WO2009093700A1 - シームレスモールドの製造方法 - Google Patents
シームレスモールドの製造方法 Download PDFInfo
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- WO2009093700A1 WO2009093700A1 PCT/JP2009/051095 JP2009051095W WO2009093700A1 WO 2009093700 A1 WO2009093700 A1 WO 2009093700A1 JP 2009051095 W JP2009051095 W JP 2009051095W WO 2009093700 A1 WO2009093700 A1 WO 2009093700A1
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- WIPO (PCT)
- Prior art keywords
- mold
- sleeve
- seamless
- etching
- resist
- Prior art date
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- 0 C**1C#CCC11C(*C=C)C1 Chemical compound C**1C#CCC11C(*C=C)C1 0.000 description 1
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Classifications
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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
- B29C33/38—Moulds or cores; Details thereof or accessories therefor characterised by the material or the manufacturing process
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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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- 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
- B29C33/38—Moulds or cores; Details thereof or accessories therefor characterised by the material or the manufacturing process
- B29C33/3842—Manufacturing moulds, e.g. shaping the mould surface by machining
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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
- B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
- B29C59/02—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y10/00—Nanotechnology for information processing, storage or transmission, e.g. quantum computing or single electron logic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0002—Lithographic processes using patterning methods other than those involving the exposure to radiation, e.g. by stamping
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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
- B29C33/56—Coatings, e.g. enameled or galvanised; Releasing, lubricating or separating agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2833/00—Use of polymers of unsaturated acids or derivatives thereof as mould material
- B29K2833/04—Polymers of esters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2905/00—Use of metals, their alloys or their compounds, as mould material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41C—PROCESSES FOR THE MANUFACTURE OR REPRODUCTION OF PRINTING SURFACES
- B41C1/00—Forme preparation
- B41C1/02—Engraving; Heads therefor
- B41C1/04—Engraving; Heads therefor using heads controlled by an electric information signal
- B41C1/05—Heat-generating engraving heads, e.g. laser beam, electron beam
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
- H01J2237/26—Electron or ion microscopes
- H01J2237/28—Scanning microscopes
- H01J2237/2809—Scanning microscopes characterised by the imaging problems involved
- H01J2237/281—Bottom of trenches or holes
Definitions
- the present invention relates to a method for producing a seamless mold, and more particularly, to a method for producing a seamless mold for nanoimprint or optical film.
- Patent Literature 1 Conventionally, as a method for forming a fine shape on a nanoimprint or an optical element, a method has been used in which a shape is transferred to a glass substrate, a plastic substrate, a plastic film, etc. using a mold on which a fine shape has been previously formed (patent) Literature 1, Patent Literature 2).
- These technologies include a method of mechanically transferring a pattern by pressing a mold (or also called a mold or a template) as an original plate on which a pattern such as fine grooves and holes is formed, and pressing the material to be transferred.
- a mold or also called a mold or a template
- Examples thereof include a method of transferring using a plastic resin, and a method of transferring light using a photocurable resin (Patent Document 3).
- the resolution of the pattern in these methods is determined by the mold production accuracy. That is, once the mold can be formed, a fine structure can be formed with an inexpensive apparatus.
- a parallel plate type mold also called a wafer or a plate
- a cylindrical (roller) type mold are generally known (Patent Document 4, Non-Patent Document 1).
- a semiconductor lithography technique is used to apply an ultraviolet resist, electron beam resist, X-ray resist or the like on the substrate, and then irradiate and expose with ultraviolet light, electron beam, X-ray or the like.
- Patent Document 5 there are a method for producing an original plate having a desired pattern and a method for producing an original plate through a mask (reticle) on which a pattern is drawn in advance.
- etching having anisotropy is applied for etching in order to control the ratio of width to depth, that is, the aspect ratio.
- a method is employed in which etching is performed by arranging the flat plate-shaped mold and the counter electrode to face each other so that the distance between the etching part and the counter electrode facing each other is always equal.
- Etching proceeds uniformly in the same direction in the plane of the flat plate mold.
- the etching depth is controlled using a dry etching apparatus having such an apparatus design.
- the seamless roller mold needs to etch a curved surface, when a normal flat plate-shaped counter electrode is used, a portion where the distance between the etching layer and the flat plate-shaped counter electrode is not equal is generated. Since the etching direction and the etching rate are partially different from each other, it has been difficult to control the aspect ratio using such a method.
- Patent Document 8 and Patent Document 9 there has been a method using anodized porous alumina as the only method for forming a seamless roller mold with a submicron (1 ⁇ m or less) size pattern.
- an anodized porous alumina layer having a regular pore arrangement is formed, and an uneven shape corresponding to the pore arrangement is formed in a roll mold.
- the fine shapes that can be formed are limited to regular pore shapes of the same size, and pore shapes having various sizes are formed on the same roll, or there are rectangular or V-shaped irregularities.
- such a groove-like shape cannot be produced.
- This invention is made
- the method for producing a seamless mold according to the present invention includes a step of forming a heat-reactive resist layer on a sleeve-shaped mold, and a step of forming a fine mold pattern on the heat-reactive resist layer using a laser.
- the method for producing a seamless mold according to the present invention includes a step of forming a heat-reactive resist layer on a sleeve-shaped mold, and a step of forming a fine mold pattern on the heat-reactive resist layer using a laser.
- a method of manufacturing a seamless mold comprising: the thermal reaction type resist layer comprising a thermal reaction type resist having a temperature distribution including a region that reacts at a predetermined temperature or more in the spot diameter of the laser.
- the method for producing a seamless mold of the present invention before forming the heat-reactive resist layer on the sleeve-shaped mold, an etching layer is formed on the sleeve-shaped mold, and the fine mold pattern is used as a mask. It is preferable that the method further includes a step of etching the etching layer and a step of removing the fine mold pattern.
- the thermal reaction type resist is an organic resist or an inorganic resist.
- the thermal reaction type resist is composed of an incomplete oxide of an element selected from the group consisting of a transition metal and an XII group to an XV group element, and the main fluoride of the element
- An inorganic resist having a boiling point of 200 ° C. or higher is preferable.
- the transition metal in the inorganic thermal reaction type resist is Ti, Cr, Mn, Fe, Co, Ni, Cu, Zr, Nb, Rh, Ag, Hf, Ta, and Au.
- the element is preferably selected from the group consisting of:
- the group XII to group XV in the inorganic thermal reaction resist is an element selected from the group consisting of Al, Zn, Ga, In, Sn, Sb, Pb, and Bi. It is preferable that it is.
- the transition metal in the inorganic thermal reaction type resist is an element selected from the group consisting of Ti, Cr, Mn, Co, Cu, Nb, Ag, Ta, and Au
- the group XII to group XV elements are preferably elements selected from the group consisting of Sn, Pb, and Bi.
- the etching layer is made of a material selected from the group consisting of Si and Ta and oxides, nitrides and carbides thereof.
- the thermal reaction type resist layer has a thickness of ⁇ 20 nm or less within the sleeve circumference of the thickness.
- the thermal reaction type resist layer is composed of at least two layers.
- the seamless mold manufacturing method of the present invention it is preferable to further include a step of forming a heat absorption layer on and / or below the etching layer before forming the heat-reactive resist layer on the etching layer.
- the seamless mold manufacturing method of the present invention preferably further includes a step of forming the thermal insulation layer on the sleeve-shaped mold before forming the etching layer on the sleeve-shaped mold.
- the lamination method for forming the heat-reactive resist layer, the etching layer, and the heat absorption layer is performed using any one of a sputtering method, a vapor deposition method, and a CVD method. It is preferable that
- the beam shape of the laser be an elliptical shape during the exposure using the laser.
- a dry etching apparatus in which a sleeve-shaped mold and a counter electrode are arranged at positions facing the mold surface in a vacuum chamber.
- the shape of the counter electrode of the dry etching apparatus is preferably any one selected from a cylindrical shape, a parallel plate shape, and an arc shape.
- the dry etching apparatus has a function of rotating a sleeve-shaped mold around a central axis.
- the present invention since a fine pattern of 1 ⁇ m or less can be directly produced in a sleeve-shaped mold, it has a large area, excellent productivity, a high degree of freedom of uneven shape, and the aspect ratio of the fine structure can be freely controlled.
- a master mold fabrication technique for nanoimprint or optical film is provided.
- the nanoimprint and the optical film manufactured using the master mold created by the master mold production technique of the present invention can be a seamless continuous film having a fine shape pattern of 1 ⁇ m or less on the surface. Therefore, it is possible to sufficiently cope with an increase in the area of the film.
