WO2016163510A1 - マスク付基板、および、凹凸構造付基板の製造方法 - Google Patents

マスク付基板、および、凹凸構造付基板の製造方法 Download PDF

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WO2016163510A1
WO2016163510A1 PCT/JP2016/061508 JP2016061508W WO2016163510A1 WO 2016163510 A1 WO2016163510 A1 WO 2016163510A1 JP 2016061508 W JP2016061508 W JP 2016061508W WO 2016163510 A1 WO2016163510 A1 WO 2016163510A1
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Prior art keywords
mask
substrate
particles
etching
particle film
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PCT/JP2016/061508
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English (en)
French (fr)
Japanese (ja)
Inventor
康仁 梶田
智 平間
紘太郎 大
啓 篠塚
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王子ホールディングス株式会社
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Application filed by 王子ホールディングス株式会社 filed Critical 王子ホールディングス株式会社
Priority to KR1020177026598A priority Critical patent/KR20170137070A/ko
Priority to CN201680018960.8A priority patent/CN107431010B/zh
Priority to JP2017511089A priority patent/JP6485542B2/ja
Publication of WO2016163510A1 publication Critical patent/WO2016163510A1/ja

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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 potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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 potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/005—Processes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/20—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies with a particular shape, e.g. curved or truncated substrate
    • H01L33/22—Roughened surfaces, e.g. at the interface between epitaxial layers

Definitions

  • the present invention relates to a substrate with a mask and a method for manufacturing a substrate with an uneven structure having an uneven structure on the upper surface of the substrate.
  • a substrate with a concavo-convex structure has been used as a substrate provided in a semiconductor light emitting element used for, for example, a light emitting diode.
  • the substrate with a concavo-convex structure has a concavo-convex structure on the upper surface of the substrate, and the semiconductor light-emitting element is composed of the substrate and a light-emitting structure stacked on the upper surface of the substrate.
  • Total reflection at the interface between the light emitting structure and the substrate attenuates light generated in the light emitting structure inside the light emitting structure.
  • the concavo-convex structure of the substrate suppresses the attenuation of light inside the light emitting structure and increases the light extraction efficiency in the semiconductor light emitting element.
  • the substrate with a concavo-convex structure described above is a substrate used for organic semiconductor devices and various antireflection materials, a substrate for cell culture, and a concavo-convex structure that is lyophilic or liquid repellent. It is used as a wettability control board that functions as a developing structure.
  • Such a concavo-convex structure of the substrate is formed by dry etching the upper surface of the substrate using a particle film made of a large number of fine particles as a mask, as described in Patent Document 1, for example.
  • the present invention relates to a substrate with a mask capable of enhancing the versatility of a substrate with a mask provided with a particle film, and a method for manufacturing a substrate with an uneven structure using the substrate with a mask to manufacture a substrate having an uneven structure.
  • the purpose is to provide.
  • a substrate with a mask for solving the above problem employs the following configuration.
  • the substrate with mask, which is fixed and the fixing layer is substantially composed of a material having a melting point of 100 ° C. or higher.
  • the apparatus further includes a second mask positioned on the substrate, and either the fixed layer or the particle film is a lower layer of the second mask, and the second mask follows the surface of the lower layer.
  • the manufacturing method of the substrate with a concavo-convex structure for solving the above problems employs the following configuration.
  • [6] A method for producing a substrate with a concavo-convex structure, wherein the concavo-convex structure is formed on the upper surface of the substrate by etching the upper surface of the substrate on which the mask is located, using the substrate with a mask according to [5].
  • the manufacturing method of the substrate with a concavo-convex structure in the present embodiment includes a first mask forming step of forming a first mask that is a mask including a particle film, and a second mask forming step of forming a second mask made of a resist film.
  • a composite mask process configured and an etching process are included.
  • the first mask 21 is formed on the upper surface S of the substrate 11, and the substrate with an uneven structure including the substrate 11 and the first mask 21 as an example of the substrate with mask.
  • Forming intermediate 30 is formed.
  • the first mask 21 includes a single particle film F and a fixed layer 23, and FIG. 1 shows a state where the fixed layer 23 is formed on the substrate 11.
  • the composite mask forming process including the first mask forming process and the second mask forming process includes a first mask 21 and a second mask 22 on the upper surface S of the substrate 11.
  • the composite mask 20 is formed, and the substrate forming intermediate body 30 with the concavo-convex structure including the substrate 11 and the composite mask 20 is formed as an example of the substrate with mask.
  • an etching process forms a board
  • First mask forming step In the first mask forming step, a single particle film forming step in which a single particle film F composed of particles P arranged in a plane is formed on the upper surface S of the substrate 11, and the particles P included in the single particle film F are formed on the upper surface. A fixing layer forming step in which the fixing layer 23 fixed to S is formed.
  • the single particle film F is formed on the upper surface S of the substrate 11.
  • the material constituting the particles P include metals such as Al, Au, Ti, Pt, Ag, Cu, Cr, Fe, Ni, and W, SiO 2 , Al 2 O 3 , TiO 2 , MgO 2 , and CaO 2. And metal oxides and Si.
