of 40-80 sccm, keeping the temperature for 10-20 min, and enabling the polytetrafluoroethylene film to be broken and shrunk into a spherical shape and be uniformly attached to the surface of the glass to be used as a mask of an etching process. The polytetrafluoroethylene pellets are uniformly distributed, and the duty ratio is about 1: 1.
has the advantages that: the anti-reflection film prepared by the invention has a three-dimensional nano convex structure on the surface, so that the transmitted light is enhanced, the transmissivity is increased, and the anti-reflection effect can reach 96%; good optical properties including low omnidirectional reflectivity, low haze, high transmittance, superhydrophobicity, oleophobicity, and high mechanical resistance are achieved. Through tests, the transmittance can reach 0.96.
Surface duty ratio after etching 1: 1, aspect ratio greater than 2: 1, the steepness is about 90 ℃, and the roughness is less than 40 nm. The nanometer three-dimensional structure surface anti-reflection film overcomes partial defects of a two-dimensional film coating structure and meets the requirements of partial optical industrial production.
The three-dimensional nanostructure surface antireflection film enables the energy of reflected light and transmitted light on the surface of the optical element to be redistributed, and the energy of the transmitted light is increased and the energy of the reflected light is reduced as a result of the redistribution. Light has the following characteristics: the intensity of the light in the transmissive region can be changed by changing the intensity of the light in the reflective region.
Drawings
FIG. 1 is a cross-sectional view of a Cu mask etch in the prior art;
FIG. 2 is a top view of Cu mask etching in the prior art;
FIG. 3 is a cross-sectional view of a polymer mask etch of the present invention;
FIG. 4 is a top view of the polymer mask etch of the present invention.
Detailed Description
In order to facilitate understanding of the technical means, the technical features and the objectives achieved by the present invention, the present invention will be further described with reference to the following embodiments.
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
A method for preparing a three-dimensional nanostructure surface anti-reflection membrane for electronics overcomes the defect of poor adhesion of a film prepared by a coating mode, and the three-dimensional nanostructure can resist high temperature and damp and hot environments. Firstly, preparing polytetrafluoroethylene micro-nano spheres with the diameter of 80-120 nm. And preparing nano columnar structures which are uniformly distributed and have consistent sizes on the surface of the glass by using polytetrafluoroethylene as a mask and adopting a plasma etching method.
The specific preparation process of the invention is as follows:
step one, use C4F8Preparing polytetrafluoroethylene by gas coating: using plasma enhanced chemical vapor deposition equipment to place the substrate on a lower flat plate with a temperature control device, wherein an upper flat plate can have the same radio frequency, so that a potential difference is generated between the upper flat plate and the lower flat plate, and C is introduced into the cavity at the working moment4F8The working pressure of the cavity is kept above 5Pa, so that a capacitive coupling type gas discharge phenomenon can occur between the upper plate and the lower plate, and plasma is generated; applying a radio frequency voltage to a medium containing C4F8Between upper and lower parallel plates of gas, C4F8Dissociating CF in plasma2Chain structure, CF2Chain structure consisting of cyclic C4F8Into linear-CF2-n，-CF2-nDeposited on the surface of the substrate. Growing a polytetrafluoroethylene film with the thickness of 100-200 nm on a substrate; wherein, the pressure of the cavity in the plasma enhanced chemical vapor deposition equipment is 10-20 Pa, the power is 200-300W, and C4F8The flow rate of the gas is 40-80 sccm.
Step two, mask preparation: heating the polytetrafluoroethylene film prepared in the first step to 280-350 ℃, and preserving heat for 10-20 min to prepare a polytetrafluoroethylene ball mask layer; under the vacuum degree of less than 5.0 multiplied by 10-4Is carried out under the condition of Pa; -CF2-nWhen the temperature of the film layer is higher than 280 ℃, the C-C chain part is broken, the Teflon film on the surface of the substrate shrinks to form a hemispherical substance, and the diameter of the Teflon hemisphere is 200-300 nm;
step three, etching: etching quartz glass serving as a substrate by adopting a plasma etching method; under the vacuum degree of less than 5.0 multiplied by 10-4Is carried out under the condition of Pa;
the ICP etching equipment comprises two sets of 13.56MHz radio frequency power supplies controlled by automatic matching: a set of electric field which enables the coil to generate inductive coupling, and etching gas introduced into the cavity generates high-density plasma through glow discharge under the action of the electric field; the second set of radio frequency power supply is connected to the electrode at the lower part in the chamber.
Etching quartz glass by using an inductively coupled plasma etching machine, wherein the pressure of a cavity is 1-5 Pa, the power of an upper electrode is 400-600W, the power of a lower electrode is 200-300W, and CHF (CHF) is adopted3As an etching gas, CHF3The flow rate is 40-80 sccm.