- 1 is a diagram of a dry etching apparatus that does not rotate a sleeve according to the present invention. It is the figure which showed the incident direction of the ion with respect to the sleeve by this invention. 1 is a diagram of a dry etching apparatus in which a sleeve according to the present invention is rotated. It is a figure of the dry etching apparatus at the time of applying a high frequency to the counter electrode by this invention.
- FIG. 1 It is a schematic diagram which shows an example of a structure and optical system of the exposure apparatus used for the method which concerns on this invention. It is a figure which shows the form of the sleeve mold in an Example. 2 is a cross-sectional view showing a sleeve mold in Example 1. FIG. It is sectional drawing which shows the sleeve mold in Example 2. FIG. FIG. 6 is a cross-sectional view showing a sleeve mold in Example 3. It is a schematic diagram which shows one example of the apparatus for apply
- FIG. It is the schematic which showed the example of the structure of the exposure apparatus in the comparative example 1, and an optical system.
- the intensity of the laser beam focused by the normal lens shows a Gaussian distribution shape as shown in FIG.
- the spot diameter is defined as 1 / e 2 .
- the temperature of the object when an object is irradiated with laser light having the distribution shown in FIG. 1, the temperature of the object also exhibits the same Gaussian distribution as the intensity distribution of the laser light.
- a resist that reacts at a certain temperature or higher that is, a heat-reactive resist
- the reaction proceeds only at a portion that exceeds a predetermined temperature (resist reaction temperature) as shown in FIG. The area) can be exposed. Therefore, a pattern finer than the spot diameter can be formed without shortening the wavelength of the exposure light source.
- the thermal reaction type resist the influence of the exposure light source wavelength is reduced.
- the thermal reaction type resist has a characteristic of reacting at a predetermined light intensity or higher in the light intensity distribution at the laser spot diameter, or has a region that reacts at a predetermined temperature or higher in the laser spot diameter. It has a temperature distribution that includes it.
- a DUV (Deep Ultra Violet) light source such as KrF or ArF, or an electron beam or an X-ray
- these light sources have complicated optical systems. Therefore, it is a very expensive and large facility.
- an evacuation facility is required for electron beams, X-rays, etc., it is very difficult to form a large mold with a small irradiation area.
- the parallelism of the exposure original plate is required because the depth of focus is shallow, it is possible to expose a parallel plate mold, but while maintaining high resolution in a cylindrical sleeve-shaped mold, In principle, exposure is difficult.
- a semiconductor laser that is small, inexpensive, and does not require special incidental equipment.
- a short-wavelength semiconductor laser currently on the market has a wavelength of about 405 nm and a spot diameter of about 400 nm. Therefore, microfabrication of 400 nm or less is impossible in principle as long as a photoresist is used, but this limit can be exceeded by using a heat-reactive resist.
- the feature of the present invention includes a region in which a heat-reactive resist reacts at a predetermined light intensity or higher in the light intensity distribution at the laser spot diameter or reacts at a predetermined temperature or higher in the laser spot diameter. By having a temperature distribution, it is possible to realize processing finer than the spot diameter.
- a linear pattern 4 can be formed on a film 3 or substrate as shown in FIG. 4 by using a heat-reactive resist as described above for a sleeve-shaped mold. it can. Moreover, this method has a feature that it is excellent in mass productivity.
- an electrophotographic apparatus As a technique for irradiating a semiconductor laser in a cylindrical shape, an electrophotographic apparatus, a lithographic printing plate apparatus, an image recording apparatus, and the like can be given.
- a photosensitive material is provided on a cylindrical cylinder (also called a drum) and irradiated (exposed) with a laser beam, so that the photosensitive material can be changed depending on the presence or absence of irradiation.
- a principle is used in which the amount of charge transport or retention is changed, and the toner is adsorbed and transferred to paper or the like by utilizing the difference in the charge (for example, Japanese Patent Application Laid-Open No. 2004-151519).
- the lithographic printing technology provides a photosensitive material or a heat-reactive resin on a flat plate or a cylindrical roller or sleeve, and irradiates (exposes) laser light, thereby sensitizing the photosensitive material depending on whether irradiation is performed.
- Ink that changes the affinity (hydrophilicity or oleophilicity) of the ink or changes the affinity by sublimating the photosensitive material and exposing the layer provided below it, and transferring the ink from the difference in affinity This is a method of providing a difference in the amount of adhesion (for example, JP-A-7-214744 and JP-A-10-858).
- the printing technique is a technique for transferring the presence or absence of a pattern formed on a plate, that is, transferring two-dimensional information to a medium
- the technique for shaping a nanoimprint or optical film according to the present invention is applied to a mold.
- This is a technique for transferring information on both the width and depth of a formed pattern, that is, three-dimensional information, to a medium. Therefore, the lithographic printing technique is a completely different principle from the present invention, and its intended purpose is also completely different. Further, the resolution that can be realized in the current lithographic printing is about 20 ⁇ m to 100 ⁇ m, and the resolution of 1 ⁇ m or less intended by the present invention cannot be obtained.
- the technique for shaping the nanoimprint or the optical film is a technique for transferring not only the resolution of the pattern formed on the mold but also the information in the depth direction as described above.
- printing technology transfers the two-dimensional information of the plate to the medium
- the technology for shaping the nanoimprint or the optical film is a technology for transferring the three-dimensional information of the mold to the medium, and has a completely different concept. Is.
- the method for producing a seamless mold according to the present invention comprises forming a heat-reactive resist layer on a sleeve-shaped mold and forming a fine mold pattern on the heat-reactive resist layer using a laser.
- the heat-reactive resist layer is made of a heat-reactive resist having a characteristic of reacting at a predetermined light intensity or higher in the light intensity distribution at the laser spot diameter.
- the seamless mold manufacturing method includes a seamless mold in which a heat-reactive resist layer is formed on a sleeve-shaped mold and a fine mold pattern is formed on the heat-reactive resist layer using a laser.
- the thermal reaction type resist layer is composed of a thermal reaction type resist having a temperature distribution including a region that reacts at a predetermined temperature or more in the spot diameter of the laser.
- an etching layer is formed on the sleeve-shaped mold, and the etching layer is etched using the fine mold pattern as a mask, It is preferable that the method further comprises removing the fine mold pattern.
- a method of producing a mold by forming a heat-reactive resist layer on a sleeve-shaped mold, exposing using a semiconductor laser, and developing the exposed portion (2) A method of forming a mold by forming an etching layer and a heat-reactive resist layer on a sleeve-shaped mold, exposing using a semiconductor laser, etching, and removing the heat-reactive resist layer; (3) An etching layer and a heat-reactive resist layer are formed on a sleeve-shaped mold, exposed using a semiconductor laser, the exposed portion is developed, and etched after development to remove the heat-reactive resist layer.
- the method of producing a mold is mentioned by this.
- the resist is preferably ablated by exposure and is suitable for applications requiring a relatively shallow depth. Since there is no development or etching process, the process is simple and inexpensive.
- the resist is a type that is ablated by exposure, and is suitable for applications requiring relatively deep (high aspect ratio) processing.
- the resist is preferably of a type that undergoes a phase change upon exposure or a type that chemically reacts, and is suitable for applications that require high resolution and high aspect ratio processing. However, the process is slightly complicated accordingly.
- the heat-reactive resist used in the present invention is preferably an organic resist or an inorganic resist.
- the resist layer formed by these resists may be a single layer or a multilayer structure in which several resist layers are combined.
- the type of resist to be selected can be changed as appropriate depending on the process, required processing accuracy, and the like.
- the organic resist can be applied with a roll coater or the like when it is formed on the sleeve, the process is simple. However, since it is applied onto the sleeve, there is a limit to the viscosity of the resist, and it becomes difficult to control the coating thickness and control or coat multiple layers.
- a photoresist is made of an epoxy-based or acrylate-based organic material and is applied to a substrate in a liquid state.
- a photoresist is dropped onto a wafer by a spin coater, and the resist film thickness is controlled by the viscosity of the photoresist or the rotational speed of the wafer.
- the photoresist is formed on the sleeve-shaped mold surface in the same way, the photoresist is a liquid having a certain viscosity, so that the resist film thickness is unevenly formed in the circumference according to gravity.
- Japanese Patent Publication No. 2007-507725 discloses a method in which a photoresist is sandwiched between transparent films and wound around a sleeve. In this method, the non-uniformity of the film thickness in the circumference and in the axial direction is eliminated, but a seam of the film is always generated in the circumference, so that there is a problem that the seamless mold aimed by the present invention cannot be achieved.
