WO2011065429A1 - モスアイ用型、ならびに、モスアイ用型およびモスアイ構造の作製方法 - Google Patents
モスアイ用型、ならびに、モスアイ用型およびモスアイ構造の作製方法 Download PDFInfo
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- WO2011065429A1 WO2011065429A1 PCT/JP2010/071030 JP2010071030W WO2011065429A1 WO 2011065429 A1 WO2011065429 A1 WO 2011065429A1 JP 2010071030 W JP2010071030 W JP 2010071030W WO 2011065429 A1 WO2011065429 A1 WO 2011065429A1
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- moth
- mold
- antireflection
- eye
- depth
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/42—Moulds or cores; Details thereof or accessories therefor characterised by the shape of the moulding surface, e.g. ribs or grooves
- B29C33/424—Moulding surfaces provided with means for marking or patterning
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/045—Anodisation of aluminium or alloys based thereon for forming AAO templates
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/18—After-treatment, e.g. pore-sealing
- C25D11/24—Chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
- C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24355—Continuous and nonuniform or irregular surface on layer or component [e.g., roofing, etc.]
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24479—Structurally defined web or sheet [e.g., overall dimension, etc.] including variation in thickness
Definitions
- the present invention relates to a moth-eye mold and a method for producing a moth-eye mold and a moth-eye structure.
- Non-Patent Document 1 and Patent Documents 1 to 4 When light is reflected at an interface having a different refractive index (for example, an interface between air and glass), the transmitted light intensity may be reduced and visibility may be lowered. In order to prevent such reflection of light, use of an antireflection film having a moth-eye structure has been studied (see Non-Patent Document 1 and Patent Documents 1 to 4).
- the two-dimensional size of the convex portion is 10 nm or more and less than 500 nm.
- the incident angle dependence of the antireflection effect by such a moth-eye structure is small over a wide wavelength range.
- the moth-eye structure can be realized with various materials and can be directly formed on the substrate, so that it can be manufactured at low cost.
- the moth-eye structure can be produced by a laser interference exposure method, an EB exposure method, or the like, but if anodization of aluminum is used, a large-area moth-eye structure can be produced inexpensively and easily. Specifically, the manufacturing cost can be greatly reduced by utilizing a porous alumina layer obtained by anodizing aluminum as at least a part of a mold having a moth-eye structure. For this reason, it has been noted that a moth-eye structure is produced using anodization (Patent Documents 2 to 4).
- the “mold” here includes molds used in various processing methods (stamping and casting) and is also called a stamper. It can also be used for printing (including nanoprinting).
- a mold for producing a moth-eye structure is also referred to as a “moth-eye mold”.
- Patent Document 2 discloses a mold having a porous alumina layer produced by anodic oxidation on its surface.
- a nano-order cylindrical depression formed in the porous alumina layer by anodic oxidation extends in a direction perpendicular to the surface of the porous alumina layer, and is also called a pore.
- the porous alumina layer formed under specific conditions has an array in which almost regular hexagonal cells are two-dimensionally filled with the highest density when viewed from the normal direction of the surface. Each cell has a pore in the center, and the arrangement of the pores has periodicity. Further, in the porous alumina layer formed under different conditions, an array with irregularity to some extent or an irregular arrangement (that is, having no periodicity) is formed.
- Patent Document 3 discloses a mold in which tapered pores in which the pore diameter continuously changes along the depth direction are formed by repeating anodization of aluminum and a pore diameter expansion process by etching. Yes. Further, Patent Document 4 discloses a stamper (mold) that is manufactured by repeating anodization of aluminum and a hole diameter expansion process until adjacent holes are partially connected.
- FIG. 18A shows a schematic perspective view of the stamper 700 disclosed in Patent Document 4, and FIG. 18B shows a schematic plan view of the stamper 700.
- On the surface of the stamper 700 six protrusions are provided around each of the plurality of holes, and the adjacent protrusions are connected by a ridge line through the flange.
- the antireflection material manufactured using such a stamper 700 since the continuity of the effective refractive index at the interface between the antireflection material and the incident medium (typically air) increases, high antireflection performance. Is realized.
- the present invention has been made in view of the above problems, and its object is to provide a moth-eye mold used for the production of an antireflection material that sufficiently suppresses reflection of light, and a moth-eye mold and a method for producing a moth-eye structure. Is to provide.
- a mold according to the present invention is a mold having a surface having an inverted shape of the surface shape of a moth-eye structure, and a plurality of projections and a plurality of projections each connecting the plurality of projections via a flange on the surface. And a plurality of holes each defined by an arbitrary at least three protrusions of the plurality of protrusions and a ridgeline connecting the at least three protrusions, and the adjacent holes
- the average distance p between the centers and the average depth r of the collar portion satisfy the relationship of 0.15 ⁇ r / p ⁇ 0.60.
- the average distance p is not less than 180 nm and not more than 420 nm.
- the average depth q of the plurality of holes is 380 nm or more and 410 nm or less.
- the surface is a surface of a porous alumina layer.
- a mold manufacturing method is a mold manufacturing method having a surface having a surface shape inverted from the surface shape of a moth-eye structure, comprising a step of preparing a base material provided with aluminum on the surface, and anodizing the aluminum And performing etching, a plurality of protrusions, a plurality of ridge lines each connecting the plurality of protrusions via a flange, and each of the at least three protrusions of the plurality of protrusions and the Forming a porous alumina layer having a surface provided with a plurality of holes defined by ridge lines connecting at least three protrusions, and in the step of forming the porous alumina layer, adjacent holes
- the average distance p between the centers and the average depth r of the heel satisfy the relationship of 0.15 ⁇ r / p ⁇ 0.60.
- the average distance p is not less than 180 nm and not more than 420 nm.
