CN110194436A - A method of antireflection micro-nano structure is prepared on organic material surface - Google Patents
A method of antireflection micro-nano structure is prepared on organic material surface Download PDFInfo
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- CN110194436A CN110194436A CN201910504740.1A CN201910504740A CN110194436A CN 110194436 A CN110194436 A CN 110194436A CN 201910504740 A CN201910504740 A CN 201910504740A CN 110194436 A CN110194436 A CN 110194436A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00523—Etching material
- B81C1/00531—Dry etching
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C2201/00—Manufacture or treatment of microstructural devices or systems
- B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
- B81C2201/0101—Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
- B81C2201/0128—Processes for removing material
- B81C2201/013—Etching
- B81C2201/0132—Dry etching, i.e. plasma etching, barrel etching, reactive ion etching [RIE], sputter etching or ion milling
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- Drying Of Semiconductors (AREA)
- Surface Treatment Of Optical Elements (AREA)
Abstract
The present invention relates to micro-nano structure preparation technical fields, and in particular to a method of antireflection micro-nano structure is prepared on organic material surface.The present invention carries out reactive ion etching to organic material, forms antireflection micro-nano structure;Wherein, etching gas used in reactive ion etching is oxygen and inert gas, and the flow of oxygen is 1~50SCCM, and the flow of inert gas is 1~100SCCM, and the flow-rate ratio of oxygen and inert gas is 1:(1~10);The power of reactive ion etching is 10~250W.The present invention is based on dry etchings, any mask plate is not used additionally, during carrying out reactive ion etching to organic material, pass through the flow of control oxygen and inert gas, the two proportionate relationship of flow and the power of reactive ion etching, organic material surface can be made to generate redeposited object, redeposited object can be as micro- mask of reactive ion etching, to prepare antireflection micro-nano structure on organic material surface.
Description
Technical field
The present invention relates to micro-nano structure preparation technical fields, and in particular to a kind of micro- in organic material surface preparation antireflection
The method of micro-nano structure.
Background technique
The antireflection of optical element is due to caused by refractive index and the air refraction mutation of optical element.Optical element
The antireflection on surface brings very big uncertainty to optical system, thus antireflection technology is always optical element field emphasis
One of the problem of concern.Currently used antireflection technology is anti-reflective film technology, but anti-reflective film swashs there are at high cost, anti-
The disadvantages of light injury threshold is low, low contamination resistance.And emerging micro-nano structure antireflection technology then in some application fields can be with
Make up the limitation of anti-reflective film.
The scale of antireflection micro-nano structure typically belongs to micro/nano-scale, so its processing belongs to micro-nano technology scope.Micro-nano
The preparation method of structure is broadly divided into two big steps, and the first step is mask preparation, and second step is etching, and mask preparation is limitation
The key factor of micro-nano structure.Existing template fabrication techniques include photoetching process, colloidal crystal template method, thermal annealing method and aluminium oxide
The technologies such as template, but these technologies have some limitations.Photoresist as used in photoetching process works as needs for organic matter
When the substrate for making antireflection micro-nano structure is also organic matter, it will lead to cannot achieve selective etch, another aspect photoetching
Method is limited by diffraction limit, can not prepare smaller micro nano structure;Colloidal crystal template method is difficult to realize heavy caliber, low
The production of cost, mass;Thermal annealing method needs that nano surface metal agglomeration is made to form micro-nano island exposure mask by high temperature, and
The unbearable high temperature of organic substrate, thus antireflection micro-nano knot can not be prepared on organic material surface using thermal annealing method
Structure;Alumina formwork method needs conductive layer, thus is also not suitable for organic material.
Summary of the invention
The purpose of the present invention is to provide a kind of method in organic material surface preparation antireflection micro-nano structure, the present invention
The method of offer, which can additionally not realized using any mask plate, prepares antireflection micro-nano structure on organic material surface, and
It is simple, convenient, it is at low cost.
In order to achieve the above-mentioned object of the invention, the present invention the following technical schemes are provided:
The present invention provides a kind of methods in organic material surface preparation antireflection micro-nano structure, comprising the following steps:
Reactive ion etching is carried out to organic material, forms antireflection micro-nano structure on the organic material surface;Wherein,
Etching gas used by the reactive ion etching is oxygen and inert gas, and the flow of the oxygen is 1~50SCCM, lazy
Property gas flow be 1~100SCCM, and the flow-rate ratio of the oxygen and inert gas be 1:(1~10);The reactive ion
The power of etching is 10~250W.
Preferably, the reactive ion etching carries out under conditions of operating pressure is 0.5~200Pa.