- a photoresist As a manufacturing problem when using a photoresist, there is an influence of exposure time. Depending on the size of the mold, the exposure of the mold takes 1 day to several days if it is long. Therefore, the resist needs to exhibit stable characteristics within a long exposure time.
- a photoresist is diluted with an organic solvent or the like in order to control its viscosity. Therefore, if the resist is left at room temperature for a long time, the organic solvent volatilizes and the exposure characteristics change. Therefore, in integrated circuit manufacturing or the like, exposure is completed promptly after resist application.
- a heat-reactive resist that is exposed by heat which is based on the premise that the solvent is volatilized by heat, is more advantageous than a light source such as a photoresist.
- a light source such as a photoresist.
- it is inferior to the inorganic resist described later in terms of film thickness uniformity.
- novolak resin or a mixture of novolak resin and diazonaphthoquine examples include methacrylate resins, polystyrene resins, polyethylene resins, phenol resins, polyimide resins, polyamide resins, silicone resins, polyester resins, epoxy resins, melamine resins, and vinyl resins.
- the heat-reactive resist material using an inorganic material such as a metal or an oxide according to the present invention can also solve the above-described problem of non-uniform film thickness.
- the resist material can be formed on the sleeve-shaped mold by using a physical thin film forming method instead of coating, so that the resist is not in a liquid state and the influence of gravity can be eliminated. It has become possible to form a resist with a uniform film thickness.
- a normal thin film forming apparatus is formed on a parallel plate base material such as a wafer, a thin film cannot be formed on the sleeve. The problem was solved by inventing a sputtering apparatus as disclosed in.
- the film thickness uniformity described so far, but how much uniformity is required depends on the required size of the microstructure. For example, since the exposure characteristics are not constant when the resist film thickness varies by several tens of ⁇ m, it is very difficult to form a fine structure with a size of 100 nm.
- the allowable resist film thickness accuracy is at least ⁇ 20 nm of the target film thickness (hereinafter sometimes referred to as “d”). Hereinafter, it is more preferably ⁇ 10 nm or less, particularly preferably ⁇ 3 nm or less.
- the variation width of the film thickness expressed by the notation is referred to as “variation width”.
- a method of rotating the sleeve during film formation is employed in order to ensure film thickness accuracy within the circumference of the sleeve. Even in the case where the sleeve is rotated, it is necessary to appropriately select the film forming speed and the sleeve rotating speed in order to ensure the film thickness accuracy. For example, when the film formation speed is high, film thickness unevenness is likely to occur if the sleeve rotation speed is low. When the film forming speed is slow, the rotational speed may be slow, but the film forming time becomes long.
- the film forming speed per one rotation of the sleeve needs to be 20 nm / rotation or less at the earliest. More preferably, it must be 10 nm / rotation or less.
- the film thickness unevenness occurs if the position at the start of film formation does not coincide with the end position.
- the deposition rate is not 0.00001 nm / rotation or more, the deposition is not completed in a realistic time.
- the rotation speed of the sleeve is roughly determined from the total number of rotations, which is the product of the film formation time. If the total number of film rotations is small, the film thickness within the circumference is affected by variations in film formation speed due to the shutter opening and closing time at the start and end of film formation, mechanical axis blurring of the sleeve rotation axis, or temperature fluctuations during film formation. Uniformity decreases. In order to solve this problem, the variation can be reduced by increasing the total number of revolutions during film formation to average the film formation speed fluctuation.
- the film thickness variation factor per rotation can be reduced to 1/100, so that the influence on the film thickness accuracy can be suppressed to 1%.
- the total number of rotations from the start to the end of film formation varies depending on the film formation speed fluctuation factors such as the shutter structure of the film formation apparatus, the opening / closing time, or the sleeve rotation axis accuracy, but it is desirable that at least 500 rotations or more can be secured. More preferably, it is 1000 rpm or more. On the other hand, if the total number of rotations is not less than 1 million, for example, even if the sleeve is rotated at 1000 rpm, it takes about 16 hours for the film formation time, which is not realistic.
- Thermal resists using inorganic materials such as metals and oxides have extremely stable chemical and physical properties at room temperature, and use organic solvents because they are formed using physical thin film formation methods. Therefore, even with long-term exposure, the characteristics are very stable without changing the properties.
- the inorganic thermal reaction resist is preferably formed by a physical thin film formation method such as a resistance heating vapor deposition method, a magnetron high frequency sputtering method, an electron beam sputtering method, or a CVD method. Since these methods are basically vacuum processes, it takes more man-hours to form on the sleeve than the coating method. However, as described above, the film thickness can be controlled with high accuracy, and further, the resist layer and etching are performed. It is also easy to stack the layers in multiple layers.
- a physical thin film formation method such as a resistance heating vapor deposition method, a magnetron high frequency sputtering method, an electron beam sputtering method, or a CVD method. Since these methods are basically vacuum processes, it takes more man-hours to form on the sleeve than the coating method. However, as described above, the film thickness can be controlled with high accuracy, and further, the resist layer and etching are performed. It is also easy to stack the layers in multiple layers.
- the inorganic heat-reactive resist material suitable for the present invention can be variously selected depending on the reaction temperature. Examples thereof include Al, Si, P, Ni, Cu, Zn, Ga, Ge, As, Se, In, Sn, Sb, Te, Pb, Bi, Ag, Au, and alloys thereof.
- the inorganic thermal reaction type resist material particularly suitable for the present invention is preferably an incomplete oxide with an element selected from the group consisting of transition metals and XII to XV group elements.
- incomplete oxide refers to an element selected from the group consisting of transition metals and XII to XV elements, which contains more oxygen than an oxide having a stoichiometric composition according to the valence that the element can take. A state where the amount is insufficient.
- one element can form oxides with different valences.
- a state in which the oxygen content is insufficient as compared with the oxide having the stoichiometric composition corresponding to the valence is also regarded as the incomplete oxide of the present invention.
- the element valence and oxygen content can be analyzed by, for example, a fluorescent X-ray analyzer.
- the inorganic heat-reactive resist material of the present invention is composed of an incomplete oxide and has high resistance to dry etching using a chlorofluorocarbon gas.
- the thermal reaction type resist material when it is desired to form a pattern in which the depth of the groove is increased along with the fine pattern shape, it is difficult to use the thermal reaction type resist material alone, and an etching layer is formed under the thermal reaction type resist material. A laminated structure is required. In this case, while the lower etching layer is dry-etched, the heat-reactive resist material functioning as a mask is required to have high dry etching resistance. In other words, it is important that the heat-reactive resist material of the present invention has a low etching rate or is not etched in a dry etching process using a fluorocarbon gas.
- fluorine activated in the vacuum chamber of the dry etching apparatus combines with the elements used in the resist to form fluoride.
- the fluoride has a relatively high vapor pressure (ie, when the fluoride has a relatively low boiling point)
- the fluoride vaporizes and disappears from the resist material, resulting in etching.
- the vapor pressure of the fluoride is relatively low (that is, when the boiling point of the fluoride is relatively high)
- the etching rate is slow or not etched because vaporization is difficult.
- the present inventors have selected, as a heat-reactive resist material, an element in which the boiling point of the main fluoride of the element is 200 ° C. or higher among transition metals and XII to XV elements.
- the resist material exhibits high resistance to dry etching treatment using a chlorofluorocarbon gas, and the effect was confirmed.
- the boiling point of the main fluoride of the element constituting the heat-reactive resist material according to the present invention is about 200 ° C. or more, more preferably about 250 ° C. or more, further preferably about 700 ° C. or more, and most preferably about 950 ° C. That's it. As the boiling point of fluoride increases, the resistance to dry etching using a fluorocarbon gas increases. Table 1 below shows boiling points of main fluorides of elements constituting the heat-reactive resist material according to the present invention.
- an optical material, a film, or the like is required to have an aspect ratio (a value obtained by dividing the groove depth by the groove opening width) of at least 1, preferably 2 or more, and more preferably 3 or more. .
- the ability to freely select the aspect ratio increases the degree of freedom in optical design. Accordingly, it is essential that the heat-reactive resist material according to the present invention has high resistance to dry etching.
- the heat-reactive resist material has an etching resistance of about three times or more the etching resistance of the etching layer.
- the heat-reactive resist material functions as a mask for forming a deep groove, the etching layer can be etched, and a deep pattern shape of the groove can be formed. It becomes possible to form.