- an average depth q of the plurality of holes is 380 nm or more and 410 nm or less.
- the method for producing a moth-eye structure according to the present invention includes a step of producing a mold by the production method described above, and curing the photocurable resin by irradiating light while the mold is in contact with the photocurable resin. Process.
- an antireflection material that sufficiently suppresses reflection of light can be suitably produced.
- (A) is a bird's-eye view SEM image of the embodiment of the mold according to the present invention
- (b) is a schematic cross-sectional view of the mold shown in (a).
- (A) is a planar SEM image of the mold of this embodiment
- (b) is a cross-sectional SEM image of the mold shown in (a)
- (c) is a bird's-eye SEM image of the mold shown in (a). is there.
- (A) And (b) is a schematic diagram which shows embodiment of the manufacturing method of the type
- (A)-(e) is a schematic diagram which shows the formation method of the porous alumina layer in the moth-eye type
- FIG. 1 It is a schematic diagram which shows embodiment of the manufacturing method of the reflection preventing material by this invention.
- A) is a typical top view of the type
- (b) is typical sectional drawing of the type
- (c) is antireflection of the comparative example 1. It is typical sectional drawing of material
- (d) is a graph which shows the change of the effective refractive index in the interface of the antireflection material of (c), and air.
- (A) is a typical top view of the type
- (b) is typical sectional drawing of the type
- (c) is the antireflection material of this embodiment.
- (d) is a graph which shows the change of the effective refractive index in the interface of the antireflection material of (c), and air.
- (A) is typical sectional drawing of the type
- (b) is typical sectional drawing of the antireflection material of the comparative example 2 produced using the type
- (C) is a schematic cross-sectional view of a moth-eye mold of Comparative Example 3
- (d) is a schematic diagram of an antireflection material of Comparative Example 3 produced using the mold shown in (c).
- FIG. (E) is a schematic cross-sectional view of the moth-eye mold of the present embodiment, and (f) is the antireflection material of the present embodiment manufactured using the mold shown in (e).
- FIG. (A) to (e) are cross-sectional SEM images of molds a to e.
- (A) to (e) are bird's-eye SEM images taken from a direction inclined 45 degrees with respect to the normal direction of the entire surface of the molds a to e.
- (A) to (e) are cross-sectional SEM images of the antireflection materials A to E.
- (A)-(c) is a schematic diagram which shows the measuring method of the cross-sectional SEM image of antireflection material AE.
- FIG. 5 is a graph showing reflection spectra of antireflection materials A to E.
- (A) to (h) are cross-sectional SEM images of molds f to m.
- (A) to (h) are bird's-eye SEM images taken from a direction inclined by 45 degrees with respect to the normal direction of the entire surface of the molds f to m.
- (A) to (h) are cross-sectional SEM images of the antireflection materials F to M.
- A) is a graph showing the reflection spectra of the antireflection materials F to I
- (b) is a graph showing the reflection spectra of the antireflection materials J to M.
- (A) And (b) is a schematic diagram of a conventional moth-eye mold (stamper).
- FIG. 1A shows a bird's-eye SEM image of the moth-eye mold 100
- FIG. 1B shows a schematic cross-sectional view of the moth-eye mold 100.
- the SEM image is captured with a scanning electron microscope (SEM).
- SEM scanning electron microscope
- the bird's-eye view SEM image is an image taken from a direction inclined with respect to the normal direction of the entire surface of the moth-eye mold 100.
- the moth-eye mold 100 has a surface in which the surface shape of the moth-eye structure is inverted, and is used for the production of an antireflection material having a moth-eye structure.
- a plurality of protrusions On the surface of the moth-eye mold 100, a plurality of protrusions, a plurality of ridge lines each connecting the plurality of protrusions via the collar, and each of at least three of the plurality of protrusions and an arbitrary And a plurality of holes defined by ridge lines connecting at least three protrusions.
- each protrusion is pointed and each hole is tapered.
- Each protrusion is provided at a position surrounded by at least three holes.
- FIG. 1 (b) shows the distance p between the centers of adjacent holes in the moth-eye mold 100, the depth q of the hole, and the depth r of the buttock.
- adjacent holes are provided so as to be partially connected, and the average distance between the centers of the adjacent holes is substantially equal to the average value of the hole diameters. Strictly speaking, the distance between the centers of adjacent holes is not constant, but the difference in the distance between the centers of any two adjacent holes is relatively small. In the following description of this specification, this average distance may be simply referred to as “adjacent distance”.
- the measuring method of the average distance p between the centers of the adjacent holes in the moth-eye mold 100, the average depth q of the holes, and the average depth r of the buttocks will be described.
- FIG. 2 (a) shows a planar SEM image of the moth-eye mold 100.
- FIG. An average distance p between the centers of adjacent holes in the planar SEM image is obtained.
- the average distance p for example, three holes having a short distance between centers with respect to a certain hole are selected, and these distances are measured.
- the average distance p is obtained by measuring the distance between the centers adjacent to each hole and calculating the average value.
- the average distance p is, for example, not less than 180 nm and not more than 420 nm.
- a value obtained by dividing the standard deviation of the distance p by the average value is about 30%.
- the ridge line extends in a direction connecting the vertices of two adjacent protrusions with the shortest distance as seen from the normal direction of the entire surface. For example, when looking at the cross section of the collar along a certain direction, the surface has a convex shape upward, and when looking at the cross section of the collar along another direction, the surface has a convex shape downward. Further, typically, the projecting portion is connected to the other three projecting portions by a ridge line through the collar portion.
- 3 to 6 protrusions are provided around one hole. Further, the protrusion is provided at a position surrounded by 3 or more and 6 or less holes. Specifically, when attention is paid to any one protrusion, the protrusion is changed from the protrusion to the protrusion.
