CN107949901B - Method for manufacturing anti-reflection surface by plasma etching and substrate with anti-reflection surface - Google Patents
Method for manufacturing anti-reflection surface by plasma etching and substrate with anti-reflection surface Download PDFInfo
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- CN107949901B CN107949901B CN201680047856.1A CN201680047856A CN107949901B CN 107949901 B CN107949901 B CN 107949901B CN 201680047856 A CN201680047856 A CN 201680047856A CN 107949901 B CN107949901 B CN 107949901B
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Images
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/3065—Plasma etching; Reactive-ion etching
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/50—Assembly of semiconductor devices using processes or apparatus not provided for in a single one of the subgroups H01L21/06 - H01L21/326, e.g. sealing of a cap to a base of a container
- H01L21/56—Encapsulations, e.g. encapsulation layers, coatings
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0216—Coatings
- H01L31/02161—Coatings for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/02167—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells
- H01L31/02168—Coatings for devices characterised by at least one potential jump barrier or surface barrier for solar cells the coatings being antireflective or having enhancing optical properties for the solar cells
Abstract
The present invention relates to a method for manufacturing an anti-reflection surface and a substrate having an anti-reflection surface formed thereon, which can improve durability and ensure excellent light transmittance and anti-reflection effect by controlling an anti-reflection structure layer formed by repeating plasma dry etching and deposition of an inorganic substance to various structures, and which has functions such as easy cleaning, stain resistance, scratch resistance, and the like.
Description
Technical Field
The present invention relates to a method for manufacturing an antireflection surface by plasma etching and a substrate having an antireflection surface formed thereon.
Background
In the field of optical applications in the display and optical industry, that is, in optical lenses, glasses, solar panels, Personal Computers (PCs), Televisions (TVs), Automated Teller Machines (ATMs), car navigators, and the like, antireflection technology is used in order to prevent a decrease in energy efficiency due to reflection of light, irritation to the eyes of a user, a phenomenon in which it is difficult to confirm a screen or an object, and the like. In such an antireflection technology, a technology has been proposed which is realized by imitating the surface of an insect or a plant in the natural world.
In particular, many studies have been made on the production of a surface that simulates a Moth-eye (Moth-eye) surface to obtain an antireflection effect. This technology can obtain an antireflection effect by forming a protrusion pattern such as moth-eye on the surface of the substrate to guide scattering of light on the surface. However, there is a problem that the durability is reduced when realizing a surface such as a moth eye.
In addition, as the application field of the anti-reflection technology is changed from the existing Display market to the Flexible Display (Flexible Display) market, the used substrate shows a tendency to be changed from Glass (Glass) to polymer series. The use of such materials is expected to be more and more active because of the visual, spatial, and mechanical flexibility of polymer-based substrates.
Korean patent application No. 10-2012-0027763, which is a conventional anti-reflective technology, discloses a method for manufacturing an anti-reflective substrate by deforming a surface of the substrate and depositing an inorganic substance. However, the antireflection structure cannot be controlled to various forms, and can be reproduced only to the same structure.
Also, korean laid-open patent publication No. 10-2014-0074874 discloses a technique of applying a hydrophobic layer after forming a structure on a substrate using a metal dot as a mask when dry etching is performed, removing a metal substance with an acid, and depositing an antireflection film. However, since the metal dots are used, it is necessary to remove the metal dots by an acid after forming the uneven portions on the substrate by dry etching, which is relatively complicated, and since the metal dots are deposited unevenly in units of nm to μm, a uniform thin film cannot be obtained.
Also, korean laid-open patent publication No. 10-2012-0063725 discloses a technique of controlling a structure by forming a polymer layer on a substrate, using the polymer layer as a protective layer (Mask) when etching is performed, and removing the polymer layer after forming a protrusion pattern on the substrate. Although this technique can control the morphology of the substrate, it is unpredictable in which morphology an inorganic or organic material will grow when deposited on the substrate, and the polymer layer needs to be completely removed before subsequent processes can be performed.