- the element used in the heat-reactive resist material according to the present invention is one or more elements selected from elements having transition metal and XII to XV elements whose main fluoride has a boiling point of 200 ° C. or higher.
- transition metals Ti, Cr, Mn, Fe, Co, Ni, Cu, Zr, Nb, Rh, Ag, Hf, Ta, Au, and for XII to XV group elements, Al, Zn, Ga, In, Sn, Sb, Pb, Bi.
- the transition metal includes Ti, Cr, Mn, Co, Cu, Nb, Ag, Ta, and Au
- the XII to XV group elements include Sn, Pb, and Bi.
- the resist layer subjected to the same treatment can be used in the heat-reactive resist material as compared with the etching layer subjected to the dry etching treatment with the fluorocarbon gas. It has a dry etching resistance of about 3 times or more.
- Ti, Cr, Nb, Ta, and Sn are particularly preferable elements.
- the boiling points of the main fluorides of the elements W, Mo, As, and S constituting the heat-reactive resist material reported so far are as low as 17 ° C., 35 ° C., 63 ° C., and ⁇ 64 ° C., respectively. It cannot function as an element of the heat-reactive resist material according to the present invention having high dry etching resistance (International Publication No. 2004-064057, The 19th Symposium Phase Phase Change Optical Information Storage (2007) p77).
- an etching layer 6 is formed on a cylindrical mold 5 and a resist layer 7 is formed on the etching layer 6 as a semiconductor laser sleeve-shaped irradiated body in the method of the present invention.
- the etching layer 6 is formed on the cylindrical mold 5
- the heat absorption layer 8 is formed on the etching layer 6
- the resist layer 7 is formed on the heat absorption layer 8.
- the thermal insulating layer 9 is formed on the cylindrical mold 5
- the etching layer 6 is formed on the thermal insulating layer 9, and the resist layer 7 is formed on the etching layer 6.
- the heat absorption layer 8 in FIG. 6 may be disposed under the etching layer 6.
- the processing depth of the pattern can be freely controlled, and the thickness of the heat-reactive resist layer can be selected to an optimum thickness for processing. become.
- the processing depth can be freely controlled by controlling the thickness of the etching layer.
- the heat-reactive resist layer may be selected to have a thickness that can be easily exposed and developed.
- the material used for the etching layer in the present invention is a semiconductor material such as Si, polysilicon, GaAs or InP, a metal such as Al, Cu, W, Ti, Ta, or their oxidation.
- Suitable materials are nitrides, nitrides, carbides, alloys thereof, insulating materials such as SiO 2 , Si 3 N 4 , glass, silicide materials such as WSi 2 , TiS 2 , and CoSi 2 , and organic materials such as polyfluoroethylene, PMMA, and PC It is.
- materials selected from the group consisting of Si, Ta and oxides, nitrides and carbides thereof are preferable, and semiconductors and insulating materials such as SiO 2 , Si, Si 3 N 4 and Ta 2 O 5 are particularly preferable. It is.
- the roles of the etching layer and the thermal reaction resist are the same as those in FIG.
- the role of the heat absorption layer is to widen the selection range of light absorption characteristics in the heat-reactive resist.
- the thermal reaction resist has many materials that absorb in a wide wavelength range, but some materials do not have optical absorption near the wavelength of the semiconductor laser, for example, around 405 nm. In that case, the heat-reactive resist can be reacted with the heat by absorbing the energy of the semiconductor laser in the heat absorption layer and converting it into heat.
- a material used for the heat absorption layer in the present invention a material having light absorptivity in the wavelength region of the semiconductor laser is suitable.
- C Mg, Al, Si, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ge, Se, Zr, Nb, Mo, Pd, Ag, In, Sn, Sb, Te, Hf, Ta, W, Pt, Au, Pb, Bi, and alloys thereof may be mentioned.
- Oxides, nitrides, sulfides, carbides or a mixture thereof may be used.
- the irradiated object shown in FIG. 7 has an effect of preventing the dissipation of thermal energy in the portion heated by the semiconductor laser irradiation.
- the sleeve material is made of metal, glass, or the like, which is rich in workability.
- metal and glass have a higher thermal conductivity than materials such as plastic, a phenomenon occurs in which the thermal energy of the portion heated by irradiation with the semiconductor laser escapes to the sleeve side. Therefore, in order to raise the temperature of the exposed portion to the reaction temperature of the heat-reactive resist, a semiconductor laser with a larger output is required. Increasing the output of a semiconductor laser is not preferable because it leads to an increase in the size of optical components and a reduction in laser life.
- thermo insulating layer on the sleeve, heat dissipation can be prevented and the energy of the semiconductor laser can be used more efficiently.
- a material such as acrylic is preferable as a material used for the heat insulating layer.
- the inorganic thermal reaction type resist layer and the etching layer are preferably formed by a sputtering method.
- the method for forming the inorganic thermal reaction type resist layer various methods are conceivable as described above, and the sputtering method is most preferable in consideration of the uniformity of the film composition, the film thickness control, the productivity, and the like.
- the sputtering method is preferable among the vapor phase film formation.
- the conventional sputtering apparatus since the conventional sputtering apparatus is manufactured on the premise that the film is formed on a parallel plate such as a Si wafer or a glass substrate, it cannot be directly applied to the sleeve-shaped mold in the present invention. Therefore, in order to suitably use the present invention, a sputtering apparatus as shown in FIG. 8 was newly developed, which is suitable for applying a heat-reactive resist to a sleeve-shaped mold.
- the sputtering apparatus shown in FIG. 8 mainly includes a load lock chamber 11 for loading an object to be processed, and a chamber 13 connected to the load lock chamber 11 via a valve 12.
- a target 14 is disposed in the chamber 13, and a sleeve mold 15 is installed so as to face the target 14.
- the sleeve mold 15 is installed so as to be erected, and is rotated in the direction of the arrow.
- a vacuum pump 17 is connected to the chamber 13 via a valve 16 so as to depressurize the inside of the chamber 13.
- the chamber 13 is connected to a discharge gas supply unit 18 that supplies a discharge gas such as Ar gas and a reaction gas supply unit 19 that supplies a reaction gas.
- a power source 21 is connected to the target 14 via a matching circuit 20.
- the inside of the chamber 13 is decompressed by the vacuum pump 17 and the sleeve mold 15 is rotated.
- the discharge gas is supplied from the discharge gas supply unit 18, the reaction gas is supplied from the reaction gas supply unit 19, and the power is turned on, sputtering is performed on the sleeve mold 15.
- a target may be installed in each of a plurality of chambers, and a resist layer may be continuously formed in multiple layers. Thereby, it can avoid exposing a to-be-processed object to air
- the conventional dry etching apparatus is manufactured on the premise that the film is formed or etched on a parallel plate such as a Si wafer or a glass substrate, and therefore cannot be applied as it is to the sleeve-shaped mold in the present invention. .
- the normal dry etching apparatus generates plasma by applying the high frequency 21 to the substrate 10 placed on the stage 26 by introducing the etching gas 25 with the vacuum chamber 13 in a reduced pressure state.
- the principle of dry etching is that etching gas molecules are ionized or radicalized by plasma and etched by chemical or physical reaction with the substrate.
- the characteristic of dry etching is that etching anisotropy is easily obtained as compared with wet etching.
- etching proceeds by immersing the substrate in an etchant. Therefore, as shown in FIG. 10, the substrate is isotropically etched because the etching layer 6 provided under the resist layer 7 has no directionality.
- dry etching accelerates ions by an electric field applied between the substrate 10 and the counter electrode 22 so that the ions collide with the surface in a direction perpendicular to the substrate, thereby reacting with the substrate. Etching proceeds. Therefore, as shown in FIG. 11, the etching layer 6 is etched in the direction perpendicular to the substrate surface.
- the present invention it is necessary to etch a substrate having a curved surface, for example, a roll or an arc-shaped mold, in a direction perpendicular to the tangent to the mold surface from the mold surface toward the central axis.
- a substrate having a curved surface for example, a roll or an arc-shaped mold
- the sleeve-shaped mold 15 and the surface of the mold are placed in a vacuum chamber.
- the dry etching apparatus has a configuration in which a cylindrical counter electrode 22 is disposed at an opposing position. The outline of the apparatus is shown in FIG.
- the mold surface is located between the mold and the electrode from the mold surface toward the central axis.
- a uniform electric field is formed in a direction perpendicular to the tangential direction. Accordingly, a stable plasma is formed along the mold surface.