- the centers of 3 or more and 6 or less holes are located within the range up to the distance between the apex and the apex of the projecting part closest to the apex of the projecting part.
- FIG. 2B shows a cross-sectional SEM image of the moth-eye mold 100.
- the average depth q of the holes is, for example, not less than 380 nm and not more than 410 nm.
- the value obtained by dividing the standard deviation of the depth q by the average value is about 5%.
- FIG. 2C shows a bird's-eye view SEM image of the moth-eye mold 100.
- This bird's-eye view SEM image is an image taken from a direction inclined 45 degrees with respect to the normal direction of the entire surface of the moth-eye mold 100.
- a distance s between a virtual straight line connecting the vertices of the two protrusions connected by the ridge line and the heel part is obtained, and the distance s is measured for each heel part to obtain an average value thereof.
- the average depth r of the buttock is obtained by calculating the product of this average value and ⁇ 2. Needless to say, the average depth r of the holes is smaller than the average depth q of the flange.
- the average distance p between the centers of adjacent holes may be simply referred to as the average distance p.
- the average depth q of the holes in the mold may be simply referred to as the depth q, and similarly, the average depth r of the collar portion may be simply referred to as the depth r.
- a value obtained by dividing the standard deviation of the depth r by the average value is about 30%.
- the moth-eye mold 100 is used for producing an antireflection material.
- the antireflection material provided with the moth-eye structure is produced by transferring the surface shape of the moth-eye mold 100 to a resin.
- a plurality of convex portions are provided on the surface of the antireflection material, and the convex portions of the antireflection material are formed corresponding to the holes of the mold 100.
- the distance between the vertices of two adjacent convex portions is not constant, but the distance between the vertices of any two adjacent convex portions is approximately equal. This distance is, for example, not less than 180 nm and not more than 420 nm.
- the average distance between the centers of any adjacent convex portions in the antireflection material is simply referred to as “adjacent distance”. is there.
- the shorter the adjacent distance between the protrusions in the antireflection material the greater the wavelength dependency of the light reflectance, and the color of the emitted light is more likely to change compared to the incident light. Even if this light is incident, the reflected light may be tinted.
- the press pressure when producing the antireflection material by the transfer method can be reduced and the releasability can be improved. Can be improved.
- the ratio r / p of the average distance p between the centers of adjacent holes and the average depth r of the heel satisfies the relationship of 0.15 ⁇ r / p ⁇ 0.60. ing.
- the ratio r / p reflects the shape of the protrusion in the moth-eye mold 100. As the ratio r / p is larger, that is, as p is constant and r is larger, or as r is constant and p is smaller, the protrusion becomes sharper. Although details will be described later, when the ratio r / p satisfies the above relationship, the antireflection material produced using the moth-eye mold 100 can sufficiently suppress the reflection of light.
- Such a moth-eye mold 100 is manufactured as follows. Hereinafter, with reference to FIG. 3, a method for manufacturing the moth-eye mold 100 will be described.
- a base material 100t having a surface formed of aluminum 100a is prepared.
- a base material 100t is produced, for example, by depositing an aluminum film 100a on an insulating substrate (typically a glass substrate) 100s.
- the thickness of the aluminum film 100a is, for example, 1.0 ⁇ m. Note that bulk aluminum may be used as the substrate 100t.
- a part of the aluminum film 100a of the substrate 100t is changed into a porous alumina layer 100c by performing anodic oxidation and etching.
- the average distance p between the centers of adjacent holes and the average depth r of the flange portion satisfy the relationship of 0.15 ⁇ r / p ⁇ 0.60.
- the moth-eye mold 100 is manufactured.
- a base material 100t having a surface provided with an aluminum film 100a is prepared.
- a porous alumina layer 100b having pores 100p extending in a direction perpendicular to the surface of the substrate 100t is formed by anodizing the substrate 100t. To do.
- the oxidation and dissolution of the aluminum film 100a proceed simultaneously on the surface of the substrate 100t, and the pores 100p extending in the direction perpendicular to the surface of the substrate 100t are formed.
- anodic oxidation is performed by immersing the base material in an acidic electrolytic solution or alkaline electrolytic solution such as sulfuric acid, oxalic acid, or phosphoric acid, and applying a voltage using this as an anode.
- an acidic electrolytic solution or alkaline electrolytic solution such as sulfuric acid, oxalic acid, or phosphoric acid
- the average distance between the centers of adjacent pores and the depth of the pores change according to the conditions of the anodic oxidation.
- the average distance between the centers of adjacent pores corresponds to approximately twice the thickness of the barrier layer and is approximately proportional to the voltage during anodization.
- the average distance between the centers of the pores is, for example, in the range of 180 nm to 420 nm.
- the pore diameter depends on the type, concentration, temperature, etc. of the electrolytic solution.
- the pores are preferably arranged with regularity that is somewhat disturbed. However, the pores may be arranged irregularly (that is, having no periodicity) or may be
- anodic oxidation is performed for 25 seconds at an conversion voltage of 80 V using 0.6 wt% oxalic acid at a liquid temperature of 5 ° C. as an electrolyte.
- anodic oxidation is performed at a conversion voltage of 200 V for 30 seconds to 45 seconds using 2 wt% tartaric acid at a liquid temperature of 5 ° C. as an electrolyte.
- the hole diameter of the pores 100p is enlarged by performing etching. Etching is performed for several tens of minutes using 1 mol / L of phosphoric acid having a liquid temperature of 30 ° C.
- the aluminum 100a is partially anodized again to grow the pores 100p in the depth direction and to thicken the porous alumina layer 100b.
- the growth of the pore 100p starts from the bottom of the already formed pore 100p, the side surface of the pore 100p is stepped.
- the porous alumina layer 100b is further etched to further expand the pore diameter of the pores 100p. Etching is performed in the same manner as the etching described above. In this way, the porous alumina layer 100c shown in FIG. 3B is formed.