Disclosure of Invention
Technical problem to be solved
The present invention has an object to provide a method for manufacturing an anti-reflection surface and a substrate having an anti-reflection surface formed thereon, in which a structure layer having an anti-reflection structure formed thereon is controlled to have various structures by repeating plasma dry etching and inorganic deposition, thereby improving durability, ensuring excellent light transmittance and anti-reflection effect, and providing functions such as easy cleaning, stain resistance, scratch resistance, and the like.
(II) technical scheme
The method for manufacturing an antireflection surface by plasma etching according to the present invention includes the steps of: i) forming a concave-convex part on the surface of the base material by using plasma dry etching; ii) forming an antireflection structure capable of preventing light reflection on the uneven portion by depositing inorganic particles, thereby forming an antireflection layer on the surface of the substrate; and iii) stand-alone rethreadingPerforming one or more of said steps i) or ii), in which step i) the plasma dry etching is at 5 x 10-3To 5 x 10-2Initial pressure conditions of torr, 5 x 10-2To 5 x 10-1torr under process pressure conditions.
An antireflection substrate according to the present invention includes: a substrate having a concave-convex portion formed on one surface thereof; and an anti-reflection layer formed on the surface of the substrate and including anti-reflection structures formed on the uneven portion by depositing inorganic particles, the anti-reflection layer including a plurality of anti-reflection structures having a trapezoidal cross section, a plurality of anti-reflection structures having an air layer therein and an inverted trapezoidal cross section, or a plurality of anti-reflection structures having a triangular cross section, the uneven portion being formed on one surface of the substrate by plasma dry etching, the plasma dry etching being performed at 5 x 10-3To 5 x 10- 2Initial pressure conditions of torr, 5 x 10-2To 5 x 10-1torr under process pressure conditions.
(III) advantageous effects
According to the present invention, an anti-reflection surface can be manufactured, and by controlling the anti-reflection layer to have various structures, it is possible to improve durability, ensure excellent light transmittance and anti-reflection effect, and have functions such as easy cleaning, stain resistance, scratch resistance, and the like.
Drawings
Fig. 1 is a schematic view of an antireflection substrate having antireflection layers of structures 1 to 3 according to an embodiment of the present invention.
Fig. 2 is a flowchart showing a method for manufacturing an antireflection surface by plasma etching according to an embodiment of the present invention.
Fig. 3 is a schematic view showing a process for manufacturing an antireflection substrate having antireflection layers of structures 1 to 3 according to an embodiment of the present invention.
Fig. 4 is a photograph of the cross-section of the anti-reflection layer of structures 1 to 3 according to one embodiment of the present invention taken with an electron microscope.
Fig. 5 is a photograph of the surfaces of the antireflection layers of structures 1 to 3 according to one embodiment of the present invention taken with an electron microscope.
Fig. 6 is a graph showing light transmittance of the anti-reflection substrate having the anti-reflection layer of structures 1 to 3 according to the embodiment of the present invention and the anti-reflection substrate of the comparative example.
FIG. 7 is a photograph (SEM Image) of the uneven portions formed after the plasma dry etching process was performed in examples 4 to 7 and comparative examples 1 to 3, taken by an electron microscope.
Fig. 8 is a photograph (SEM Image) of the anti-reflection structure formed after the inorganic deposition process in examples 4 to 7 and comparative example 2, taken with an electron microscope.
FIG. 9 is a graph showing the results of measuring a plurality of contact angles after durability tests were performed on the anti-reflection substrates of examples 4 to 7 and comparative examples 1 to 3.
Fig. 10 is a graph of the measurement results of the light transmittance and the reflectance of the substrate manufactured under the same conditions as in example 6.
Detailed Description
The present invention will be described in more detail below with reference to the accompanying drawings.