- a potential called a sheath potential is generated between the plasma and the mold so as to wrap the mold, and an electric field perpendicular to the mold is generated.
- etching gas ions are accelerated along this electric field, and etching proceeds in a direction perpendicular to the tangent to the mold surface from the mold surface toward the central axis. .
- FIG. 12 Another feature of the apparatus shown in FIG. 12 is that it is not necessary to rotate the mold during the etching process. In order to apply a high frequency to the rotating mold, it is necessary to adopt a method in which electricity flows simultaneously with the rotating mechanism. Therefore, the structure of the coupler 23 is complicated, but in this method, it is not necessary to rotate the mold. Becomes easier.
- the etching rate may vary due to unevenness of the gas flowing through the mold or variation in the distance between the mold and the electrode.
- the sleeve-shaped mold 15 is rotated around its central axis via the motor 24 and the coupler 23 during the etching process. be able to.
- the shape of the counter electrode is not limited to the cylindrical shape, but also an arc shape, a parallel plate Shapes can also be used.
- FIG. 14 shows an apparatus in which the counter electrode has a cylindrical shape.
- the coupler 23 that holds the mold needs to be designed to have both a rotation mechanism and a high-frequency transmission mechanism.
- the circuit configuration is such that a high-frequency is applied to the electrode side and the mold side is grounded.
- the design of the coupler 23 is not complicated (FIG. 15).
- the etching apparatus can of course etch an etching layer formed on a sleeve-shaped mold, and can also perform etching by forming an etching layer and a resist layer on the mold surface. .
- the etching gas suitable for the present invention may be selected variously according to the resist and the material to be etched, and is not limited at all.
- CF 4 , CHF 3 , C 2 F 6 , C 3 F 8 , C 4 F 8 , C 5 F 8 , CH 2 F 2 , CCl 2 F 2, etc. or a mixture of these gases with a gas such as Ar, O 2 , H 2 , N 2 , CO, etc., or HBr, NF 3 , SF 6 , CF 3 Br, HBr, Cl 2 , HCl, HI, BBr 3 , BCI 3 , CI 2 , SiCl 4 mixed gas, and Ar, O 2 , H 2 , N 2 , CO, etc.
- a mixture of gases may be used.
- the etching direction can also be controlled by optimizing the conditions such as the type, composition, and etching temperature of the etching gas.
- a groove having the same width toward the central axis direction of the mold can be manufactured, or a V-shaped groove whose width becomes narrower toward the central axis direction can be manufactured.
- FIG. 16 is a view showing an exposure apparatus for exposing the resist layer formed on the sleeve mold in the method according to the present invention.
- This exposure apparatus adopts a configuration in which light is irradiated through an optical system 33 to a sleeve mold 32 rotated by a spindle motor 31.
- the laser light emitted from the semiconductor laser 331 for exposure is sent to the objective lens 333 through the mirror 334 as parallel light by the collimator 332.
- laser light emitted from the semiconductor laser 335 for focusing is sent to the objective lens 333 through the dichroic mirror 337 as parallel light by the collimator 336.
- the light collected by the objective lens 333 is irradiated to the sleeve mold 32.
- the laser light emitted from the semiconductor laser 335 for focusing is changed in optical path by the dichroic mirror 337, condensed by the condenser lens 338, and detected by the photodetector 339.
- the optical system 33 is configured to move in the long axis direction of the sleeve mold 32, so that the end portion of the sleeve mold 32 can be exposed. In addition, by shifting the position of the head of the optical system 33 in accordance with the rotation of the sleeve mold 32, a seamless mold without a joint can be produced. Further, since the objective lens 333 of the semiconductor laser has a focus servo that follows the fluctuation of the sleeve mold 32, the amount of light emitted from the semiconductor laser can be controlled to be constant. This focus servo may follow up / down movement, follow up left / right fluctuations, or may have both mechanisms. Also, as shown in FIG. 16, in order to stabilize the servo, by using a focus semiconductor laser 335 having a wavelength different from that of the exposure semiconductor laser 331, the exposure semiconductor laser 331 has servo characteristics. It is also possible to make it less susceptible to fluctuations.
- the output light amount of the semiconductor laser is monitored by the photodetector 339 and feedback control is performed, so that the output can be stabilized according to the output light amount.
- a plurality of semiconductor lasers 331 for exposure may be used and a plurality of optical systems 33 may be provided in order to improve the exposure speed.
- the beam shape of the semiconductor laser can be variously selected depending on the shape formed on the mold.
- the beam shape of the semiconductor laser is also preferably circular.
- the semiconductor laser beam shape is made elliptical and the major axis of the elliptical sleeve is used to avoid thermal interference during adjacent exposure. It is good to arrange in the direction perpendicular to the major axis.
- the long axis of the elliptical semiconductor laser beam is arranged parallel to the long axis of the sleeve. It is preferable.
- the fine shape formed on the mold in the present invention can form various shapes.
- the fine shape manufacturing method according to the present invention is a method that has a remarkably high degree of freedom of fine shapes that can be formed in a mold as compared with conventional methods.
- the hole shape in the case of continuous production, if the hole shape is nearly vertical, there will be a problem that the resin transferred to the mold will fall out, so it is also necessary that the hole shape be a tapered shape with a certain angle. is there. Furthermore, in the field of optical films, for example, a film having a grid structure in which the fine shape is a groove shape may be required.
- the transfer mold must be formed by a method capable of forming at least a fine pattern with a high degree of freedom in the uneven shape.
- the above-mentioned problem can be solved by using a mask on which a pattern is drawn in advance in the method using a parallel plate mold for the conventional original plate.
- a seam is always generated somewhere in the film, so that it does not become a continuous product and the productivity is significantly reduced. It was.
- the mold In order to produce such a fine film with a high degree of freedom in the uneven shape and a seamless film, the mold itself has both a fine shape with a high degree of freedom and a seamless seamless pattern. There was a need.
- the mold produced according to the present invention has a high degree of freedom in concave and convex shapes and is seamless and seamless, so it can be used for films having various shapes compared to conventional methods, and has a significantly higher productivity. It has characteristics such as high.
- thermoplastic film or a base film is transferred to a seamless sleeve by pressing a film coated with a thermoplastic resin in a heated state, or a so-called thermal nanoimprint method or a base film having low viscosity.
- a film coated with UV curable resin is pressed against the seamless sleeve and cured by UV light, so-called UV imprinting, and a dry film resist that is laminated with a semi-cured UV curable resin is pressed against the seamless sleeve to make it fine
- UV imprinting so-called UV imprinting
- the transfer target may not be a film.
- a method using a parallel plate mold or a method of winding a thin film mold into a sleeve mold can synchronize the mold seam and the plate length. It is possible to produce without seams. However, it is necessary to change the mold in order to adjust the position of the seam whenever the length of the plate to be produced changes. On the other hand, in the case of a seamless mold, it is not necessary to replace any size plate, and it is also possible to continuously produce plates of different lengths on the same line.
- a seamless mold having a fine shape formed on the surface which is produced by the seamless mold production method of the present invention. Further, by producing a film using the seamless mold, it is possible to produce a seamless film having a fine uneven pattern on the surface. Furthermore, the film produced by film production using the seamless mold is cut into an appropriate size by the user, and becomes a film having a fine concavo-convex pattern with no waste of material and high yield. In producing a member having a fine structure of 1 ⁇ m or less on the surface, it is preferable to use a seamless mold having a surface fine shape size of 1 ⁇ m or less.
- the seamless mold by producing a film using the seamless mold, it is possible to produce a seamless film having a fine uneven pattern on the surface. Furthermore, the film produced by film production using the seamless mold is cut into an appropriate size by the user, and becomes a film having a fine concavo-convex pattern with no waste of material and high yield.
- Example 1 As shown in FIG. 17, a metal sleeve 41 processed to ⁇ 30 mm and ⁇ 58 mm was prepared, and an acrylic pipe 42 having a length of 200 mm, an inner diameter of ⁇ 58 mm, and an outer diameter of ⁇ 60 mm was attached to the outer side to constitute a cylindrical sleeve. .
- the acrylic pipe plays the role of a heat insulation layer.
- a resist layer 43 was formed on the sleeve 41 via the acrylic pipe 42.
- sputtering was performed while rotating the sleeve during sputtering.
- the fluctuation width was ⁇ 3 nm or less with respect to the target thickness (d) of 40 nm.
- SnOx was used as the thermal reaction type inorganic resist.
- a Sn target was attached to the sputtering apparatus, and sputtering was performed in a mixed gas atmosphere of Ar and O 2 .