- Anodization and etching are repeated several times until adjacent holes are partially connected.
- the last is preferably anodic oxidation rather than etching. Thereby, the bottom of the hole can be made relatively narrow.
- a moth-eye mold 100 and a workpiece 150 are prepared.
- the photocurable resin is cured by irradiating light (for example, ultraviolet light) in a state where the photocurable resin is sandwiched between the moth-eye mold 100 and the workpiece 150, and the antireflection material 200 is cured.
- the workpiece 150 is, for example, a flexible polymer film.
- the polymer film is, for example, a TAC (triacetyl cellulose) film.
- an acrylic resin is used as the photocurable resin, the viscosity thereof is 500 ⁇ 200 cP, and the shrinkage rate at the time of curing is about 10%.
- the transfer is performed at a pressure of 20 kg / cm 2 or less.
- the pressure may be 20 kg / cm 2 or 10 kg / cm 2 .
- the transfer may be performed manually or at a pressure of 1 kg / cm 2 or less.
- a photocurable resin is applied between the moth-eye mold 100 and the workpiece 150.
- the photocurable resin may be applied to the surface of the workpiece 150 or may be applied to the surface of the moth-eye mold 100.
- a photocurable resin may be dropped on the moth-eye mold 100, and then a TAC film may be bonded with a roller so that bubbles do not enter the resin.
- the photocurable resin is cured by irradiating the photocurable resin with light (for example, ultraviolet light) through the moth-eye mold 100.
- light irradiation is performed using i-line (365 nm).
- the irradiation energy is 100 mJ / cm 2 or more and 3 J / cm 2 or less, for example, 2 J / cm 2 .
- the height of the convex portion in the antireflection material is smaller than the depth of the hole of the moth-eye mold.
- the depth of the flange portion of the mold when the depth of the flange portion of the mold is relatively small, the height of the convex portion in the antireflection material becomes substantially constant according to the depth of the hole of the mold, but the depth of the flange portion of the mold.
- the resin constituting the antireflection material stays in the portion corresponding to the collar portion of the mold, and the height of the convex portion is lowered.
- a cured resin hardly absorbs light, and specifically has a relative transmittance of 90% or more with respect to air with visible light (wavelength 380 to 780 nm).
- the cured resin preferably has high reliability. For example, even if left for a long time (for example, 500 hours) at a high temperature (for example, 95 ° C.) or a low temperature (for example, ⁇ 40 ° C.), the surface does not change at least visually at room temperature. Further, even after a rapid temperature change (for example, ⁇ 40 ° C. for 30 minutes to 85 ° C. for 30 minutes) is repeated a plurality of times (for example, 100 times), at least the surface is not visually observed. Furthermore, even when left for a long time (for example, 100 hours) under high temperature and high humidity (for example, temperature 60 ° C., humidity 95%), the surface does not change at least visually. Moreover, the pencil hardness of such resin is 1H or more.
- the moth-eye mold 100 is separated from the antireflection material 200.
- the antireflection material 200 provided with the moth-eye structure can be produced.
- a plurality of convex portions are provided on the surface of the antireflection material 200.
- the convex portions have a substantially conical shape.
- the refractive index of the antireflection material 200 is, for example, 1.5.
- the adjacent holes are partially connected, and the adjacent protrusions are connected by a ridge line via the flange. Since the antireflection material 200 manufactured using such a moth-eye mold 100 does not have a flat surface between the convex portions, the refractive index of light incident on the antireflection material 200 changes continuously. , Reflection is suppressed.
- FIG. 6A shows a schematic plan view of the moth-eye mold 500
- FIG. 6B shows a schematic cross-sectional view of the mold 500.
- the surface of the moth-eye mold 500 is not provided with a flange, and the surface of the mold 500 is provided with a flat surface surrounded by three holes.
- FIG. 6C is a schematic cross-sectional view of the antireflection material 600 manufactured using the moth-eye mold 500.
- the surface of the antireflection material 600 is formed corresponding to the surface of the moth-eye mold 500.
- the shape of the convex portion of the antireflection material 600 is shown to match the shape defined by the hole of the moth-eye mold 500.
- the surface of the moth-eye mold 500 is provided with a flat surface surrounded by three holes, and the projections are also formed on the surface of the antireflection material 600. Between the two, a flat surface is provided. In this case, as shown in FIG. 6D, the effective refractive index changes abruptly on a flat surface, and light reflection cannot be sufficiently suppressed.
- FIG. 7A shows a schematic plan view of the moth-eye mold 100
- FIG. 7B shows a schematic cross-sectional view of the moth-eye mold 100.
- a protrusion surrounded by at least three holes is provided, and a ridge line connecting adjacent protrusions is provided.
- FIG. 7C shows a schematic cross-sectional view of the antireflection material 200 manufactured using the moth-eye mold 100.
- the surface of the antireflection material 200 is formed corresponding to the surface of the moth-eye mold 100.
- the shape of the convex portion of the antireflection material 200 is shown to match the shape defined by the hole of the moth-eye mold 100.
- a flat surface is not formed between the convex portions on the surface of the antireflection material 200.
- the effective refractive index changes gently along the height direction of the convex portion, and as a result, reflection of light is sufficiently suppressed.
- the shape of the convex portion of the antireflection material coincided with the shape defined by the hole of the mold.
- the shape of the protrusion of the prevention material does not match the shape defined by the mold hole. For this reason, an antireflection material that sufficiently suppresses reflection cannot be realized only by using a mold having a flange portion on the surface.
- FIG. 8A shows a schematic cross-sectional view of the moth-eye mold 300A of Comparative Example 2.
- the moth-eye mold 300A is provided with a flange, but the depth r of the flange with respect to the average distance p between the centers of adjacent holes is relatively small, and the slope of the protrusion is relatively gentle.