  • the material constituting the particles P include nitrides such as SiN and TiN, carbides such as SiC and WC, organic polymers such as polystyrene and polymethyl methacrylate, other semiconductor materials, and inorganic polymers.
  • grains P can also use together at least 2 types of these.
  • the material constituting the particles P is preferably an inorganic oxide from the viewpoint of a high degree of freedom in the etching selectivity with respect to the upper surface S.
  • the material constituting the particles P is more preferably silica among inorganic oxides.
  • the particle size of the particles P is preferably 10 nm or more and 10 ⁇ m or less.
  • the single particle film F is formed by using any one of the following five methods or a combination of two or more.
  • LB method Langmuir-Blodget method
  • Dip coating method Spin coating method
  • Slit (die) coating method Particle adsorption method (electrical method)
  • LB method a dispersion liquid in which particles P are dispersed in a solvent having a specific gravity lower than that of water is used.
  • the dispersion liquid is dropped onto the liquid surface of water.
  • the solvent is volatilized from the dispersion, whereby a single particle film F made of particles P is formed on the water surface.
  • the single particle film F formed on the water surface is transferred to the upper surface S of the substrate 11, whereby the single particle film F is formed on the upper surface S of the substrate 11.
  • a dispersion in which particles P are dispersed in a solvent is used.
  • the substrate 11 is immersed in the dispersion.
  • the single particle film F made of particles P and the solvent adhere to the upper surface S of the substrate 11.
  • the single particle film F is formed on the upper surface S of the substrate 11 by drying the solvent on the upper surface S of the substrate 11.
  • a dispersion in which particles P are dispersed in a solvent is used.
  • the substrate 11 is placed on a spin coater, and the dispersion is dropped onto the spin coater.
  • the dispersion liquid is uniformly applied to the upper surface S of the substrate 11 by rotating the substrate 11.
  • the single particle film F is formed in the upper surface S of the board
  • a dispersion liquid in which particles P are dispersed in a solvent is used.
  • the substrate 11 is placed on a slit coater.
  • the dispersion liquid is uniformly applied to the upper surface S of the substrate 11 by applying the dispersion liquid to the upper surface S of the substrate 11 as a thin film having a uniform concentration using a slit.
  • the single particle film F is formed in the upper surface S of the board
  • the substrate 11 is immersed in a suspension of colloidal particles.
  • the second and higher particles P are removed so that only the first particle layer electrostatically coupled to the upper surface S of the substrate 11 remains. Thereby, the single particle film F is formed on the upper surface S of the substrate 11.
  • the film forming method used in the single particle film forming step is preferably a method in which the filling degree D (%) represented by the following formula (1) is 15% or less.
  • the LB method is preferable from the viewpoints of the accuracy of monolayer formation, the ease of operation required for film formation, the expandability of the area of the single particle film F, the reproducibility of the characteristics of the single particle film F, and the like.
  • the filling degree D is an index indicating the degree of close packing of the particles P in the single particle film F.
  • the filling degree D is preferably 10% or less, and more preferably 1.0% or more and 3.0% or less.
  • the average particle size A of the particles P is the average primary particle size of the particles P constituting the single particle film F.
  • the average primary particle size of the particles P is obtained from the peak of the particle size distribution.
  • the particle size distribution is obtained from an approximation of the particle size distribution obtained by the particle dynamic light scattering method.
  • the particle size P coefficient of variation is preferably 20% or less, and preferably 10% or less. Is more preferable, and it is further more preferable that it is 5% or less.
  • the mode value in the pitch between the particles P is the mode value of the distance between the vertices of the two particles P adjacent to each other.
  • the distance between the vertices of the adjacent particles P is the distance between the centers of the adjacent particles P.
  • the filling degree D (%) in the single particle film is smaller, the arrangement of the particles P is closer to a two-dimensional hexagonal filling structure or becomes a polycrystalline structure in which a plurality of two-dimensional hexagonal filling structures are aggregated.
  • the material constituting the fixing layer 23 is substantially a substance having a melting point of 100 ° C. or higher, and preferably has resistance to the developer, specifically, alkali resistance.
  • An example of having alkali resistance is that when the fixing layer 23 is immersed in a 2.38% aqueous solution of tetramethylammonium hydroxide, which is an example of a developing solution, at room temperature and normal pressure, the volume in the fixing layer 23 is 15 minutes. This is a property in which the amount of decrease is 5% or less, that is, the dissolution rate is 5% or less compared to the fixed layer 23 before being immersed.
  • the fixing layer 23 is formed in the process of immersing the substrate for forming a concavo-convex structure 30 in the alkaline solution. Is removed and the particles P are prevented from separating from the upper surface S of the substrate 11.
  • the melting point of the material constituting the fixing layer 23 is substantially 100 ° C. or higher. Therefore, it is possible to prevent a deviation in the arrangement of the particles and a deformation of the second mask associated therewith. From such a viewpoint, the melting point of the material constituting the fixed layer 23 is preferably substantially 150 ° C. or higher, and more preferably 200 ° C. or higher.