The method for manufacturing an antireflection surface by plasma etching according to the present invention is characterized by comprising: i) forming a concave-convex part on the surface of the base material by using plasma dry etching; ii) forming an antireflection structure capable of preventing light reflection on the uneven portion by depositing inorganic particles, thereby forming an antireflection layer on the surface of the substrate; and iii) performing said step i) or step ii) one or more times separately, in which step i) the plasma dry etch is at 5 x 10-3To 5 x 10-2Starting at an initial pressure of 5 x 10 torr-2To 5 x 10-1Torr (torr).
The initial pressure condition in the step i) (hereinafter also referred to as "pretreatment step") was 5 × 10-3To 5 x 10- 2torr, preferably 6 x 10-3To 5 x 10-2torr, more preferably 1 x 10-2To 4 x 10-2torr。And, the process pressure conditions in said step i) are 5 x 10-2To 5 x 10-1torr, preferably 9 x 10-2To 3 x 10-1torr. When the initial pressure condition and the process pressure condition in the step i) are higher than the above-mentioned levels, the plasma dry etching cannot be smoothly performed, and on the contrary, when the initial pressure condition and the process pressure condition in the step i) are lower than the levels, the density of the pattern becomes excessively high, and when an inorganic substance is deposited on the pattern in a subsequent step, the concave and convex portions are not supported and broken, and the durability of the nano surface structure is lowered.
Conventional methods for producing an antireflection surface cannot control various nano-surface structures and reduce durability due to repeated touch.
The method for manufacturing an anti-reflection surface using plasma etching according to the present invention can improve such disadvantages of the prior art, and can manufacture an anti-reflection surface having improved durability and excellent light transmittance and anti-reflection effect by controlling and realizing the anti-reflection layers of various nano surface structures as shown in fig. 1. The structure of the anti-reflection surface can be controlled by the number of repetitions of each step, etching time, etching gas type, inorganic substance thickness, and the like.
Fig. 2 is a flowchart showing a method for manufacturing an anti-reflection surface by plasma etching according to an embodiment of the present invention, and fig. 3 is a schematic view showing a process for manufacturing an anti-reflection substrate having an anti-reflection layer of structures 1 to 3 according to an embodiment of the present invention, and the following description will be made with reference to the above drawings.
In step i), the uneven portion may be formed on the surface of the base material by plasma dry etching. Although not particularly limited, the plasma dry etching may utilize plasma (direct current (DC), direct current pulse, Radio Frequency (RF), End-Hole (End-Hole), etc.) dry etching installed in the vacuum deposition apparatus. And, the plasma dry etching of step i) may be performed in the presence of a material selected from Ar, O2、H2He and N2Under at least one gas condition.
Since the step of forming the concave-convex portion on the surface of the base material uses the plasma dry etching, the formation of the concave-convex portion can be controlled more accurately than in the case of performing etching using wet etching. When the substrate is exposed to plasma formed from at least one gas including the gas species, the surface of the substrate is etched to form the concave-convex portion.
In this case, the optical characteristics of the antireflection surface of the present invention are controlled by an antireflection layer composed of an antireflection structure described in detail later, and in order to control the pitch between the antireflection structures, it is necessary to control the pitch of the uneven portions forming the antireflection structure. Only if the uneven structure of the surface is accurately formed in the step i), the morphology and durability of the deposited inorganic (e.g., oxide) antireflection structure desired in the subsequent process can be obtained.
In one embodiment, Ar, O2Etc. and the distance between the gas inlet and the substrate (hereinafter also referred to as "substrate distance") may be less than or equal to 200mm (e.g., 50 to 200mm), preferably less than or equal to 150mm (e.g., 50 to 150 mm).
In one embodiment, the power per unit area for plasma dry etching may be 0.2 to 17W/cm2Preferably 0.5 to 16W/cm2More preferably 1 to 16W/cm2. Also, the voltage may be 10 to 1000V, preferably 50 to 600V.
In one embodiment, Ar, O for plasma dry etching2The gas flow rate can be 10sccm to 200sccm, preferably 20sccm to 100sccm, more preferably 20sccm to 50 sccm.