Preferably, the time of the reactive ion etching is 1~60min.
Preferably, the inert gas includes argon gas or helium.
Preferably, the organic material includes cross-linked polyester, polymethyl methacrylate, polyethylene terephthalate
Ester, polyethylene naphthalate, Triafol T, fluorinated ethylene propylene copolymer, polyvinyl alcohol or polycarbonate.
Preferably, the organic material carries out reactive ion etching with organic matter substrate or organic matter coating form.
Preferably, the organic material is using preceding progress surface cleaning processing.
The present invention provides a kind of methods in organic material surface preparation antireflection micro-nano structure, carry out to organic material
Reactive ion etching forms antireflection micro-nano structure on the organic material surface;Wherein, the reactive ion etching is used
Etching gas be oxygen and inert gas, the flow of the oxygen is 1~50SCCM, the flow of inert gas is 1~
100SCCM, and the flow-rate ratio of the oxygen and inert gas is 1:(1~10);The power of the reactive ion etching be 10~
250W.The present invention is based on dry etchings, do not use any mask plate additionally, are carrying out reactive ion etching mistake to organic material
Cheng Zhong passes through the flow of control oxygen and inert gas, the two proportionate relationship of flow and the power of reactive ion etching, energy
So that organic material surface is generated redeposited object, the redeposition object can as micro- mask of the reactive ion etching, from
And antireflection micro-nano structure is prepared on organic material surface, and it is simple, convenient, it is at low cost.
Detailed description of the invention
Fig. 1 is the schematic illustration of method provided by the invention;
Fig. 2 is the scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of sample S1;
Fig. 3 is the scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of sample S2;
Fig. 4 is the scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of sample S3;
Fig. 5 is the scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of sample S4;
Fig. 6 is the transmission spectrum of sample S1~S4 and untreated coating;
Fig. 7 is the strabismus scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of sample S5;
Fig. 8 is the antireflection micro-nano structure of sample S5 and the transmission spectrum of untreated substrate;
Fig. 9 is the strabismus scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of sample S6;
Figure 10 is the antireflection micro-nano structure of sample S6 and the transmission spectrum of untreated coating;
Figure 11 is the strabismus scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of sample S7;
Figure 12 is the antireflection micro-nano structure of sample S7 and the transmission spectrum of untreated substrate;
Figure 13 is the strabismus scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of sample S8;
Figure 14 is the antireflection micro-nano structure of sample S8 and the transmission spectrum of untreated substrate.
Specific embodiment
The present invention provides a kind of methods in organic material surface preparation antireflection micro-nano structure, comprising the following steps:
Reactive ion etching is carried out to organic material, forms antireflection micro-nano structure on the organic material surface;Wherein,
Etching gas used by the reactive ion etching is oxygen and inert gas, and the flow of the oxygen is 1~50SCCM, lazy
Property gas flow be 1~100SCCM, and the flow-rate ratio of the oxygen and inert gas be 1:(1~10);The reactive ion
The power of etching is 10~250W.
The present invention does not have the type of the organic material special restriction, hydrocarbonization well known to those skilled in the art
Close object and its derivative.In the present invention, the organic material preferably includes cross-linked polyester, polymethyl methacrylate
(PMMA), polyethylene terephthalate (PET), polyethylene naphthalate (PEN), Triafol T (TAC), complete
Fluoroethylene-propylene copolymer (FEP), polyvinyl alcohol (PVA) or polycarbonate (PC).
In the present invention, the organic material preferably carries out reactive ion quarter with organic matter substrate or organic matter coating form
Erosion.The present invention does not have special restriction for the organic matter substrate or organic matter coating, selects organic matter according to actual needs
Substrate or organic matter coating.
In the present invention, the organic material is using preceding preferred progress surface cleaning processing.The present invention is for the table
The concrete operation method of face cleaning treatment does not have special restriction, using technical solution well known to those skilled in the art.
In the present invention, etching gas used by the reactive ion etching is oxygen and inert gas, the inertia
Gas preferably includes argon gas or helium.
In the present invention, the flow of the oxygen be 1~50SCCM, preferably 3~30SCCM, more preferably 5~
15SCCM;The flow of the inert gas is 1~100SCCM, preferably 20~80SCCM, more preferably 40~60SCCM;Institute
The flow-rate ratio for stating oxygen and inert gas is 1:(1~10), preferably 1:(5~10), more preferably 1:10;The reactive ion
The power of etching is 10~250W, preferably 50~200W, more preferably 70~150W.
In the present invention, the reactive ion etching preferably carries out under conditions of operating pressure is 0.5~200Pa, more
Preferably 5~100Pa, most preferably 10~50Pa.