  • the material constituting the fixing layer 23 is substantially a substance having a melting point of 100 ° C. or higher, and resistance to a resist stripper, for example, resistance to acetone, amine or amine and water. It preferably has resistance to amine-based drugs.
  • acetone which is a general resist stripping solution, at room temperature and normal pressure for 1 hour, the volume decrease in the fixing layer 23 is fixed before being immersed.
  • the volume of the layer 23 is 5% or less, that is, the dissolution rate is 5% or less. Further, when the fixing layer 23 is immersed in acetone at room temperature and normal pressure and ultrasonic treatment is performed for 30 minutes by applying an ultrasonic wave of 100 W at an oscillation frequency of 35 kHz, the volume of the fixing layer 23 is reduced. However, it is preferable that it is 5% or less with respect to the volume of the fixed layer 23 before being immersed, that is, the dissolution rate is 5% or less. According to such a configuration, even when the rework of the resist film is performed, it is possible to prevent the fixed layer 23 from being removed and the particles P from separating from the upper surface S of the substrate 11 during the rework.
  • the material constituting the fixing layer 23 can be selected from inorganic or organic coating agents.
  • the inorganic coating agent include a compound group based on a silane, titanate, or aluminate alkoxide hydrolyzate, and a silicone resin compound group.
  • the organic coating agent include vinyl, polystyrene, polypropylene, polyacetal, acrylic, cellulose acetate, polycarbonate, polyethylene terephthalate, polyamide, polyurethane, and fluorine.
  • the material constituting the fixing layer 23 may have a selection ratio of the fixing layer 23 to the particles P larger than 1 and 1.2 or more and 7.0 or less. preferable.
  • the etching of the fixed layer 23 is preferentially performed over the etching of the single particle film F, and the substrate 11 is etched in a state where only the single particle film F remains on the upper surface S. It becomes possible. Then, it is possible to form a concavo-convex structure on the substrate 11 with the portion covered with the particles P in the upper surface S as a protrusion.
  • the selection ratio of the fixed layer 23 to the particles P may be a value smaller than 1 or 0.1 or more and 0.9 or less.
  • the etching of the single particle film F proceeds preferentially over the etching of the fixed layer 23, and the substrate 11 is etched with only the fixed layer 23 remaining on the upper surface S. Is possible. In other words, it is possible to form a concavo-convex structure on the substrate 11 with the portion covered with the fixing layer 23 in the upper surface S as a protrusion.
  • the film thickness of the fixing layer 23 is the thickness from the upper surface S of the substrate 11 to the upper end of the fixing layer 23, and is preferably 0.3 times or more and 2.0 times or less the average particle diameter A of the particles P. More preferably, it is more than 0.5 times and not more than 1.5 times the average particle diameter A of the particles P. Further, when the average particle diameter A of the particles P is 1 ⁇ m or more, the value obtained by subtracting the average particle diameter A of the particles P from the film thickness of the fixed layer 23 is preferably 300 nm or less.
  • the film thickness of the fixed layer 23 is 0.3 times the average particle diameter A of the particles P, gaps such as holes penetrating the single particle film F in the thickness direction of the single particle film F are formed in the single particle film F. Formation is suppressed.
  • the 2nd mask 22 is formed by apply
  • the gap of the single particle film F is filled with the resist material of the second mask 22, the effect of the single particle film F as a mask is reduced, and the formation of the unevenness following the first mask 21 does not proceed sufficiently. There is.
  • An adhesive force is generated at the interface between the fixing layer 23 and the particles P. Since the adhesive force increases as the area of the interface increases, the retention force of the particles P increases as the thickness of the fixing layer increases.
  • the fixing layer 23 exceeds 0.5 times the average particle diameter A of the particles P, the fixing layer 23 has the particles so that the fixing layer 23 wraps each particle P as shown in FIG. It is filled between P. In this case, a physical anchor effect is generated between the particles P and the fixed layer 23, and the retention force of the particles is increased.
  • An opening is formed in a portion of the upper surface of the fixed layer 23 where the particle P protrudes, and the diameter of the peripheral line in the opening is smaller than the particle diameter of the particle P.
  • the physical anchor effect described above is obtained by the fact that the diameter of the circumferential line at the opening of the pinned layer 23 is smaller than the particle size of the particles P, thereby preventing the particles from passing through the opening of the pinned layer 23. It is. As described above, when the film thickness of the fixing layer 23 exceeds 0.5 times the average particle diameter A of the particles P, the interfacial adhesive force is increased and the anchor effect is exhibited, whereby the particles P are bonded to the fixing layer 23. Is held stably.
  • the fixed layer 23 between the first mask 21 and the second mask 22 advances along the upper surface S of the substrate 11. It is possible to prevent the second mask 22 from being peeled off during the etching by being exposed to the etching gas.
  • a known coating method such as a spin coating method, a slit & spin coating method, a slit coating method, or a dip coating method can be used.
  • the fixing layer 23 is dried, heated, and solidified to increase the force for fixing the particles P.