- the average distance p and the depth r of the heel satisfy the relationship r / p ⁇ 0.15.
- FIG. 8B shows an antireflection material 400A of Comparative Example 2.
- the antireflection material 400A is manufactured using a moth-eye mold 300A. As described above, since the slope of the protrusion in the moth-eye mold 300A is relatively gentle, a substantially flat surface is formed between the protrusions in the antireflection material 400A. As a result, the effective refractive index is increased. Changes rapidly in the vicinity of the bottom surface of the antireflection material 400A, as shown in FIG. For this reason, the antireflection material 400A cannot sufficiently prevent reflection of light.
- the inclination of the convex portion is substantially constant from the apex of the convex portion toward the bottom surface.
- the rate of change of the effective refractive index increases from the top of the convex portion toward the bottom surface.
- the rate of change of the effective refractive index is relatively large, reflection cannot be sufficiently prevented.
- the color of the reflected light of the antireflection material 400A changes compared to the incident light.
- FIG. 8 (c) shows a schematic cross-sectional view of the moth-eye mold 300B of Comparative Example 3.
- the moth-eye mold 300B is provided with a flange, but the depth r of the flange with respect to the average distance p between the centers of adjacent holes is relatively large, and the slope of the protrusion is relatively steep.
- the average distance p and the depth r of the heel satisfy the relationship of 0.60 ⁇ r / p.
- FIG. 8D shows the antireflection material 400B of Comparative Example 3.
- the antireflection material 400B is manufactured using the moth-eye mold 300B. As described above, since the slope of the protrusion in the moth-eye mold 300B is relatively steep, the distance between the protrusions in the antireflection material 400B is relatively high. For this reason, even if the depths of the holes of the moth-eye molds 300A and 300B are substantially equal, the convex portion in the antireflection material 400B is lower than the convex portion in the antireflection material 400A, and the aspect ratio of the convex portion is reduced. For this reason, the antireflection material 400B cannot sufficiently prevent reflection of light.
- the half width of the convex portion is considerably larger than half of the distance between the centers of the convex portions, and the slope of the convex portion is gentle from the apex of the convex portion toward the bottom surface, and the rate of the change Is relatively large.
- the rate of change of the effective refractive index decreases as it goes from the apex of the convex portion to the bottom surface.
- FIG. 8E shows a schematic cross-sectional view of the moth-eye mold 100 of the present embodiment.
- the average distance p between the centers of adjacent holes and the depth r of the flange portion satisfy the relationship of 0.15 ⁇ r / p ⁇ 0.60.
- FIG. 8 (f) shows the antireflection material 200 of the present embodiment.
- the antireflection material 200 is manufactured using the moth-eye mold 100.
- the convex portion in the antireflection material 200 has substantially the same height as the convex portion in the antireflection material 400A of Comparative Example 2, and in the antireflection material 200, while maintaining the aspect ratio of the convex portion high, A convex part can be made into a bell shape.
- the average distance p between the centers of the adjacent holes and the depth r of the flange satisfy the relationship of 0.15 ⁇ r / p ⁇ 0.60.
- reflection of light can be sufficiently prevented.
- Mold a is produced as follows. First, a 5 cm square glass substrate is prepared, and a base material is formed by depositing an aluminum film having a thickness of 1.0 ⁇ m on the glass substrate.
- a porous alumina layer having pores is formed by anodizing the base material.
- anodic oxidation is performed for 25 seconds at an formation voltage of 80 V using oxalic acid of 0.6 wt% at a liquid temperature of 5 ° C., thereby forming pores having an adjacent distance p of 180 nm.
- etching is performed for 19 minutes using 1 mol / L of phosphoric acid at a liquid temperature of 30 ° C. This etching enlarges the pore diameter.
- Anodization and etching are repeated until adjacent holes are partially connected. Specifically, the anodic oxidation is repeated 5 times and the etching process is alternately repeated 4 times. In this way, the mold a is produced. In the mold a, the adjacent distance p of the holes is approximately 180 nm, and the average depth q of the holes is approximately 380 nm.
- the molds b to e are manufactured in the same manner as the mold a except that the etching times are different.
- the etching times for molds b to e are 21 minutes, 23 minutes, 25 minutes and 30 minutes, respectively.
- FIGS. 9A to 9E show cross-sectional SEM images of the molds a to e, respectively, and FIGS. 10A to 10E show the normal direction of the entire surface of the molds a to e.
- a bird's-eye view SEM image captured from a direction inclined by 45 degrees is shown.
- Table 1 shows the etching time for producing the molds a to e, the adjacent distance p of the molds a to e, the depth q of the hole, and the depth r of the flange.
- the distance to the center of three holes having a short distance from the center of each hole in the planar SEM images of the molds a to e is measured, and the average is the adjacent distance p. Further, the depth q of the hole is obtained from the cross-sectional SEM image. Furthermore, the depth r of the buttock is measured by measuring the distance between the imaginary line segment connecting the vertices of two protrusions formed around a hole in the bird's eye SEM image inclined at 45 degrees and the buttock at 20 points.
- the bird's-eye view SEM image is obtained from the product of the average value and ⁇ 2 in consideration that the bird's-eye view SEM image is an image taken from a direction inclined 45 degrees with respect to the normal direction of the mold surface. .
- the adjacent distance p of the holes is about 180 nm, and the depth of the holes is about 380 nm.
- the depth r of the flange portion is different. The longer the etching time, the larger the depth r of the flange portion.
- the antireflection materials A to E are produced using the molds a to e.
- the antireflection materials A to E are produced by transferring the surface shapes of the molds a to e to the curable resin as described above, and the antireflection materials A to E are formed in correspondence with the holes of the molds a to e. A convex part is formed.