In the present invention, the time of the reactive ion etching is preferably 1~60min, more preferably 2~40min, into one
Step is preferably 3~20min, is still more preferably 4~10min.In the present invention, the time of reactive ion etching will affect micro-
The height of micro-nano structure, the too long micro-nano structure that can make organic material surface of etch period is excessive, generates scattering effect to light, causes
Part light is scattered, and transmitance is made to decrease;And the too long organic material that may result in of etch period is denaturalized, and light is produced
It is raw to absorb, to reduce transmitance.The present invention preferably micro-nano structure according to needed for the type of organic material, organic material surface
Size and transmitance select suitable etch period.
The present invention does not have special restriction for carrying out equipment used by the reactive ion etching, using this field skill
Plasma etching equipment known to art personnel.The present invention is preferably to the plasma before carrying out the reactive ion etching
Etching apparatus is cleaned.In the present invention, the cleaning preferably includes the ethyl alcohol successively carried out cleaning and plasma clean;
In an embodiment of the present invention, specifically the reaction chamber of the plasma etching equipment is cleaned using ethyl alcohol, to second
Alcohol carries out inert gas and oxygen gas plasma cleaning again after volatilizing completely, to remove the deposition for being deposited on reaction chamber side wall
Object.
The present invention is based on dry etchings, provide a kind of by preparing anti-reflective on organic material surface from mask etching technology
The method for penetrating micro-nano structure, specifically, passing through control oxygen and inertia during carrying out reactive ion etching to organic material
Flow, the two proportionate relationship of flow and the power of reactive ion etching of gas, can be such that organic material surface generates again
(during the reactive ion etching, oxonium ion reacts deposit with organic material surface, the volatile etch of generation
Product, such as CO, CO2And H2O, as vacuum system is pumped, remaining fixedness etch product is redeposited object), it is described
Redeposited object can be as micro- mask of the reactive ion etching, to prepare antireflection micro-nano knot on organic material surface
Structure (schematic illustration is as shown in Figure 1).
Method provided by the invention does not use any mask plate additionally, only passes through the stream of control oxygen and inert gas
Amount, the two proportionate relationship of flow and the power of reactive ion etching, can be realized and prepare antireflection on organic material surface
Micro-nano structure, it is simple, convenient, it is at low cost.
Below in conjunction with the embodiment in the present invention, the technical solution in the present invention is clearly and completely described.It is aobvious
So, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on the reality in the present invention
Example is applied, every other embodiment obtained by those of ordinary skill in the art without making creative efforts all belongs to
In the scope of protection of the invention.
Examples 1 to 4
According to etching parameters in table 1, reactive ion etching is carried out using cross-linked polyester coating as sample to be etched, described
The surface of sample to be etched forms antireflection micro-nano structure, respectively obtains sample S1~S4;Wherein, the reactive ion is being carried out
Before etching, surface cleaning processing is carried out to the sample to be etched, and using ethyl alcohol to the reaction chamber of plasma etching equipment
It is cleaned, carries out argon gas and oxygen gas plasma cleaning again after ethyl alcohol volatilizees completely, be deposited on reaction chamber to remove
The deposit of side wall.
The selection of etching parameters in 1 Examples 1 to 4 of table
Fig. 2~5 are the scanning electron microscope (SEM) photographs of the antireflection micro-nano structure of the sample S1~S4, wherein (A) is to overlook scanning
Electron microscope, (B) are side view scanning electron microscope (SEM) photograph.By Fig. 2~5 it is found that the average height of the antireflection micro-nano structure of sample S1~S4
It is followed successively by 210nm, 252nm, 308nm, 345nm.
Fig. 6 is the transmission spectrum of the sample S1~S4 and untreated coating, wherein the anti-reflection effect uses
950 spectrophotometer of Lambda (Perkin Elmer) is tested, and the test scope of transmitted spectrum is 400~1100nm.By
Fig. 6 it is found that when etch period be 60s when (counter sample S1), since surface only has the nano dot structure of very little, thus, anti-reflective
It is general to penetrate performance, highest transmitance is 93%;When etch period reaches 120s (counter sample S2), highest transmitance is close
97%;When etch period is 180s (counter sample S3), transmitance is about 99%;It is (right to 240s to further increase etch period
Answer sample S4), discovery transmitance declines instead, and highest transmitance is 97.2%.It is best to etch thus for cross-linked polyester
Time is 180s.