  • the second mask 22 is laminated on the first mask 21 on the substrate 11.
  • the second mask 22 is a mask patterned into a predetermined shape.
  • the second mask 22 is formed by applying a liquid material containing a resist material on the first mask 21 and then patterning the applied resist material into a predetermined shape.
  • the resist material a material that can be suitably patterned and that is suitable as a mask in an etching process, such as a known photosensitive functional polymer material, may be used.
  • the liquid containing the resist material is, for example, a mixture containing a polymer, a photosensitizer, an additive, and a solvent as main components.
  • a resist material patterning method nanoimprint or photolithography is used.
  • the second mask 22 composed of a plurality of mask elements is formed on the first mask 21 which is the lower layer of the second mask 22.
  • Each mask element constituting the second mask 22 is a minimum unit of a structure functioning as a mask in the second mask 22, and is a protrusion 24 protruding from the first mask 21 in the present embodiment.
  • the shape of the protruding portion 24 is not particularly limited, and the protruding portion 24 may have a cone shape that narrows from the base end toward the tip end, such as a hemispherical shape, a conical shape, and a pyramid shape. However, it may have a truncated cone shape in which the tip portion is formed flat, such as a shape in which the top of the hemisphere is cut off, a truncated cone shape, or a truncated pyramid shape. Alternatively, the protruding portion 24 may have a rectangular parallelepiped shape, and the protruding portion 24 is a linear shape extending in one direction along the upper surface S of the substrate 11 when viewed from the direction facing the upper surface S of the substrate 11. It may be formed.
  • the plurality of protrusions 24 may include protrusions 24 having different shapes. When viewed from the direction facing the upper surface S of the substrate 11, the plurality of protrusions 24 may be arranged regularly or irregularly.
  • the protrusion 24 is larger than the particles P constituting the first mask 21 when viewed from the direction facing the upper surface S of the substrate 11.
  • the maximum dimension of the outer shape of the protruding portion 24 when viewed from the direction facing the upper surface S of the substrate 11 is The diameter A is preferably 2 times or more and 100 times or less.
  • the maximum dimension of the outer shape of the protruding portion 24 when viewed from the direction facing the upper surface S of the substrate 11 is relative to the average particle size A of the particles P. It is preferably 2 times or more and 100 times or less.
  • the second mask 22 is formed by applying a liquid material to the first mask 21 and curing the applied liquid material, such a step is required as long as the surface of the first mask 21 is a step surface.
  • the bottom surface of the second mask 22 has a shape that fills the surface. That is, the bottom surface of the second mask 22 has a surface shape that follows the shape of the surface of the first mask 21.
  • the composite mask 20 is formed by stacking the first mask 21 and the second mask 22.
  • the upper surface S of the substrate 11 on which the composite mask 20 is formed is covered with the particles P of the first mask 21 in the gap between the protruding portion 24 of the second mask 22 and the protruding portion 24 adjacent to each other. A portion and a portion that is not covered by any of the protrusions 24 and the particles P are partitioned.
  • the upper surface S of the substrate 11 is etched using the composite mask 20. Specifically, the upper surface S is etched using the second mask 22 as a mask, and the upper surface S is etched using the first mask 21 positioned between the protrusions 24 of the second mask 22 as a mask. Further, as the protrusion 24 is reduced, the upper surface S is etched using the particles P covered by the protrusion 24 as a mask. That is, in the etching process using the composite mask 20, the etching using the second mask 22 and the etching using the first mask 21 are performed simultaneously.
  • the etching rate of the first mask 21, the second mask 22, and the substrate 11 is controlled by selecting the type of etching gas, the flow rate of the etching gas, and the etching time, and a desired uneven shape is obtained. Can do.
  • (Etching condition example 1) An example of etching conditions for forming a concavo-convex structure on the upper surface S of the substrate 11 is shown.
  • the ratio of the etching rate of the upper surface S to the etching rate of the particles P is determined by the material constituting the particles P and the material constituting the substrate 11.
  • the shape of the desired concavo-convex structure can be obtained by appropriately selecting the etching gas used for reactive etching according to the desired shape.
  • the etching gas used for reactive etching for reactive etching according to the desired shape.
  • one or more gases selected from the group consisting of Cl 2 , BCl 3 , SiCl 4 , HBr, HI, HCl, Ar are used as the etching gas. That's fine.
  • the large protrusion 12 and the small protrusion 12 are formed on the upper surface S of the substrate 11 masked between the protrusions 24.
  • a composite structure of the protrusions 13 is formed.
  • the small protrusions 15 are formed between the adjacent composite structures, but the adjacent composite structures can be changed by changing the etching conditions, for example, by increasing the etching time. It is also possible to eliminate the small protrusions 15 formed between the bodies.
  • Etching condition example 2 is an etching condition for realizing at least one of enlarging the flat part 14 positioned between the large protrusions 12 adjacent to each other and enhancing the flatness of the flat part 14.
  • the ratio of the etching rate of the upper surface S to the etching rate of the particles P is preferably 25% or less, which is smaller than that of the etching condition example 1.