In one specific example, the plasma dry etching may be performed for, for example, 20 seconds to 1 hour, preferably 30 seconds to 50 minutes.
In one embodiment, after the plasma dry etching is performed, the width of the obtained pattern is preferably 10 to 300nm, more preferably 10 to 250nm, the height of the pattern is preferably 10 to 200nm, more preferably 10 to 150nm, and the pitch between the patterns is preferably 10 to 200nm, more preferably 10 to 150 nm.
The base material used in the present invention may be a polymer-based substrate, for example, a material of polyether ether ketone (PEEK), polyether sulfone (PES), polyether imide (PEI), Polycarbonate (PC), polyethylene naphthalate (PEN), polyethylene terephthalate (PET), or polymethyl methacrylate (PMMA), but is not particularly limited thereto, and a substrate subjected to Hard Coating (Hard Coating) may be used.
The substrate of the present invention may include a strengthening coating formed on the surface. The strengthening coating can improve physical properties such as strength and hardness of the substrate, and can also improve adhesion of an anti-reflection layer subsequently laminated on the substrate. Further, the formation of the reinforcing coating layer can improve the optical properties of the base material and also improve the chemical resistance.
The polymer coating material used for forming the reinforced coating layer may be one composed of at least one of acrylic, polyurethane, epoxy and primer coating materials, and any polymer coating material that can exert the above-described effects on the substrate may be included in the scope of the present invention.
Also, the reinforced coating layer provided according to the present embodiment may be formed by mixing inorganic fine particles, such as metal oxide, sulfide, alumina, silica, zirconia, iron oxide, etc., into the polymer paint.
In step ii), an antireflection structure capable of preventing reflection of light may be formed on the uneven portion by depositing inorganic particles, so as to form an antireflection layer on one surface of the substrate. Although not particularly limited, the inorganic particles may include at least one selected from the group consisting of oxides, nitrides, oxynitrides (oxynitrides), and fluorides of metals, wherein the metals may Be selected from the group consisting of Al, Ba, Be, Ca, Cr, Cu, Cd, Dy, Ga, Ge, Hf, In, Lu, Mg, Mo, Ni, Rb, Sc, Si, Sn, Ta, Te, Ti, W, Zn, Zr, Yb, and combinations thereof.
The deposition method of the inorganic particles is not particularly limited, and may be performed by, for example, a physical vapor deposition method, a chemical vapor deposition method, or an ion-assisted vapor deposition method.
In step iii), the previously performed step i) or step ii) may be performed one or more times separately again. That is, by repeatedly performing inorganic deposition and dry etching using plasma, an antireflection layer having the structure of structures 1 to 3 shown in fig. 1 can be formed.
In one embodiment, the initial pressure condition in said step ii) (hereinafter also referred to as "inorganic deposition step") may be 1 x 10-3To 5 x 10-2torr, preferably 1 x 10-3To 2 x 10-2torr. And, the process pressure conditions in said step ii) are 1 x 10-3To 5 x 10-1torr, preferably 1 x 10-2To 2 x 10-1torr。
In one embodiment, the final anti-reflective layer deposited with the inorganic material has a thickness of preferably 10 to 500nm, more preferably 20 to 300 nm.
In one embodiment, the width of the final anti-reflective structure deposited with the inorganic substance is preferably 10 to 500nm, more preferably 30 to 450 nm.
In one embodiment, the final anti-reflective structure deposited with the inorganic material has a height of preferably 10 to 400nm, more preferably 20 to 350 nm.
In one embodiment, the spacing between the final anti-reflective structures deposited with the inorganic is preferably 10 to 200nm, more preferably 10 to 150 nm.
When the anti-reflection layer (anti-reflection layer composed of a plurality of anti-reflection structural bodies having a trapezoidal cross section) of the structure 1 shown in fig. 1 is formed, after step i) and step ii) are performed again 1 to 20 times, step i) is finally performed, and the thickness of the inorganic substance deposited in each step ii) is gradually reduced. For example, a plasma etch is carried out for 10 minutes in step i), and a deposition is carried out in step ii)
After the inorganic substance(s), plasma etching was performed for 10 minutes in step iii) to deposit
Then, plasma etching was again performed for 10 minutes,then depositing
Finally, the inorganic substance (2) was subjected to plasma etching for 10 minutes.