With CHF3Etching the quartz substrate by the etching gas in an ICP reactive ion etching machine, wherein the reaction is shown as a formula (1):
CHF3+SiO2→ SiF4+H2O+ CFx （1）；
step four, cleaning: the reagents used were: sulfuric acid (98%) + H2O2(30%), adopting a mixed solution of concentrated sulfuric acid and hydrogen peroxide in a weight ratio of 3: 1 or the volume ratio of 1.8: 1, heating at 80-100 ℃ for 10-15 min to remove un-etched polytetrafluoroethylene and other residues in the quartz groove.
The etching depth of the quartz glass is more than 200nm, so that the aspect ratio is more than 2: 1.
the selection ratio of the polytetrafluoroethylene pellet mask layer to the quartz glass adopted by the invention can reach 2: 1.
example 1
A preparation method of a three-dimensional nanostructure surface anti-reflection membrane for electrons comprises the following steps:
(1) film coating: the grown polytetrafluoroethylene is thin and 200nm thick.
(2) Preparing a mask: and preparing a polytetrafluoroethylene ball mask layer.
(3) Etching: and etching the quartz substrate by adopting a plasma etching method.
(4) Cleaning: heating mixed solution of concentrated sulfuric acid and hydrogen peroxide at 80 deg.C for 10 min. The un-etched teflon and other residues in the quartz groove are removed.
In the step (1), a vapor deposition method is adopted to grow a polytetrafluoroethylene film in a PECVD (plasma enhanced chemical vapor deposition) film coating machine, the pressure of a cavity is 10Pa, and the power is 200W, C4F8The flow rate was 40 sccm.
The mask is prepared in the step (2), and the adopted heat treatment process comprises the following steps: rising the temperature to 300 ℃ for 10min, and preserving the temperature for 10 min.
The etching process in the step (3) comprises the following steps: the pressure of the cavity is 1Pa, the upper electrode is 400W, the power of the lower electrode is 200W, and CHF3The flow rate was 40 sccm.
The uniformly distributed micro-nano structure surface is prepared, the diameter of a single column on the structure surface is 100nm, and the depth is 200 nm.
Example 2
A preparation method of a three-dimensional nanostructure surface anti-reflection membrane for electrons comprises the following steps:
(1) film coating: the grown polytetrafluoroethylene is thin and 160nm thick.
(2) Preparing a mask: and preparing a polytetrafluoroethylene ball mask layer.
(3) Etching: and etching the quartz substrate by adopting a plasma etching method.
(4) Cleaning: heating mixed solution of concentrated sulfuric acid and hydrogen peroxide at 100 deg.C for 15 min. The un-etched teflon and other residues in the quartz groove are removed.
In the step (1), a vapor deposition method is adopted to grow a polytetrafluoroethylene film in a PECVD (plasma enhanced chemical vapor deposition) film plating machine, the pressure of a cavity is 15Pa, and the power is 280W, C4F8The flow rate was 60 sccm.
The mask is prepared in the step (2), and the adopted heat treatment process comprises the following steps: raising the temperature to 380 ℃ for 18min, and preserving the heat for 10 min.
The etching process in the step (3) comprises the following steps: cavity pressure 2Pa, upper electrode 500W, lower electrode power 300W, CHF3The flow rate was 40 sccm.
The uniformly distributed micro-nano structure surface is prepared, the diameter of a single column on the structure surface is 100nm, and the depth is 200 nm.
Example 3
A preparation method of a three-dimensional nanostructure surface anti-reflection membrane for electrons comprises the following steps:
(1) film coating: the grown polytetrafluoroethylene is thin and 180nm thick.
(2) Preparing a mask: and preparing a polytetrafluoroethylene ball mask layer.
(3) Etching: and etching the quartz substrate by adopting a plasma etching method.
(4) Cleaning: heating the mixed solution of concentrated sulfuric acid and hydrogen peroxide to 90 deg.C, and decocting for 12 min. The un-etched teflon and other residues in the quartz groove are removed.
In the step (1), a vapor deposition method is adopted to grow a polytetrafluoroethylene film in a PECVD (plasma enhanced chemical vapor deposition) film plating machine, the pressure of a cavity is 18Pa, and the power is 300W, C4F8The flow rate was 50 sccm.
The mask is prepared in the step (2), and the adopted heat treatment process comprises the following steps: rising the temperature to 320 ℃ for 15min, and preserving the heat for 16 min.
The etching process in the step (3) comprises the following steps: cavity pressure 3Pa, upper electrode 400W, lower electrode power 200W, CHF3The flow rate was 50 sccm.