Embodiment 5
According to the preparation method of embodiment 1, carried out using polymethyl methacrylate (PMMA) substrate as sample to be etched
Reactive ion etching forms antireflection micro-nano structure on the surface of the sample to be etched, obtains sample S5;Wherein, etching ginseng
Number is listed in Table 2 below.
The selection of etching parameters in 2 embodiment 5 of table
Fig. 7 is the strabismus scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of the sample S5, as shown in Figure 7, the surface sample S5
After etched, pass meshed texture is presented in the antireflection micro-nano structure bottom of formation, these pass reticular structures are in sample S5 table
Face is uniformly distributed, and average height is about 233nm.
Fig. 8 be the sample S5 antireflection micro-nano structure and untreated substrate transmission spectrum, as shown in Figure 8,
In 400~1100nm wave-length coverage, sample S5 antireflective property is preferable, and highest transmitance is up to 98.3%.
Embodiment 6
According to the preparation method of embodiment 1, reactive ion quarter is carried out using polyvinyl alcohol (PVA) coating as sample to be etched
Erosion forms antireflection micro-nano structure on the surface of the sample to be etched, obtains sample S6;Wherein, etching parameters are listed in table 3
In.
The selection of etching parameters in 3 embodiment 6 of table
Fig. 9 is the strabismus scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of the sample S6, as shown in Figure 9, the surface sample S6
After etched, the antireflection micro-nano structure of formation is uniformly distributed, and average height is about 169nm.
Figure 10 be the sample S6 antireflection micro-nano structure and untreated coating transmission spectrum, can by Figure 10
Know, in 400~1100nm wave-length coverage, the antireflective property of sample S6 is relatively good, and highest transmitance is 96.6%.
Embodiment 7
According to the preparation method of embodiment 1, carried out using fluorinated ethylene propylene copolymer (FEP) substrate as sample to be etched
Reactive ion etching forms antireflection micro-nano structure on the surface of the sample to be etched, obtains sample S7;Wherein, etching ginseng
Number is listed in Table 4 below.
The selection of etching parameters in 4 embodiment 7 of table
Figure 11 is the strabismus scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of the sample S7, as shown in Figure 11, sample S7 table
After face is etched, some tiny nanometer paxillas are formd, average height is about 107nm.
Figure 12 be the sample S7 antireflection micro-nano structure and untreated substrate transmission spectrum, can by Figure 12
Know, in 400~1100nm wave-length coverage, the antireflective property of sample S7 is relatively good, and highest transmitance is 96.4%.
Embodiment 8
According to the preparation method of embodiment 1, reactive ion quarter is carried out using polycarbonate (PC) substrate as sample to be etched
Erosion forms antireflection micro-nano structure on the surface of the sample to be etched, obtains sample S8;Wherein, etching parameters are listed in table 5
In.
The selection of etching parameters in 5 embodiment 8 of table
Figure 13 is the strabismus scanning electron microscope (SEM) photograph of the antireflection micro-nano structure of the sample S8, as shown in Figure 13, sample S8 table
After face is etched, the anti-reflection structure profile of formation is obvious, and average height is about 187nm.
Figure 14 be the sample S8 antireflection micro-nano structure and untreated substrate transmission spectrum, can by Figure 14
Know, in 400~1100nm wave-length coverage, the antireflective property of sample S8 is relatively good, and highest transmitance is 97.3%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of method in organic material surface preparation antireflection micro-nano structure, which comprises the following steps:
Reactive ion etching is carried out to organic material, forms antireflection micro-nano structure on the organic material surface;Wherein, described
Etching gas used by reactive ion etching is oxygen and inert gas, and the flow of the oxygen is 1~50SCCM, indifferent gas
The flow of body is 1~100SCCM, and the flow-rate ratio of the oxygen and inert gas is 1:(1~10);The reactive ion etching
Power be 10~250W.
2. the method according to claim 1, wherein the reactive ion etching operating pressure be 0.5~
It is carried out under conditions of 200Pa.
3. according to the method described in claim 2, it is characterized in that, the time of the reactive ion etching is 1~60min.
4. described in any item methods according to claim 1~3, which is characterized in that the inert gas includes argon gas or helium.
5. described in any item methods according to claim 1~3, which is characterized in that the organic material includes cross-linked polyester, gathers
Methyl methacrylate, polyethylene terephthalate, polyethylene naphthalate, Triafol T, perfluoroethylene
Propylene copolymer, polyvinyl alcohol or polycarbonate.
6. according to the method described in claim 5, it is characterized in that, the organic material is with organic matter substrate or organic matter coating
Form carries out reactive ion etching.
7. the method according to claim 1, wherein the organic material is using at preceding progress surface cleaning
Reason.
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