When the anti-reflection layer (anti-reflection layer composed of a plurality of anti-reflection structures including an air layer inside and having an inverted trapezoidal cross section) of the structure 2 shown in fig. 1 is formed, step ii) is performed again 1 to 20 times in step iii), and the thickness of the inorganic substance deposited in each step ii) is the same. For example, a plasma etch is carried out for 10 minutes in step i), and a deposition is carried out in step ii)
After the inorganic substance(s), deposition is repeated three times without plasma etching in step iii)
The inorganic substance of (1).
When the antireflection layer (antireflection layer composed of a plurality of antireflection structures having a triangular cross section) of the structure 3 shown in fig. 1 is formed, the step i) and the step ii) may be sequentially performed 1 to 20 times the same number of times in the step iii). For example, a plasma etch is carried out for 10 minutes in step i), and a deposition is carried out in step ii)
After the inorganic substance(s), plasma etching for 10 minutes was repeatedly performed three times in step iii) and deposition was performed
The inorganic substance of (1).
In the method of the present invention, after the step iii), the method may further include the steps of: iv) forming a protective layer on a surface of the substrate opposite to the surface on which the antireflection layer is formed.
The protective layer can prevent penetration of foreign substances, such as oxygen, water, etc., which may be absorbed by the base material to contaminate the base material and the inside of the product, or foreign substances which may cause defects in the product, and protect the surface of the base material from the external environment, and enhance the hardness of the base material itself. The protective layer may be formed by depositing a silicone Oil (Si-Oil) type compound such as Epoxy (Epoxy), Mercapto (Mercapto), Acrylate (acryl), Methacrylate (Methacrylate) or the like or a fluorine Oil (F-Oil) type compound such as Polyvinyl fluoride (PVF), Polyvinylidene fluoride (PVDF), polychlorotrifluoroethylene (pctfe), Ethylene-tetrafluoroethylene copolymer (Ethylene tetrafluoroethylene (etfe)), polytetrafluoroethylene (ptfe)), perfluoroalkylene (ptfe), perfluoroalkoxy (pfa) (pffe), Vinylidene fluoride (vihylene fluoride (F)), tetrafluoroethylene (tfe)), tetrafluoroethylene (tfe-tetrafluoroethylene (tfe)), tetrafluoroethylene (tfe-tfe) (tfe-co-tetrafluoroethylene (tfe)), tetrafluoroethylene (tfe-co-tetrafluoroethylene (tfe)), tetrafluoroethylene (tfe-tetrafluoroethylene (tfe)), tetrafluoroethylene (tfe-co-tetrafluoroethylene (tfe)), tetrafluoroethylene (tfe-tetrafluoroethylene (tfe) (tfe-tetrafluoroethylene (tfe)), tetrafluoroethylene (tfe-tetrafluoroethylene (tfe)), tetrafluoroethylene (tfe-tetrafluoroethylene (tfe) (tfe-tetrafluoroethylene (tfe)), tetrafluoroethylene (tfe) or (tetrafluoroethylene), (tfe) copolymer (tetrafluoroethylene), (tfe) and (tetrafluoroethylene), (tfe) copolymer (tetrafluoroethylene), (tfe) and (tetrafluoroethylene), (tfe) and (tetrafluoroethylene copolymer (tetrafluoroethylene), (tfe) and (tetrafluoroethylene) (tetrafluoroethylene) (tfe) and (tetrafluoroethylene copolymer (tetrafluoroethylene) (tfe) and (tetrafluoroethylene) (tfe)) may be) (tetrafluoroethylene) (tfe) and tetrafluoroethylene) (.