  • the ratio of the etching rate of the upper surface S to the etching rate of the particles P is more preferably 15% or less, and particularly preferably 10% or less.
  • Such an etching condition can be obtained by appropriately selecting an etching gas used for reactive etching.
  • an etching gas used for reactive etching For example, when the substrate 11 is sapphire and the particle P is silica, CF 4 , SF 6 , CHF 3 , C 2 F 6 , C 3 F 8 , C 4 F 8 , CH 2 F 2 , NF 3
  • gases selected from the group consisting of may be used as the etching gas.
  • a rare gas such as Ar or an additive gas such as O 2 to the etching gas as necessary for etching the substrate 11.
  • the etching gas is not limited to these, and is appropriately selected according to the material of the particles P constituting the first mask 21, the resist material constituting the second mask 22, and the material of the substrate 11.
  • the substrate 11 on which the composite mask 20 is stacked is etched in the etching condition example 2, as shown in FIG. 6, while the particles P constituting the first mask 21 between the protrusions 24 of the second mask 22 are reduced, A small protrusion 15 is formed on the upper surface S of the substrate 11.
  • the small protrusion 15 formed here is smaller than the example shown in FIG. 4, and when further etching is performed under this etching condition, the small protrusion 15 disappears, and as shown in FIG.
  • the flat portion 14 between the protruding portions 24 is expanded, and the flatness in the flat portion 14 is enhanced.
  • the large protrusion 12 protruding from the flat portion 14 is formed at a portion surrounded by the flat portion 14, that is, at a portion facing the protruding portion 24 in the upper surface S of the substrate 11. It is formed.
  • the shape of the large protrusion 12 is a shape that conforms to the shape of the protrusion 24 in the second mask 22 and the etching conditions.
  • the arrangement pattern such as the arrangement interval and arrangement rule of the large protrusions 12 is equivalent to the arrangement pattern of the protrusions 24 in the second mask 22.
  • a small protrusion 13 is formed on a portion of the upper surface S of the substrate 11 facing the particle P covered with the protrusion 24 before the etching is started. Is formed.
  • the uneven structure which has the large protrusion 12 which has the flat top part, and the small protrusion 13 which protruded from the top part of the large protrusion 12 is obtained.
  • the upper surface S of the substrate 11 includes a large protrusion 12 having a linear shape extending in the vertical direction of the paper surface, a small protrusion 13 having a cone shape, and a flat portion 14 formed flat. It has a concavo-convex structure.
  • the shape in which the large protrusion 12 shown in FIG. 10 extends in a line shape in plan view is obtained by etching using the second mask 22 having a rectangular parallelepiped protrusion 24 extending in a line shape. If the second mask 22 has a cross-sectional shape that extends in a line shape in plan view and has a cross-sectional shape in which the central portion of the protruding portion 24 is thicker than the end portion of the protruding portion 24, the cross-sectional shape is the shape shown in FIG.
  • the concavo-convex structure whose planar view shape is the shape shown in FIG. 10 can be formed.
  • the cylindrical or prismatic large projecting portion 12 is formed. Can be formed.
  • the large projecting portion formed by etching is also shown in FIG.
  • the central portion of the large protrusion 12 is thicker than the end of the large protrusion 12.
  • the composite mask 20 in which the central portion of the projecting portion 24 is thicker than the end portion of the projecting portion 24 heats the composite mask 20 shown in FIG. 8 to soften and soften the projecting portion 24 made of a resist material. It is obtained by deforming the protrusion 24 into a hemisphere by the surface tension of the resist material.
  • the etching of the upper surface S of the substrate 11 may be stopped before some or all of the plurality of particles P constituting the single particle film F disappear.
  • the small protrusion 13 having a shape different from the above, such as a frustum shape, can be formed according to the etching stop timing.
  • the etching of the upper surface S of the substrate 11 is stopped. May be.
  • the small protrusion 15 is also formed in the region located in the center of the gap between the adjacent protrusions 24 on the upper surface S of the substrate 11. That is, a small protrusion 15 protruding from the flat portion 14 is formed.
  • the etching conditions under which the substrate 11, the first mask 21, and the second mask 22 are etched are set so that, for example, the selectivity between the substrate 11 and the mask becomes a preferable value. Further, the height and the like of the protrusion 24 in the second mask 22 is set so that the large protrusion 12 has a desired size by etching using the composite mask 20.
  • the etching gas used for etching the upper surface S of the substrate 11 is not limited to the etching condition example, and the material of the particles P constituting the first mask 21, the resist material constituting the second mask 22, and the substrate 11. It is appropriately selected depending on the material.
  • the etching conditions suitable for etching using the first mask 21 as a mask and the second mask according to the progress of etching may be switched.
  • the substrate 11 is etched using the composite mask 20 that is a laminate of two types of masks, thereby forming Is formed.
  • the composite mask 20 that is a laminate of two types of masks, thereby forming Is formed.
  • the second mask 22 is more flexible than the first mask 21 including the single particle film F with respect to the setting of the shape of the mask element of the mask, and therefore compared with the method using only the particle film as the mask.