And preparing a uniformly distributed micro-nano structure surface, wherein the diameter of a single column on the structure surface is 110nm, and the depth is 230 nm.
The equipment adopted by the invention is a PECVD-601 chemical vapor phase coating machine of Wei Nake technology ltd, Chuangshi, Beijing.
The etching equipment adopted by the invention is an RIE-601 plasma etching machine of Wennake technologies, Inc. of Beijing Chuangshi.
Wherein, fig. 3 and fig. 4 are a cross-sectional view and a top view of the polymer mask etching of the present invention, respectively, the mask in fig. 3 is uniform in height, and the mask in fig. 4 is uniform.
The multifunctional nanostructured surface antireflection film was tested using a Shimadzu UV-3150 spectrophotometer, and the test results are shown in Table 1 below: the transmittance of the three-dimensional nanostructure surface is 92% or more.
TABLE 1 results of permeability data test of antireflection films of examples 1 to 3
The three-dimensional nanostructured surface of the present invention acts to redistribute the energy of reflected light and transmitted light, with the energy of reflected light decreasing and the energy of transmitted light increasing as a result of the redistribution.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A preparation method of a three-dimensional nanostructure surface antireflection film for electrons is characterized by comprising the following steps:
step one, coating a film: taking quartz glass as a substrate, and growing a polytetrafluoroethylene film with the thickness of 100-200 nm on the substrate;
step two, mask preparation: heating the polytetrafluoroethylene film prepared in the first step to 280-350 ℃, and preserving heat for 10-20 min to prepare a polytetrafluoroethylene ball mask layer;
step three, etching: etching quartz glass serving as a substrate by adopting a plasma etching method;
step four, cleaning: and (3) heating the mixed solution of concentrated sulfuric acid and hydrogen peroxide at 80-100 ℃ for 10-15 min to remove un-etched polytetrafluoroethylene and other residues in the quartz tank.
2. The method for preparing the three-dimensional nanostructure surface antireflection film for the electrons according to claim 1, wherein the method comprises the following steps: the film coating process in the first step comprises the following steps: using a plasma enhanced chemical vapor deposition apparatus, and depositing a layer of a material on a substrate with C4F8The gas is a reaction gas, and a polytetrafluoroethylene film grows on the surface of the substrate.
3. The method for preparing the three-dimensional nanostructure surface antireflection film for electrons according to claim 2, wherein the method comprises the following steps: the pressure of a cavity in the plasma enhanced chemical vapor deposition equipment is 10-20 Pa, the power is 200-300W, and C4F8The flow rate of the gas is 40-80 sccm.
4. The method for preparing the three-dimensional nanostructure surface antireflection film for the electrons according to claim 1, wherein the method comprises the following steps: the etching process of the third step is as follows: etching quartz glass by using an inductively coupled plasma etching machine, wherein the pressure of a cavity is 1-5 Pa, the power of an upper electrode is 400-600W, the power of a lower electrode is 200-300W, and CHF (CHF) is adopted3As an etching gas, CHF3The flow rate is 40-80 sccm.
5. The method for preparing the three-dimensional nanostructure surface antireflection film for the electrons according to claim 4, wherein the method comprises the following steps: the etching depth of the quartz glass is more than 200nm, and the depth-to-width ratio is more than 2: 1.
6. the method for preparing the three-dimensional nanostructure surface antireflection film for the electrons according to claim 1, wherein the method comprises the following steps: in the fourth step, the mass percentage concentration of the concentrated sulfuric acid is 98%, the mass percentage concentration of the hydrogen peroxide is 30%, and the mass percentage concentration of the concentrated sulfuric acid and the hydrogen peroxide is 3: 1 to form a mixed solution.
7. A method as claimed in claim 1The preparation method of the three-dimensional nanostructure surface antireflection film for the electrons is characterized by comprising the following steps of: the vacuum degree of the second step and the third step is less than 5.0 multiplied by 10-4Pa, and the like.
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| CN103053034A (en) * | 2010-08-02 | 2013-04-17 | 光州科学技术院 | Fabricating method of nano structure for antireflection and fabricating method of photo device integrated with antireflection nano structure |
| CN104934275A (en) * | 2015-05-18 | 2015-09-23 | 北京大学 | Metal molybdenum substrate-based field-induced electron-emitted cathode array and preparation method thereof |
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| JPH03208645A (en) * | 1990-01-11 | 1991-09-11 | Sumitomo Electric Ind Ltd | Fluororesin coated substance denoted with graduation, pattern, character, and the like |
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| CN103053034A (en) * | 2010-08-02 | 2013-04-17 | 光州科学技术院 | Fabricating method of nano structure for antireflection and fabricating method of photo device integrated with antireflection nano structure |
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