According to another aspect of the present invention, there is provided an antireflection substrate including: a base material having a surface formed with a concave-convex portion; and an anti-reflection layer formed on the surface of the substrate and including anti-reflection structures formed on the uneven portion and formed by depositing inorganic particles, wherein the anti-reflection layer includes a plurality of anti-reflection structures having a trapezoidal cross section, a plurality of anti-reflection structures having an air layer therein and an inverted trapezoidal cross section, or a plurality of anti-reflection structures having a triangular cross section, and the uneven portion is formed on one surface of the substrate by plasma dry etching at 5 × 10-3To 5 x 10-2Initial pressure conditions of torr, 5 x 10-2To 5 x 10-1torr under process pressure conditions.
The base material may be a polymer-based substrate, for example, a material of polyether ether ketone (PEEK), polyether sulfone (PES), polyether imide (PEI), Polycarbonate (PC), polyethylene naphthalate (PEN), polyethylene terephthalate (PET), or polymethyl methacrylate (PMMA), but is not particularly limited thereto, and a substrate subjected to a hardening coating may be used.
The inorganic particles may include at least one selected from the group consisting of oxides, nitrides, oxynitrides, and fluorides of metals selected from the group consisting of Al, Ba, Be, Ca, Cr, Cu, Cd, Dy, Ga, Ge, Hf, In, Lu, Mg, Mo, Ni, Rb, Sc, Si, Sn, Ta, Te, Ti, W, Zn, Zr, Yb, and combinations thereof.
The antireflection substrate of the present invention may further include a protective layer on a surface of the base material opposite to the surface on which the antireflection layer is formed.
The protective layer can prevent penetration of foreign substances, such as oxygen, water, etc., absorbed by the substrate to contaminate the substrate and the inside of the product or cause defects of the product, and protect the surface of the substrate from the external environment.
The protective layer may be formed by depositing a Si-Oil type compound or an F-Oil type compound, and the aforementioned Si-Oil type compound or F-Oil type compound may be used.
The present invention will be described in more detail below with reference to examples and comparative examples. Although the scope of the invention is not limited in this respect.
[ examples ]
1. Production of antireflection substrate
The processes as described in the following table 1 were performed to manufacture the anti-reflection substrates of examples 1 to 3 having the anti-reflection layers of structures 1 to 3. The "etching" in table 1 below refers to the time when plasma etching is performed,
means to deposit SiO2The thickness of the particles. Examples 1 to 3 used a polyethylene terephthalate (PET) substrate as a base material, and used Top Clean Safe (Ceko corporation) made of F-Oil compound for forming a protective layer.
[ Table 1]
The cross section and the surface of the antireflection layer of each of the antireflection substrates of examples 1 to 3 produced were photographed by an electron microscope, and shown in fig. 4 and 5. As can be confirmed from fig. 4, the anti-reflection layer including a plurality of anti-reflection structures having a trapezoidal cross section, a plurality of anti-reflection structures having an air layer therein and an inverted trapezoidal cross section, or a plurality of anti-reflection structures having a triangular cross section can be formed by adjusting the number of repetitions of each process, the deposition thickness of the inorganic substance, and the like. As can be seen from fig. 5, the surface of the antireflection layer is formed in a protrusion form such as a moth eye.
2. Measuring optical characteristics of anti-reflection substrate
The light transmittance of the fabricated anti-reflection substrates of examples 1 to 3 and the substrate of comparative example (PET substrate subjected to the curing coating) was measured and shown in fig. 6. As can be seen from fig. 6, the anti-reflection substrate of the present invention exhibited superior light transmittance at the same wavelength as the substrate of the comparative example.
3. Examples 4 to 7 and comparative examples 1 to 3
The anti-reflection substrate (base material) was manufactured using the plasma dry etching process [ said step i) ] conditions described in table 2 below and the inorganic substance deposition process [ said step ii) ] conditions described in table 3 below: PET). Sample numbers 1 to 4 represent examples 4 to 7, respectively, and sample numbers 5 to 7 represent comparative examples 1 to 3, respectively.