- 11A to 11E show cross-sectional SEM images of the antireflection materials A to E, respectively. Convex portions of the antireflection materials A to E are formed corresponding to the holes of the molds a to e.
- the structure of the antireflection material is measured as follows. Hereinafter, a method for measuring the antireflection material will be described with reference to FIG.
- an antireflection material 200 formed on the workpiece 150 is prepared.
- the workpiece 150 and the antireflection material 200 are divided by bending to expose the cross section of the antireflection material 200. Thereafter, gold is deposited on the cross section of the antireflection material 200.
- the cross section of the antireflection material 200 is imaged with an SEM. While measuring the height of several convex parts in a cross-sectional SEM image and calculating
- the average height T of the protrusions in the antireflection material may be simply referred to as depth T, and similarly, the average half width HW of the protrusions may be simply referred to as half width HW.
- Table 2 shows the height T and the half width HW of the convex portions of the antireflection materials A to E.
- the adjacent distance p of the convex portions in the antireflection materials A to E is substantially equal to the adjacent distance of the holes in the molds a to e, and is approximately 180 nm.
- the height T and the half width HW of the convex portions in the antireflection materials A to E are different.
- the height T of the convex portion is substantially equal.
- the adjacent distance p between the convex portions is approximately 180 nm, the aspect ratios of the convex portions in the antireflection materials A to C are substantially equal.
- the height T of the convex portion in the antireflection material D is smaller than the height T of the convex portion in the antireflection materials A to C, and the height T of the convex portion in the antireflection material E is the height of the convex portion in the antireflection material D. Even smaller than T.
- the half-value widths HW of the antireflection materials A to E are different. As described above, the adjacent distance p between the convex portions of the antireflection materials A to E is approximately 180 nm. The half width HW of the convex portion in the antireflection material A is 90 nm, and the convex portion of the antireflection material A has a substantially conical shape. On the other hand, the half width HW of the convex portions of the antireflection materials B to E is larger than 90 nm, the convex portion has a bell shape, and the convex portions are in order of the antireflection materials B, C, D, and E. Becomes a crushed shape.
- each antireflection material A is obtained from the transmittance characteristics of the standard light D 65 with respect to the XYZ color system weight coefficient.
- the object colors of ⁇ E are defined, and then the Y value, L * value, a * , b *, and saturation C * of the reflected light from the antireflection materials A to E are measured.
- FIG. 13 shows the reflection spectra of the antireflection materials A to E.
- the reflection spectrum of the antireflection material A has a relatively high reflectance in the long wavelength region, and the reflectance greatly depends on the wavelength. Further, in the reflection spectrum of the antireflection material E, the wavelength dependency of the reflectance is relatively low, and the reflectance itself is relatively high. On the other hand, in the reflection spectra of the antireflection materials B to D, the reflectance is relatively low and the wavelength dependency is relatively small.
- Table 3 shows the height T and half-value width HW of the convex portions of the antireflection materials A to E, and the Y value, L * value, a * , b *, and C * of the reflected light of the antireflection materials A to E. Show.
- the reflected light intensity of the antireflection materials A and E is higher than that of the antireflection materials B to D.
- the half width HW of the convex portion is small, and the convex portion has a substantially conical shape. For this reason, the rate of change of the effective refractive index along the height direction of the convex portion changes relatively large. As a result, the antireflection material A cannot sufficiently prevent reflection.
- the antireflection material E since the height T of the convex portion with respect to the adjacent distance p of the convex portion is small, the aspect ratio of the convex portion is small. Moreover, the half width HW of the convex part in the antireflection material E is relatively large, and the rate of change of the effective refractive index along the height direction of the convex part changes relatively large. For this reason, the antireflection material E cannot sufficiently prevent reflection.
- Table 4 shows the etching time for manufacturing the molds a to e, the adjacent distance p of the holes in the molds a to e, the depth q of the holes, the depths r, r / p, r / q of the buttock, the molds a to The height T, the half width HW, the Y value, L * value, a * , b * , C * of the reflected light of the antireflection materials A to E in the antireflection materials A to E produced using e Indicates.
- the height T of the convex portions in the antireflection materials A to E is smaller than the depth q of the holes of the moth-eye molds a to e.
- the height T of the convex portion in the antireflection materials A to C is substantially constant, but in the moth-eye molds d and e, the depth of the ridge Since the length r is relatively large, the resin constituting the antireflection materials D and E stays at the portions corresponding to the ridges of the molds d and e during transfer, and the height T of the convex portion decreases.
- the half width HW of the convex portions in the antireflection materials A to E increases.
- the depth r of the ridge is small, so that the half width HW of the convex portion in the antireflection material A is short.
- the convex portion of the antireflection material A has a substantially conical shape, and the rate of change of the effective refractive index along the height direction of the convex portion changes relatively greatly. As a result, the antireflection material A is Reflection cannot be prevented sufficiently.
- the height T of the convex portions in the antireflection materials D and E is lower than that of the antireflection materials A to C, and in particular, the antireflection material corresponding to the mold e having a large depth r of the collar portion.
- the height T of the convex portion at E is small.
- the height T of the convex portion with respect to the adjacent distance p of the convex portion is small, and the half width HW is large, and therefore the antireflection material E cannot sufficiently prevent reflection.
- the adjacent distance p of the convex portion in the antireflection material is relatively short, the Y value is relatively low, but the reflected light is likely to be colored.
- the adjacent distance p of the hole and the depth r of the flange portion in the moth-eye mold satisfy the relationship of 0.15 ⁇ r / p ⁇ 0.60, the adjacent distance p of the convex portion is approximately 180 nm. It is possible to suppress the Y value of the antireflective material to 0.27 or less and to suppress the saturation C * of reflected light to 5.0 or less.