  • various uneven structures can be formed.
  • the first mask 21 includes a fixing layer 23, and the fixing layer 23 fixes the particles P constituting the single particle film F and fixes the particles P and the upper surface S of the substrate 11. Therefore, when the second mask 22 is stacked on the first mask 21, it is possible to prevent the particles P from separating from the upper surface S of the substrate 11.
  • the second mask 22 and the first mask 21 including the single particle film F can change the shape of the mask elements of the mask, it is compared with a method using only the particle film as a mask. Thus, various uneven structures can be formed.
  • the particles P are detached from the upper surface S of the substrate 11 even when a process such as a development process or a cleaning process of the photoresist material is performed. This is suppressed by the fixing layer 23.
  • the concavo-convex structure has the large protrusion 12 and the small protrusion 13, the traveling direction of the light generated in the light emitting structure is changed by light refraction, diffraction, or the like. As a result, since the total reflection at the interface between the light emitting structure and the substrate 11 is suppressed, the light extraction efficiency can be increased. Further, in a semiconductor light emitting device having a configuration that transmits light to the outside through the substrate 11, the surface (light extraction surface) opposite to the side where the light emitting structure is provided is the upper surface S.
  • the emitted light has an incident angle greater than or equal to the critical angle with respect to the plane extending along the upper surface S, it can be less than the critical angle with respect to the slope of the concavo-convex structure. Therefore, the light extraction efficiency at the interface between the substrate 11 and the air can be greatly improved.
  • the substrate is suitable for crystal growth of the material of the semiconductor light emitting element on the upper surface S.
  • FIG. 11 shows an enlarged cross section of the concavo-convex structure shown in FIG. 5 or 7.
  • each of the plurality of small protrusions 13 protrudes from the large protrusion 12.
  • Each of the plurality of small protrusions 13 has a shape that narrows from the base of the small protrusion 13 connected to the large protrusion 12 toward the tip.
  • the large protrusion 12 is larger than the small protrusion 13.
  • the radius of the circle circumscribing the large protrusion 12 is larger than the radius of the circle circumscribing the small protrusion 13. large.
  • the distance between the large protrusions 12 adjacent to each other, and the distance along the direction parallel to the flat part 14 is the pitch PL of the large protrusions 12.
  • the outer surface of the large protrusion 12 is a surface connected to the small protrusion 13.
  • the maximum value of the distance between the surface of the large protrusion 12 connected to the small protrusion 13 and the surface of the small protrusion 13 in the normal direction of the surface of the large protrusion 12 connected to the small protrusion 13 Is the height HS of the small protrusion 13.
  • the portion having the height HS in each of the plurality of small protrusions 13 is the apex of the small protrusion 13, the distance between the apexes of the adjacent small protrusions 13, and the direction parallel to the flat portion 14. Is a pitch PS of the small protrusions 13.
  • the mode value of the pitch PL of the large protrusions 12 is preferably 300 nm or more and 5.0 ⁇ m or less, and the mode value of the pitch PS of the small protrusions 13 is preferably 100 nm or more and 1.0 ⁇ m or less. If the pitches PL and PS of the protrusions 12 and 13 are in the above ranges, the protrusions 12 and 13 are arranged on the upper surface S with the necessary arrangement and density to such an extent that total reflection of light on the upper surface S can be suppressed. It is formed.
  • FIG. 12 shows an enlarged part of the planar structure in the concavo-convex structure shown in FIG. 5, FIG. 7 or FIG.
  • the substrate 11 is etched using the single particle film in which the particles P form a plurality of hexagonal filling structures as the first mask 21, the plurality of small protrusions 13 form a hexagonal filling structure TG as shown in FIG. To do.
  • the small protrusion group TL is composed of a plurality of hexagonal filling structures TG.
  • the plurality of small protrusion groups TL includes two or more small protrusion groups in which at least one of the direction in which the hexagonal filling structure TG is arranged, the area occupied by the single small protrusion group TL, and the shape of the single small protrusion group TL is different from each other. Includes TL. That is, in a plan view, at least one of the plurality of small protrusion groups TL has a direction in which the hexagonal filling structures TG are arranged with respect to the other small protrusion groups TL, the size of the small protrusion groups TL, and At least one of the shapes is irregular.
  • One or more small protrusions TL are located on the outer surface of one large protrusion 12.
  • a plurality of small protrusions TL are divided into each small protrusion TL by a virtual line A2, and one small protrusion is formed on the outer surface of one large protrusion 12.
  • Team TL is located.
  • the two small protrusion groups TL partitioned by the virtual line A2 are different from each other in the direction in which the hexagonal filling structures TG are arranged.
  • the arrangement pattern of the small protrusions 13 is equivalent to the arrangement pattern of the particles P in the first mask 21.
  • FIG. 13 is a cross-sectional view showing the concavo-convex structure obtained by the masked substrate in which the film thickness of the fixing layer 23 in the above embodiment is 0.2 times the average particle diameter A of the particles P.