TABLE 2 plasma Dry etch Process conditions
[ Table 3 ]]Inorganic Substance (SiO)2) Deposition process conditions
NA: without measurement and imaging
The uneven portion formed after the plasma dry etching process was performed was photographed by an electron microscope, and is shown in fig. 7, and the anti-reflection structure formed after the inorganic deposition process was performed was photographed by an electron microscope, and is shown in fig. 8.
The antireflection substrates of examples 4 to 7 and comparative examples 1 to 3 thus produced were subjected to durability test (Rubber test) using loads of 500g and 1kg and cycles of 1500, 3000 and 5000 after forming a protective layer thereon. As a comparative example, a substrate (Bare polyethylene terephthalate (barepet)) was used. The initial contact angles before the test and the contact angles after the test were measured, and the results are shown in table 4 below and fig. 9.
Then, a substrate having an antireflection layer formed on one Side (Single Side Moth-eye) and a substrate having antireflection layers formed on both sides (Dual Side Moth-eye) were produced under the same conditions as in example 6, and then their transmittances and reflectances were measured, and the results are shown in table 5 below and fig. 10 below. As a comparative example, a substrate (Bare polyethylene terephthalate (barepet)) was used.
Table 4 durability test results: multiple contact angle (°)
[ Table 5] measurement results of transmittance and reflectance (550nm)
| Bare PET | Single-sided moth eye | Double-sided moth eye | |
| Reflectivity of light | 7.80％ | 4.20％ | 0.80％ |
| Transmittance of light | 92.20％ | 95.50％ | 98.50％ |
In examples 4 to 7 (sample nos. 1 to 4), when the plasma dry etching process is performed, the patterns are arranged in a width of 10 to 220nm, a height of 10 to 150nm, and a pitch of 10 to 120nm, and small fine patterns are formed between the large patterns, and when an inorganic substance and a protective layer are deposited on the patterns by a subsequent process, transmittance, reflectance, a contact angle, and durability can be simultaneously improved. The durability is improved because the inorganic substance deposited on the small pattern positioned at the lower portion of the large pattern plays a role of a support for supporting the large pattern during the inorganic substance deposition process, thereby imparting strong durability to physical pressure from the outside.
On the other hand, in the case of comparative example 1 (sample No. 5) or comparative example 2 (sample No. 6), when the plasma dry etching process is performed in a state where the initial pressure is too low or the initial pressure and the process pressure are too low, a pattern density of a pattern having a width of 20 to 80nm, a height of 80 to 250nm, and a pitch of 10 to 50nm becomes high, and in such a state where the pattern density becomes high, when an oxide is coated on the pattern, a phenomenon that the pattern is physically unsupported and is immediately broken occurs. Further, as in comparative example 3 (sample No. 7), when the plasma dry etching process was performed in a state where the process pressure was excessively high, a phenomenon that no pattern was generated was shown.
The process time is adjustable, and can be selected to be long time or short time, which is also a preparation step for carrying out mass production subsequently. In the embodiment, the time for controlling the exposure of the surface to the plasma may be adjusted to 40 seconds to 40 minutes, which means that neither process is much problematic as a subsequent process. That is, the patterning can be performed in a subsequent process time, thereby facilitating mass production.
Claims (14)
1. A method for manufacturing an antireflection surface by plasma etching, comprising the steps of:
i) forming a concave-convex part on one surface of the base material by using plasma dry etching;
ii) forming an antireflection structure capable of preventing light reflection on the uneven portion by depositing inorganic particles, thereby forming an antireflection layer on one surface of the substrate; and
iii) performing said step i) or step ii) one or more times separately,
in said step i), the plasma dry etching is at 5 x 10-3To 5 x 10-2Initial pressure conditions of torr, 5 x 10-2To 5 x 10-1the process is carried out under the process pressure conditions of the torr,
after said steps i) and ii) are performed 1 to 20 times again in step iii), step i) is finally performed,
the thickness of the mineral deposited in each step ii) gradually decreases.