- the adjacent distance p between the hole in the mold and the convex portion in the antireflection material is about 180 nm, but the adjacent distance is not limited to this.
- the molds f to m having the adjacent distance p of about 400 nm and the antireflection materials F to M manufactured using the molds f to m will be described.
- the mold f is manufactured as follows. First, a 5 cm square glass substrate is prepared, and a base material is formed by depositing an aluminum film having a thickness of 1.0 ⁇ m on the glass substrate.
- a porous alumina layer having pores is formed by anodizing the base material.
- anodization is performed for 30 seconds at a chemical conversion voltage of 200 V using 2 wt% of tartaric acid at a liquid temperature of 5 ° C. to form pores having an adjacent distance p of about 400 nm.
- etching is performed for 100 minutes using 1 mol / L of phosphoric acid at a liquid temperature of 30 ° C. Etching increases the pore diameter.
- Anodization and etching are repeated until adjacent holes are partially connected. Specifically, anodization is repeated 5 times and etching is alternately repeated 4 times.
- the molds g to i are manufactured in the same manner as the mold f except that the etching times are different.
- the etching times are 110 minutes, 120 minutes and 150 minutes, respectively.
- the types j to m are manufactured in the same manner as the types f to i except that the anodic oxidation times are different.
- the time for anodizing in each of the types j to m is 45 minutes.
- FIGS. 14 (a) to 14 (h) show cross-sectional SEM images of the molds f to m, respectively, and FIGS. 15 (a) to 15 (h) show bird's-eye view SEM images of the molds f to m inclined at 45 degrees. Respectively.
- Table 5 shows the anodic oxidation time and etching time when the molds f to m are manufactured, and the adjacent distance p of the holes of the molds f to m, the depth q of the hole, and the depth r of the flange portion.
- the distance to the center of three holes having a short distance from the center of each hole in the planar SEM images of the molds f to m is measured, and the average is the adjacent distance p. Further, the depth q of the hole is obtained from the cross-sectional SEM image. Furthermore, the depth r of the buttock is measured by measuring the distance between the imaginary line segment connecting the vertices of two protrusions formed around a hole in the bird's eye SEM image inclined at 45 degrees and the buttock at 20 points.
- the bird's-eye view SEM image is obtained from the product of the average value and ⁇ 2 in consideration of the fact that the bird's-eye view SEM image is an image taken from a direction inclined 45 degrees with respect to the normal direction of the entire mold surface. It is done.
- the depth r of the buttock is different. The longer the etching time, the larger the depth r of the buttock.
- the hole depth q is approximately 380 nm
- the hole depth q is approximately 400 nm.
- the hole depth q varies depending on the anodic oxidation time per one time. In any of the types f to m, the adjacent distance p is approximately 400 nm.
- the antireflection materials F to M are manufactured using such molds f to m.
- the antireflection materials F to M are manufactured by transferring the surface shapes of the molds f to m to the curable resin as described above, and the antireflection materials F to M are formed corresponding to the holes of the molds f to m. A convex part is formed.
- FIGS. 16A to 16H show cross-sectional SEM images of the antireflection materials F to M, respectively. The sizes of the antireflection materials F to M are measured as described above with reference to FIG.
- Table 6 shows the height T and the half width HW of the convex portions of the antireflection materials F to M.
- the adjacent distance p between the convex portions in the antireflection materials F to M is also approximately 400 nm.
- the heights T of the convex portions in the antireflection materials F and G are substantially equal. As described above, since the adjacent distance p between the convex portions is approximately 400 nm, the aspect ratios of the convex portions in the antireflection materials F and G are substantially equal. On the other hand, the height T of the convex portion of the antireflection material H is smaller than that of the antireflection materials F and G, and the height T of the convex portion of the antireflection material I is smaller than that of the antireflection material H.
- the half-value widths HW of the antireflection materials F to I are different. As described above, the adjacent distance p between the convex portions of the antireflection materials F to I is approximately 400 nm. The half width HW of the convex portions in the antireflection materials F to I is larger than 200 nm, which is half of the adjacent distance p, and the convex portions have a bell shape.
- the heights T of the convex portions in the antireflection materials J to L are substantially equal. As described above, since the adjacent distance p between the convex portions is approximately 400 nm, the aspect ratios of the convex portions in the antireflection materials J to L are substantially equal. In contrast, the height T of the convex portion of the antireflection material M is smaller than that of the antireflection materials J to L.
- the half width HW of the antireflection materials J to M is different.
- the adjacent distance p between the convex portions of the antireflection materials J to M is approximately 400 nm.
- the half width HW of the convex portions in the antireflection materials J to M is larger than 200 nm, which is half of the adjacent distance p, and the convex portions have a bell shape.
- the reflection characteristics of the antireflection materials F to M are measured.
- the reflection characteristics are measured in a state where antireflection materials F to M are pasted on a black acrylic plate.
- the Y value, L * value, a * , b * and C * of the reflected light from the antireflection materials F to M are measured.
- FIG. 17A shows the reflection spectra of the antireflection materials F to I.
- the reflectance of the antireflection material I is higher than that of other antireflection materials over a wavelength range of 450 nm to 700 nm, and the average reflectance of the antireflection material I is higher than the average reflectances of the antireflection materials F to H.
- FIG. 17B shows the reflection spectra of the antireflection materials J to M.
- the reflectance of the antireflection material M is higher than that of the antireflection materials J to L over the visible light region.
- Table 7 shows the height T and half-value width HW of the convex portions of the antireflection materials F to M, and the Y value, L * value, a * , b *, and C * of the reflected light of the antireflection materials F to M. Show.
- the reflected light intensity of the antireflection materials I and M is higher than that of the antireflection materials F to H and J to L.