- the oxidation amount of Sn was changed by the mixing ratio of Ar and O 2 .
- Table 2 The results are shown in Table 2 below. From this result, the oxidation amount of Sn can be a value of 0 ⁇ x ⁇ 2.
- the value of x was determined from the peak ratio between Sn and SnO 2 by X-ray fluorescence.
- the sleeve thus prepared was exposed using an exposure apparatus shown in FIG. 16 (exposure apparatus having two types of exposure lasers and focusing lasers having different wavelengths).
- the exposure conditions are as follows.
- the sleeve exposure width is set to 200 mm. However, if the exposure width is widened, the exposure time only becomes longer. With this exposure apparatus, exposure can be performed without any problem even if the exposure width is longer than that used in the experiment. it can.
- the resist exposed by the exposure apparatus was developed.
- development by a wet process was applied.
- An acid, an alkali, or the like can be used as the developer, but here, a tetramethylammonium aqueous solution (TMAH) was used.
- TMAH tetramethylammonium aqueous solution
- a bath of 2.38% TMAH solution at 25 ° C. was prepared, and development was performed by immersing a sleeve in this bath.
- the development time varies depending on the oxidation amount of Sn, but is preferably about 1 to 5 minutes.
- the development is performed by immersing the sleeve.
- the developer may be sprayed or dropped onto the sleeve for development.
- Example 2 As shown in FIG. 17, a metal sleeve 41 processed to ⁇ 30 mm and ⁇ 58 mm was prepared, and an acrylic pipe 42 having a length of 200 mm, an inner diameter of ⁇ 58 mm, and an outer diameter of ⁇ 60 mm was attached to the outer side to constitute a cylindrical sleeve. .
- the acrylic pipe plays the role of a heat insulation layer.
- an etching layer 44 was formed on the sleeve 41 via the acrylic pipe 42, and a resist layer 43 was formed on the etching layer 44.
- sputtering was performed while rotating the sleeve during sputtering.
- a SiO 2 film was used as the etching layer 44.
- a SiO 2 target was attached to the sputtering apparatus, and sputtering was performed in an Ar gas atmosphere.
- the sleeve thus prepared was exposed using an exposure apparatus shown in FIG.
- the exposure conditions were the same as in Example 1 except that only the exposure laser power was changed to 8 mW.
- the resist was developed with a TMAH solution.
- the development conditions were the same as in Example 1.
- the etching layer 44 was etched using the etching apparatus shown in FIG. During the etching, the sleeve was rotated so that the sleeve was uniformly etched. CF 4 gas was used as an etching gas. Etching conditions are as follows. Etching power: 150W Etching gas pressure: 10 Pa Gas flow rate: 20sccm
- the sleeve was washed to remove (peel) the resist.
- a wet process was employed for resist stripping.
- various acids and alkalis can be applied as in the case of the developer.
- potassium hydroxide (KOH) was used.
- the sleeve was immersed in a 1M KOH solution for about 5 minutes. As a result, the resist was peeled cleanly with the SiO 2 layer remaining.
- the sleeve was washed and the surface shape of the sleeve mold was observed with an SEM (scanning electron microscope). As a result, a fine groove having a depth of 100 nm and a width of about 100 nm was formed on the sleeve.
- SEM scanning electron microscope
- Example 3 As shown in FIG. 17, a metal sleeve 41 processed to ⁇ 30 mm and ⁇ 60 mm was prepared, and a cylindrical sleeve similar to that in Example 1 was configured.
- an etching layer having a thickness of 200 nm was formed on the sleeve prepared as described above using a sputtering apparatus as shown in FIG.
- a SiO 2 film was used as the etching layer 44.
- a SiO 2 target was attached to the sputtering apparatus, and sputtering was performed in an Ar gas atmosphere.
- a thermal reaction type organic resist layer 43 having a thickness of 0.5 ⁇ m was formed on the etching layer 44 of the sleeve.
- the apparatus shown in FIG. 21 is an apparatus that rotates the sleeve after the chuck 53 that holds the sleeve 52 is lifted and lowered by the motor 54 to be immersed in the resist solution contained in the resist bottle 51 and pulled up.
- a thermal reaction type organic resist was applied to the sleeve.
- the resist could be uniformly applied to the sleeve surface.
- a novolac resist having a viscosity of 700 cps was used as the thermal reaction type organic resist.
- an etching layer 44 was formed on the sleeve 41 and a resist layer 43 was formed on the etching layer 44 as shown in FIG.
- the sleeve thus prepared was exposed using an exposure apparatus shown in FIG.
- the exposure conditions were the same as in Example 1 except that the exposure laser power was 4 mW and the feed pitch was changed to 500 nm / rotation. After exposure, the resist was developed with a TMAH solution, and the development time was 1 minute.
- the etching layer 44 was etched using the etching apparatus shown in FIG. During the etching, the sleeve was rotated so that the sleeve was uniformly etched. CF 4 gas was used as the etching gas. Etching conditions were the same as in Example 2.
- the sleeve was washed to remove (peel) the resist.
- a wet process was employed for resist stripping.
- the resist stripper various acids and alkalis can be applied as in the case of the developer. Here, 1M nitric acid was used.
- the sleeve was washed and the surface shape of the sleeve mold was observed with an SEM (scanning electron microscope). As a result, fine grooves having a depth of 200 nm, a width of 300 nm, and a pitch of 500 nm were formed on the sleeve. .
- SEM scanning electron microscope
- Example 4 A metal round bar 41 processed to ⁇ 30 mm and ⁇ 78 mm was prepared, and an aluminum pipe 45 having a length of 200 mm, an inner diameter of ⁇ 78 mm, and an outer diameter of ⁇ 80 mm was attached to the outside thereof to constitute a cylindrical sleeve mold as shown in FIG. .
- an etching layer 44 was formed on the sleeve prepared as described above using a sputtering apparatus capable of sputtering the sleeve as shown in FIG.
- the etching layer was sputtered with Ar gas using a SiO 2 target.
- the thickness of the etching layer was 300 nm.
- a thermal reaction type inorganic resist layer 43 was formed.
- SnOx was used as the thermal reaction type inorganic resist.
- the oxidation amount of Sn can take a value of 0 ⁇ X ⁇ 2.
- the thickness (d) of the heat-reactive inorganic resist layer 43 was 40 nm, and was formed on the sleeve.
- FIG. 23 shows a cross-sectional view of the sleeve after the thermal reaction type inorganic resist is formed. That is, the etching layer 44 and the inorganic resist layer 43 are provided on the aluminum pipe 45 on the mold 41.
- the sleeve thus prepared was exposed with an exposure machine as shown in FIG.
- This exposure apparatus is equipped with two types of processing lasers and focusing lasers having different wavelengths.
- the optical system of the exposure apparatus is also shown in FIG.
- the exposure conditions are as follows.
- Semiconductor laser wavelength for processing 405 nm
- Lens numerical aperture 0.85
- Processing laser power 5mW-8mW
- Semiconductor laser wavelength for focusing 660 nm
- Focus laser power 0.2mW
- Rotation speed 700rpm
- Feed pitch 400 nm / rotation Sleeve exposure width: 200 mm
- the shape to be formed may be an isolated circular or elliptical shape depending on the intended application, and the present invention is not limited by the processing shape.
- the sleeve processing width is set to 200 mm. However, if the processing width is increased, only the processing time becomes longer. Even with a processing width longer than that used in the experiment, the exposure apparatus can be processed without any problem.
- TMAH tetramethylammonium aqueous solution
- the etching layer was etched with a dry etching apparatus as shown in FIG.
- the dry etching apparatus performed etching by a method that does not rotate the sleeve during etching.
- O 2 + CHF 3 (1:10) gas was used as the etching gas.
- Etching conditions are as follows. Etching power: 150W Etching gas pressure: 10 Pa Gas flow rate: 20sccm High frequency frequency: 13.56 MHz
- the sleeve was washed and the resist was removed (peeled).
- a wet process was employed for resist stripping.
- Potassium hydroxide (KOH) was used as the resist stripping solution. When immersed in a KOH solution having a concentration of 1M for about 5 minutes, the resist peeled cleanly with the SiO 2 layer remaining.
- the sleeve thus etched was washed, and the surface shape of the sleeve mold was observed with an SEM (scanning electron microscope). Been formed.
- Example 5 A metal round bar processed to ⁇ 30 mm and ⁇ 78 mm was prepared, and an aluminum pipe having a length of 200 mm, an inner diameter of ⁇ 78 mm, and an outer diameter of ⁇ 80 mm was attached to the outside thereof to form a cylindrical sleeve mold similar to that in Example 4.