2. The method of manufacturing an antireflection surface by plasma etching according to claim 1,
the power per unit area for plasma dry etching is 0.2 to 17W/cm2。
3. The method of manufacturing an antireflection surface by plasma etching according to claim 1,
plasma dry etching was performed for 20 seconds to 1 hour.
4. The method of manufacturing an antireflection surface by plasma etching according to claim 1,
after the plasma dry etching is performed, the width of the obtained pattern is 10 to 300nm, the height of the pattern is 10 to 200nm, and the pitch between the patterns is 10 to 200 nm.
5. The method of manufacturing an antireflection surface by plasma etching according to claim 1,
the base material is a substrate made of polyether-ether-ketone, polyether-sulfone, polyether-imide, polycarbonate, polyethylene naphthalate, polyethylene terephthalate or polymethyl methacrylate.
6. The method of manufacturing an antireflection surface by plasma etching according to claim 1,
step i) by reacting in the presence of a compound selected from Ar, O2、H2He and N2Is performed by performing plasma dry etching under the condition of at least one gas of (1).
7. The method of manufacturing an antireflection surface by plasma etching according to claim 6,
the distance between the gas inlet and the substrate is less than or equal to 200 mm.
8. The method of manufacturing an antireflection surface by plasma etching according to claim 6,
the gas flow rate is 10sccm to 200 sccm.
9. The method of manufacturing an antireflection surface by plasma etching according to claim 1,
the inorganic particles In step ii) include at least one selected from the group consisting of oxides, nitrides, oxynitrides, and fluorides of metals selected from the group consisting of Al, Ba, Be, Ca, Cr, Cu, Cd, Dy, Ga, Ge, Hf, In, Lu, Mg, Mo, Ni, Rb, Sc, Si, Sn, Ta, Te, Ti, W, Zn, Zr, Yb, and combinations thereof.
10. The method of manufacturing an antireflection surface by plasma etching according to claim 1,
the initial pressure conditions in said step ii) are 1 x 10-3To 5 x 10-2torr, process pressure conditions 1 x 10-3To 5 x 10-1torr。
11. The method of manufacturing an antireflection surface by plasma etching according to claim 1,
the final anti-reflection layer deposited with the inorganic substance has a thickness of 10 to 500nm, the final anti-reflection structure deposited with the inorganic substance has a width of 10 to 500nm, the final anti-reflection structure deposited with the inorganic substance has a height of 10 to 400nm, and a pitch between the final anti-reflection structure deposited with the inorganic substance is 10 to 200 nm.
12. The method of manufacturing an antireflection surface by plasma etching according to claim 1,
step ii) is performed by physical vapor deposition, chemical vapor deposition or ion assisted vapor deposition.
13. The method of manufacturing an antireflection surface by plasma etching according to claim 1,
after the step iii), further comprising the steps of: iv) forming a protective layer on the surface of the substrate opposite to the surface on which the antireflection layer is formed.
14. The method of manufacturing an antireflection surface by plasma etching according to claim 13,
in the iv) step, a protective layer is formed by depositing a silicone-based compound or a fluorine-based compound.
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| PCT/KR2016/009245 WO2017034262A1 (en) | 2015-08-21 | 2016-08-22 | Method for manufacturing anti-reflective surface using plasma etching, and substrate having anti-reflective surface formed thereon |
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| DE102018109884B4 (en) * | 2018-04-24 | 2023-07-27 | Webasto SE | Sensor arrangement with screen element and method for producing the screen element |
| JP2020184002A (en) * | 2019-05-07 | 2020-11-12 | キヤノン株式会社 | Manufacturing method of optical element, optical element, imaging device, and optical apparatus |
| CN112531124A (en) * | 2019-09-19 | 2021-03-19 | 北京小米移动软件有限公司 | Display screen and terminal |
| CN115806775A (en) * | 2022-11-16 | 2023-03-17 | 武汉光鹿科技发展有限公司 | Colored protective film for lens and preparation method thereof |
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| JP6770576B2 (en) | 2020-10-14 |
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