  • FIG. 14 is a cross-sectional view showing the concavo-convex structure obtained by the masked substrate in which the film thickness of the fixing layer 23 in the above embodiment is 0.5 times the average particle diameter A of the particles P.
  • FIG. 15 is a cross-sectional view showing a concavo-convex structure obtained by a masked substrate as a reference example in which the fixing layer 23 is omitted from the masked substrate in the embodiment.
  • the concavo-convex structure obtained by the masked substrate in which the thickness of the fixed layer 23 is 0.5 times the average particle size A of the particles P is 0.2 times the average particle size A of the particles P.
  • the height at the small protrusion 13 changes sharply, and stronger light scattering characteristics and antireflection characteristics can be obtained.
  • the concavo-convex structure obtained by the masked substrate of the reference example in which the fixing layer 23 is omitted it is unclear whether or not the small protrusion 13 exists on the large protrusion 12.
  • the cause of the difference in the uneven structure is considered as follows.
  • a liquid photoresist material that is a material for forming the second mask 22 is applied to the first mask 21.
  • the photoresist material penetrates into the gaps between the particles P constituting the particles, and fills the gaps between the particles P.
  • the difference in etching rate between the portion of the upper surface S covered by the first mask 21 and the portion not covered by the first mask 21 is reduced.
  • the fixed layer 23 having an etching rate much higher than that of the photoresist material fills the gap between the particles P, whereby the small protrusion 13 having a large aspect ratio can be formed. .
  • the form mentioned above can also be changed as follows.
  • the protrusion 24 constituting the second mask 22 may be smaller than the particles P constituting the first mask 21 when viewed from the direction facing the upper surface S of the substrate 11. Then, by using the first mask 21 and the second mask 22, the substrate with a concavo-convex structure is formed according to the shape and arrangement pattern of the protrusions 24 when viewed from the direction facing the upper surface S of the substrate 11.
  • the size of the second protrusion, which is a protrusion is smaller than the size of the first protrusion, which is a protrusion formed according to the size of the particles P and the arrangement pattern.
  • the second mask 22 is formed by curing the liquid material, it is easier to ensure the accuracy of the shape when the size of the protruding portion 24 is larger than that of the particle P. Therefore, among the convex portions included in the mask elements of the first mask 21 and the convex portions included in the mask elements of the second mask 22, the relatively small convex portions are the particles P, and the relatively large convex portions are the protruding portions 24. As compared with the configuration in which the protrusion 24 is smaller than the particle P, it is easier to ensure the shape accuracy of the mask elements in each mask.
  • the size of the protrusions arranged regularly is larger than the size of the protrusions composed of the irregularly arranged hexagonal filling structure TG.
  • the regularity of the arrangement is higher than the regularity of the arrangement of the protrusions, the overall regularity on the upper surface S of the substrate with a concavo-convex structure is easily obtained in the substrate with a concavo-convex structure.
  • the 2nd mask 22 should just have the mask element which covers the lower layer of the 2nd mask 22, and the shape and arrangement pattern of the projection part 24 which is a mask element are the shape quoted in the said embodiment and modification, It is not limited to the arrangement pattern.
  • the plurality of protrusions 24 may be positioned on the lattice points of the triangular lattice or the lattice points of the square lattice.
  • the second mask 22 may have one protrusion 24 as a whole.
  • the second mask 22 has a shape in which the unevenness of the shape illustrated in the above embodiment is inverted, and a recess.
  • the convex part which surrounds may have the structure connected to one.
  • the minimum unit of repeating unevenness that functions as a mask is a mask element.
  • the 2nd mask 22 is the structure which has the protrusion part 24 which protrudes from a lower layer, the lower layer of the 2nd mask 22 does not need to be exposed between the protrusion parts 24, and the 2nd mask 22 is a lower layer. You may cover the entire surface.
  • the mask element constituting the second mask 22 may have a protrusion connecting the protrusions 24 adjacent to each other in addition to the protrusion 24.
  • a second mask 22 As shown in FIG. 16, with a concavo-convex structure provided with a plurality of bridge portions 18 protruding from the flat portion 14 and connecting between the adjacent large protrusions 12.
  • a substrate is formed.
  • the bridge portion 18 has a protrusion shape, and the height of the bridge portion 18 is lower than the height of the large protrusion 12.
  • the shape of the bridge portion 18 is not limited to a linear shape, and may be a curved shape or a polygonal line shape, and the shape of each of the bridge portions 18 may be different from each other.
  • the shape and arrangement pattern of the bridge portion 18 can be adjusted by the shape and arrangement pattern of the protrusions connecting the protrusions 24 in the second mask 22.
  • the bridge portion 18 is formed, so that the light generated in the light emitting structure changes the direction in which the light travels at the position of the bridge portion 18 due to reflection or the like. Efficiency is further increased. Moreover, since the concavo-convex structure of the upper surface S of the substrate 11 becomes more complicated by forming the bridge portion 18, the effect of suppressing crystal defects is enhanced.
  • the material for forming the second mask 22 is not particularly limited as long as it is a material that functions as a mask in the etching process.