- etching layer was formed on the sleeve prepared as described above by a sputtering apparatus in the same manner as in Example 4, and then a thermal reaction resist was formed.
- sputtering was performed while rotating the sleeve during sputtering.
- the etching layer was made of SiO 2 and the film thickness was 100 nm.
- the sleeve prepared as described above was exposed under the same exposure conditions as in Example 4. After the exposure, the resist was developed with a TMAH solution. The development conditions were the same as in Example 4. After the development, the etching layer was etched with a dry etching apparatus as shown in FIG. The dry etching apparatus was performed while rotating the sleeve so that the sleeve could be etched uniformly. O 2 + CHF 3 (1:10) gas was used as the etching gas. Etching conditions are as follows. Etching power: 150W Etching gas pressure: 10 Pa Gas flow rate: 20sccm High frequency frequency: 13.56 MHz
- the sleeve was washed and the resist was removed (peeled).
- a wet process was employed for resist stripping.
- As the resist stripping solution various acids and alkalis can be applied as in the case of the developing solution.
- potassium hydroxide (KOH) is used as the resist stripping solution.
- KOH potassium hydroxide
- the sleeve was washed to complete the master sleeve.
- the surface shape of the sleeve mold was observed with an SEM (scanning electron microscope), a groove having a depth of about 100 nm and a width of about 100 nm was formed on the sleeve.
- SEM scanning electron microscope
- Example 6 The same metal sleeve processed into ⁇ 30 mm and ⁇ 78 mm as in Example 4 was prepared to constitute a cylindrical sleeve.
- a heat-reactive inorganic resist layer was formed.
- an etching layer was formed on the sleeve, and a resist layer was formed on the etching layer.
- sputtering was performed while rotating the sleeve during sputtering.
- a SiO 2 film was used as the etching layer.
- a SiO 2 target was attached to the sputtering apparatus, and sputtering was performed in an Ar gas atmosphere.
- the sleeve thus prepared was exposed using an exposure apparatus shown in FIG.
- the exposure conditions were the same as in Example 4 except that only the exposure laser power was changed to 3 mW.
- the resist was developed with a KOH solution.
- the etching layer 44 was etched using the etching apparatus shown in FIG. During the etching, the sleeve was rotated so that the sleeve was uniformly etched. CHF 3 gas was used as an etching gas. Etching conditions are as follows. Etching power: 150W Etching gas pressure: 10 Pa Gas flow rate: 20sccm
- the sleeve was washed to remove (peel) the resist.
- a wet process was employed for resist stripping.
- various acids and alkalis can be applied as in the case of the developer.
- the sleeve was immersed in a TMAH solution having a concentration of 2.38% for about 5 minutes. As a result, the resist was peeled cleanly with the SiO 2 layer remaining.
- the sleeve was washed and the surface shape of the sleeve mold was observed with an SEM (scanning electron microscope). As a result, a fine groove having a depth of 100 nm and a width of about 100 nm was formed on the sleeve.
- SEM scanning electron microscope
- Example 7 The same metal sleeve processed into ⁇ 30 mm and ⁇ 78 mm as in Example 4 was prepared to constitute a cylindrical sleeve.
- a SiO 2 film was used as the etching layer.
- a SiO 2 target was attached to the sputtering apparatus, and sputtering was performed in an Ar gas atmosphere.
- Cr 1-x O x , Nb 1-x O x , Ta 1-x O x , and Ti 1-x O x were used as the thermal reaction type inorganic resist. Table 3 shows the film forming conditions of each material.
- the sleeve thus prepared was exposed using an exposure apparatus shown in FIG.
- the exposure conditions were the same as in Example 4 except that the exposure laser power was changed to be optimal for each resist.
- each resist was developed under the conditions shown in Table 4.
- the etching layer 44 was etched using the etching apparatus shown in FIG. During the etching, the sleeve was rotated so that the sleeve was uniformly etched. CF 4 gas was used as an etching gas.
- Etching conditions are as follows. Etching power: 150W Etching gas pressure: 10 Pa Gas flow rate: 20sccm
- the sleeve was washed and the surface shape of the sleeve mold was observed with an SEM (scanning electron microscope). As a result, a fine groove having a depth of 100 nm and a width of about 100 nm was formed on the sleeve.
- SEM scanning electron microscope
- Example 1 A metal round bar processed to ⁇ 30 mm and ⁇ 78 mm was prepared, and an aluminum pipe having a length of 200 mm, an inner diameter of ⁇ 78 mm, and an outer diameter of ⁇ 80 mm was attached to the outside thereof to form a cylindrical sleeve mold similar to that in Example 4.
- An etching layer 44 was first formed on the sleeve prepared as described above using the same sputtering apparatus as in Example 4.
- SiO 2 was used as in Example 5.
- Sputtering was performed with Ar gas using a SiO 2 target.
- the thickness of the etching layer was 1 ⁇ m.
- FIG. 24 shows a cross-sectional view of the sleeve manufactured by the above method. That is, the etching layer 45 and the organic resist layer 43 are provided on the aluminum pipe 45 on the mold 41.
- the sleeve thus prepared was exposed with an exposure machine as shown in FIG.
- the present exposure machine has a function of attaching and rotating a sleeve 64 to a spindle motor 65, and a function of moving it forward, backward, left and right by an XY stage 66.
- the light emitted from the blue laser light source 61 is condensed on the sleeve surface by the lens 63 through the pinhole slit 62.
- the present exposure apparatus does not have an autofocus function, the spot diameter varies during rotation due to rotational shaft blurring and sleeve processing errors.
- Expoding pitch 50 ⁇ m / rotation Processing width: 22 ⁇ m
- a step of removing (stripping) the resist by ashing with O 2 gas was performed using a method of applying a high frequency to the counter electrode with the same etching apparatus.
- the sleeve was washed to complete the sleeve mold.
- grooves having a depth of 1 ⁇ m, a width of 22 ⁇ m, and a pitch of 50 ⁇ m were formed on the sleeve.
- various exposure conditions were examined using this method, a submicron size structure having a width of 1 ⁇ m or less could not be formed on the sleeve.
- Example 2 The same metal sleeve processed into ⁇ 30 mm and ⁇ 78 mm as in Example 4 was prepared to constitute a cylindrical sleeve.
- a SiO 2 film was used as the etching layer.
- a SiO 2 target was attached to the sputtering apparatus, and sputtering was performed in an Ar gas atmosphere.
- the thermal reaction type inorganic resist an element W having a boiling point of the main fluoride of 200 ° C. or less was selected, and WOx was used as the thermal reaction type resist. Table 3 shows the film forming conditions.
- the sleeve thus prepared was exposed using an exposure apparatus shown in FIG.
- the exposure conditions were the same as in Example 4 except that the exposure laser power was changed to be optimal for the WOx resist.
- the WOx resist was developed under the conditions shown in Table 4.
- the etching layer 44 was etched using the etching apparatus shown in FIG. Etching was performed under the same conditions as in Example 7. After etching, when the shape and cross-sectional shape of the roll surface were observed with an SEM (scanning electron microscope), the resist disappeared and a clear uneven pattern was not observed. This is presumably because the heat-reactive resist did not perform the mask effect because it was volatilized as fluoride by dry etching.
- the present invention can be applied to the production of seamless molds for nanoprints and optical films that are large and capable of forming fine shapes.