- the height T of the convex portion with respect to the adjacent distance p of the convex portion is small, and the aspect ratio of the convex portion is small. For this reason, the antireflection materials I and M cannot sufficiently prevent reflection.
- Table 8 shows the anodic oxidation time, etching time, the adjacent distance p of the holes in the molds f to m, the depth q of the holes, the depth r of the ridge, r / p, r / q , The height T of the convex portion, the half-value width HW, and the Y value, L * value, a * , b of the reflected light of the antireflection materials F to M in the antireflection materials F to M manufactured using the molds f to m. * And C * are shown.
- the height T of the convex portions in the antireflection materials F to M is smaller than the depth q of the holes of the moth-eye molds f to m.
- the greater the depth r of the flange portion in the mold the more resin stays between the convex portions in the antireflection material, and as a result, the convex portions in the antireflection material have a lower crushed shape.
- the height T of the convex portion in the antireflection materials F to H is substantially constant, but in the moth-eye mold i, the depth r of the ridge portion. Is relatively large, the resin constituting the antireflection material I stays in the portion corresponding to the ridge portion of the mold i during transfer, and the height T of the convex portion is greatly reduced.
- the depth r of the ridge portion is relatively small in the moth-eye molds j to l, the height T of the convex portion in the antireflection materials J to L is substantially constant, but in the moth-eye mold m, the depth of the ridge portion is set. Since r is relatively large, at the time of transfer, the resin constituting the antireflection material M stays in the portion corresponding to the flange portion of the mold m, and the height T of the convex portion is greatly reduced.
- the antireflection materials I and M corresponding to the molds i and m having the large depth r of the flange portion have a small height T of the convex portion with respect to the adjacent distance p of the convex portion, and thus the antireflection materials I and M are reflective. Cannot be prevented sufficiently.
- the adjacent distance p of the convex portion in the antireflection material is relatively long, although the reflected light is hardly colored, the scattering component increases and the Y value becomes relatively high.
- the adjacent distance p of the hole and the depth r of the flange portion in the moth-eye mold satisfy the relationship of 0.15 ⁇ r / p ⁇ 0.60, the adjacent distance p of the convex portion is approximately 400 nm.
- the Y value of the antireflection material can be suppressed to 0.52 or less.
- an antireflection material that sufficiently suppresses reflection of light can be suitably produced.
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Abstract
Description
まず、図1を参照して本発明によるモスアイ用型100の実施形態を説明する。図1(a)にモスアイ用型100の鳥瞰SEM像を示し、図1(b)にモスアイ用型100の模式的な断面図を示す。SEM像は、走査型電子顕微鏡(Scanning Electron Microscope:SEM)で撮像される。鳥瞰SEM像はモスアイ用型100の表面全体の法線方向に対して傾斜した方向から撮像した画像である。
200 反射防止材
Claims (8)
- モスアイ構造の表面形状の反転した形状の表面を有する型であって、
前記表面には、複数の突起部と、それぞれが鞍部を介して前記複数の突起部を結ぶ複数の稜線と、それぞれが前記複数の突起部のうちの任意の少なくとも3つの突起部および前記任意の少なくとも3つの突起部を結ぶ稜線で規定される複数の穴とが設けられており、
隣接する穴の中心間の平均距離p、および、前記鞍部の平均深さrが、
0.15≦r/p≦0.60
の関係を満たす、型。 - 前記平均距離pは180nm以上420nm以下である、請求項1に記載の型。
- 前記複数の穴の平均深さqは380nm以上410nm以下である、請求項1または2に記載の型。
- 前記表面はポーラスアルミナ層の表面である、請求項1から3のいずれかに記載の型。
- モスアイ構造の表面形状の反転した形状の表面を有する型の作製方法であって、
表面にアルミニウムが設けられた基材を用意する工程と、
前記アルミニウムに陽極酸化およびエッチングを行うことによって、複数の突起部と、それぞれが鞍部を介して前記複数の突起部を結ぶ複数の稜線と、それぞれが前記複数の突起部のうちの任意の少なくとも3つの突起部および前記任意の少なくとも3つの突起部を結ぶ稜線で規定される複数の穴とが設けられた表面を有するポーラスアルミナ層を形成する工程と
を包含し、
前記ポーラスアルミナ層を形成する工程において、隣接する穴の中心間の平均距離p、および、前記鞍部の平均深さrが、
0.15≦r/p≦0.60
の関係を満たす、型の作製方法。 - 前記ポーラスアルミナ層を形成する工程において、前記平均距離pは180nm以上420nm以下である、請求項5に記載の型の作製方法。
- 前記ポーラスアルミナ層を形成する工程において、前記複数の穴の平均深さqは380nm以上410nm以下である、請求項5または6に記載の型の作製方法。
- 請求項5から7のいずれかに記載の作製方法で型を作製する工程と、
前記型が光硬化性樹脂と接した状態で光を照射することによって前記光硬化性樹脂を硬化する工程と
を包含する、モスアイ構造の作製方法。
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US13/511,315 US8747683B2 (en) | 2009-11-27 | 2010-11-25 | Die for moth-eye, and method for producing die for moth-eye and moth-eye structure |
CN201080052752.2A CN102639307B (zh) | 2009-11-27 | 2010-11-25 | 模具的制作方法和蛾眼结构的制作方法 |
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US (1) | US8747683B2 (ja) |
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WO2015105071A1 (ja) * | 2014-01-10 | 2015-07-16 | デクセリアルズ株式会社 | 反射防止構造体及びその設計方法 |
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Also Published As
Publication number | Publication date |
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US8747683B2 (en) | 2014-06-10 |
US20120234794A1 (en) | 2012-09-20 |
CN102639307B (zh) | 2014-08-06 |
CN102639307A (zh) | 2012-08-15 |
TWI457589B (zh) | 2014-10-21 |
TW201131196A (en) | 2011-09-16 |
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