  • the second mask 22 may be a mask formed by curing a liquid material such as a liquid or a sol-like substance.
  • a liquid material such as a liquid or a sol-like substance.
  • the second mask 22 is a resist mask, it is possible to use an exposure technique suitable for fine processing for forming the second mask 22, and it is also versatile for etching using the second mask 22. Technology is available. Therefore, it is easy to form and etch the second mask 22.
  • the particle size of the particles P constituting the single particle film F may not be constant, and the single particle film F may include particles P having different particle sizes. Further, the particle film composed of the particles P in the first mask 21 may not be a film in which the particles P are arranged in a single layer, and the particle film has a region where the particles P are stacked. May be. In short, the first mask 21 may be a mask including a particle film composed of a plurality of particles P and a fixed layer.
  • the first mask 21 may include two or more single particle films F.
  • the first mask 21 is a first single particle film and a second single particle film made of particles P stacked on the first single particle film and having a particle diameter different from the particles P constituting the first single particle film.
  • the composite mask 20 used in the above embodiment has a three-layer film of a first single particle film, a second single particle film, and a resist film as a film that functions as a mask for etching.
  • the fixed layer may be formed in one layer with respect to the entire laminated single particle film, or may be formed for each single particle film.
  • the first mask 21 includes the first single particle film, the second single particle film stacked on the first single particle film, and the first single particle film from above the second single particle film. You may be comprised from the 1st adhering layer which covers a 2nd single particle film.
  • the first mask 21 includes a first single particle film, a first fixed layer covering the first single particle film, a second single particle film formed on the first fixed layer, and a second single particle film. And a second fixing layer covering the substrate.
  • the first mask 21 includes a two-layer single particle film F of a first single particle film and a second single particle film, the upper surface S of the substrate 11 among the first single particle film and the second single particle film.
  • the average particle diameter A of the particles P constituting the second single particle film which is the single particle film F far from the first particle film constitutes the first single particle film which is the single particle film F closer to the upper surface S of the substrate 11. It is preferable that the average particle diameter A of the particles P is larger.
  • the first single particle is smaller than the case where the average particle size A of the particles P constituting the second single particle film is smaller than the average particle size A of the particles P constituting the first single particle film.
  • the particles P constituting the second single particle film are easily arranged uniformly. Therefore, it is possible to obtain a substrate with a concavo-convex structure in which the uneven arrangement of the concavo-convex structure is suppressed from being biased, the shape accuracy is high, and a plurality of concavo-convex patterns having different periods are superimposed.
  • a third mask may be formed on the substrate 11, and etching using the third mask may be further performed.
  • the third mask may be a mask including a particle film composed of a plurality of particles P, or may be a mask formed by curing a liquid material, such as a resist mask.
  • the mask positioned on the substrate 11 in the substrate with mask is not limited to the composite mask, and may be only the first mask. That is, the substrate with a mask includes a single particle film F composed of a plurality of particles P, and the plurality of particles P are fixed to the substrate 11 by the fixing layer 23, and the fixing layer 23 has a melting point of substantially 100. What is necessary is just the structure comprised by the substance more than degreeC.
  • the upper surface S of the substrate 11 before the first mask 21 and the second mask 22 are formed may be non-planar.
  • the non-planar surface can be formed by the same method as the concavo-convex structure formed using the first mask 21 or the second mask 22 as a mask.
  • the non-planar surface can be formed using various known methods such as cutting, laser processing, casting, sand blasting, and shot peening.
  • the substrate 11 may be used for an organic semiconductor device or various antireflection materials, a substrate for cell culture, or a wettability control substrate that functions as a structure in which unevenness exhibits lyophilicity or liquid repellency. May be used.
  • a material corresponding to the use of the substrate 11 may be selected, and the flat portion 14 may be a flat surface, not a flat surface extending along one crystal plane.
  • FIG. 17 shows a shape example obtained by etching the upper surface S under the condition where the selective ratio of the pinned layer 23 to the particles P is smaller than 1 in the embodiment, that is, the mask elements of the first mask 21.
  • An example of the fixing layer 23 is shown. As shown in FIG.
  • a concave portion is formed in a portion of the surface of the large protrusion 12 where the particle P is located, and conversely, the particle P of the surface of the large protrusion 12
  • a convex part may be formed in the part which was not located. Even with such an uneven structure, light scattering characteristics and antireflection characteristics are imparted to the upper surface S of the substrate 11.
  • P particle, F ... single particle film, S ... upper surface, TG ... hexagonal filling structure, TL ... small projection group, 11 ... substrate, 12 ... large projection, 13,15 ... small projection, 14 ... flat portion, DESCRIPTION OF SYMBOLS 16 ... Light-emitting structure, 18 ... Bridge part, 20 ... Composite mask, 21 ... 1st mask, 22 ... 2nd mask, 23 ... Adhesion layer, 24 ... Projection part, 30 ... Intermediate for substrate formation with uneven structure.

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PCT/JP2016/061508 2015-04-09 2016-04-08 マスク付基板、および、凹凸構造付基板の製造方法 WO2016163510A1 (ja)

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