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Abstract
Description
通常レンズで絞り込まれたレーザー光の強度は、図1に示すようなガウス分布形状を示す。このときスポット径は1/e2で定義される。一般的にフォトレジストの反応は、E=hν(E:エネルギー、h:プランク定数、ν:波長)で表されるエネルギーを吸収することよって反応が開始される。したがって、その反応は、光の強度には強く依存せず、むしろ光の波長に依存するため、光の照射された部分(露光部分)は、ほぼ全て反応が生じることになる。このため、フォトレジストを使った場合は、スポット径に対して忠実に露光されることになる。これは、露光精度を重視する半導体等の分野では良い特性と言える。
一般にフォトレジストは、その粘性を制御するために有機溶媒等で希釈されている。従って、レジストを室温に長時間放置すると有機溶媒が揮発して露光特性が変化するといった問題があった。そのため集積回路製造等ではレジスト塗布後、速やかに露光を完了させるようにしている。
(実施例1)
図17に示すように、φ30mmとφ58mmに加工された金属のスリーブ41を準備し、その外側に、長さ200mmで内径φ58mm、外径φ60mmのアクリルパイプ42を取り付け、円筒形状のスリーブを構成した。ここでは、アクリルパイプが熱断熱層の役割を果たしている。
露光用レーザー波長:405nm
レンズ開口数:0.85
露光用レーザーパワー:3mW~8mW
フォーカス用レーザー波長:665nm
フォーカス用レーザーパワー:0.2mW
回転速度:700rpm
送りピッチ:200nm/回転
スリーブ露光幅:200mm
図17に示すように、φ30mmとφ58mmに加工された金属のスリーブ41を準備し、その外側に、長さ200mmで内径φ58mm、外径φ60mmのアクリルパイプ42を取り付け、円筒形状のスリーブを構成した。ここでは、アクリルパイプが熱断熱層の役割を果たしている。
エッチングパワー:150W
エッチングガス圧:10Pa
ガス流量:20sccm
図17に示すように、φ30mmとφ60mmに加工された金属のスリーブ41を準備し、実施例1と同様の円筒形状のスリーブを構成した。
φ30mmとφ78mmに加工された金属の丸棒41を準備し、その外側に、長さ200mmで内径φ78mm、外径φ80mmのアルミパイプ45を取り付け図22に示すような円筒形状のスリーブモールドを構成した。
加工用半導体レーザー波長:405nm
レンズ開口数:0.85
加工レーザーパワー:5mW~8mW
フォーカス用半導体レーザー波長:660nm
フォーカスレーザーパワー:0.2mW
回転速度:700rpm
送りピッチ:400nm/回転
スリーブ露光幅:200mm
エッチングパワー:150W
エッチングガス圧:10Pa
ガス流量:20sccm
高周波周波数:13.56MHz
φ30mmとφ78mmに加工された金属の丸棒を準備し、その外側に、長さ200mmで内径φ78mm、外径φ80mmのアルミパイプを取り付け実施例4と同様な円筒形状のスリーブモールドを構成した。
エッチングパワー:150W
エッチングガス圧:10Pa
ガス流量:20sccm
高周波周波数:13.56MHz
実施例4と同様のφ30mmとφ78mmに加工された金属のスリーブを準備し、円筒形状のスリーブを構成した。
エッチングパワー:150W
エッチングガス圧:10Pa
ガス流量:20sccm
実施例4と同様のφ30mmとφ78mmに加工された金属のスリーブを準備し、円筒形状のスリーブを構成した。
エッチングパワー:150W
エッチングガス圧:10Pa
ガス流量:20sccm
φ30mmとφ78mmに加工された金属の丸棒を準備し、その外側に、長さ200mmで内径φ78mm、外径φ80mmのアルミパイプを取り付け実施例4と同様な円筒形状のスリーブモールドを構成した。
加工用半導体レーザー波長:473nm
レンズ開口数:0.25
加工レーザーパワー:15mW
回転速度:30rpm
送りピッチ:50μm/回転
加工幅:22μm
実施例4と同様のφ30mmとφ78mmに加工された金属のスリーブを準備し、円筒形状のスリーブを構成した。
Claims (25)
- スリーブ形状のモールド上に熱反応型レジスト層を形成する工程と、前記熱反応型レジスト層に対してレーザーを用いて微細モールドパターンを形成する工程と、を具備するシームレスモールドの製造方法であって、前記熱反応型レジスト層は、前記レーザーのスポット径での光強度分布において所定の光強度以上で反応する特性を持つ熱反応型レジストで構成されていることを特徴とするシームレスモールドの製造方法。
- スリーブ形状のモールド上に熱反応型レジスト層を形成する工程と、前記熱反応型レジスト層に対してレーザーを用いて微細モールドパターンを形成する工程と、を具備するシームレスモールドの製造方法であって、前記熱反応型レジスト層は、前記レーザーのスポット径において所定の温度以上で反応する領域を含む温度分布を持つ熱反応型レジストで構成されていることを特徴とするシームレスモールドの製造方法。
- スリーブ形状のモールド上に熱反応型レジスト層を形成する前に、前記スリーブ形状のモールド上にエッチング層を形成する工程と、前記微細モールドパターンをマスクとして前記エッチング層をエッチングする工程と、前記微細モールドパターンを除去する工程と、をさらに具備することを特徴とする請求項1又は請求項2記載のシームレスモールドの製造方法。
- 前記熱反応型レジストが有機レジスト又は無機レジストであることを特徴とする請求項1から請求項3のいずれかに記載のシームレスモールドの製造方法。
- 前記熱反応型レジストが、遷移金属及びXII族~XV族元素から成る群から選ばれる元素の不完全酸化物から成り、かつ、該元素の主要フッ化物の沸点が200℃以上であることを特徴とする請求項1から請求項3のいずれかに記載のシームレスモールドの製造方法。
- 前記遷移金属がTi、Cr、Mn、Fe、Co、Ni、Cu、Zr、Nb、Rh、Ag、Hf、Ta、及びAuから成る群から選ばれる元素であることを特徴とする請求項5に記載のシームレスモールドの製造方法。
- 前記XII族~XV族元素が、Al、Zn、Ga、In、Sn、Sb、Pb、及びBiから成る群から選ばれる元素であることを特徴とする請求項5又は請求項6に記載のシームレスモールドの製造方法。
- 前記遷移金属が、Ti、Cr、Mn、Co、Cu、Nb、Ag、Ta、及びAuから成る群から選ばれる元素であり、かつ、前記XII族~XV族元素が、Sn、Pb、及びBiから成る群から選ばれる元素であることを特徴とする請求項5に記載のシームレスモールドの製造方法。
- 前記エッチング層が、SiとTa並びにそれらの酸化物、窒化物、及び炭化物からなる群より選ばれる材料であることを特徴とする請求項3から請求項8のいずれかに記載のシームレスモールドの製造方法。
- 前記熱反応型レジスト層の膜厚が、膜厚のスリーブ周内での変動幅±20nm以下であることを特徴とする請求項1から請求項9のいずれかに記載のシームレスモールドの製造方法。
- 前記熱反応型レジスト層が少なくとも2層で構成されたことを特徴とする請求項1から請求項10のいずれかに記載のシームレスモールドの製造方法。
- 前記エッチング層上に熱反応型レジスト層を形成する前に、前記エッチング層上又は下に熱吸収層を形成する工程をさらに具備することを特徴とする請求項3から請求項11のいずれかに記載のシームレスモールドの製造方法。
- 前記スリーブ形状のモールド上にエッチング層を形成する前に、前記スリーブ形状のモールド上に熱絶縁層を形成する工程をさらに具備することを特徴とする請求項3から請求項12のいずれかに記載のシームレスモールドの製造方法。
- 前記熱反応型レジスト層、エッチング層、熱吸収層のいずれかを形成する方法が、スパッタリング法、蒸着法又はCVD法を用いて行なわれることを特徴とする請求項1から請求項13のいずれかに記載のシームレスモールドの製造方法。
- 前記レーザーを用いた露光の際に、前記レーザーのビーム形状を楕円形状とすることを特徴とする請求項1から請求項14のいずれかに記載のシームレスモールドの製造方法。
- 前記エッチング層をエッチングする際、真空槽中に、スリーブ形状のモールドと、該モールド表面の対向する位置に対向電極とが配置されていることを特徴とするドライエッチング装置を使用することを特徴とする請求項3から請求項15のいずれかに記載のシームレスモールドの製造方法。
- 請求項16で使用されたドライエッチング装置であって、真空槽中に、スリーブ形状のモールドと、該モールド表面の対向する位置に対向電極とが配置されていることを特徴とするドライエッチング装置。
- 該対向電極の形状が、円筒形状、平行平板形状、円弧形状から選択されるいずれかの形状であることを特徴とする請求項17に記載のドライエッチング装置。
- 該スリーブ形状のモールドが中心軸を中心に回転する機能を有することを特徴とする請求項17又は請求項18に記載のドライエッチング装置。
- 請求項1から請求項16のいずれかに記載のシームレスモールドの製造方法によって製造され、表面に微細形状が形成されたことを特徴とするシームレスモールド。
- 請求項20に記載のシームレスモールドを用いて製造することを特徴とする、表面に微細な凹凸パターンを有する継ぎ目の無い連続したフィルムの製造方法。
- 請求項21に記載の製造方法によって製造された、表面に微細な凹凸パターンを有するフィルム。
- 表面の微細形状のサイズが1μm以下であることを特徴とするシームレスモールド。
- 請求項23に記載のシームレスモールドを用いることを特徴とする表面上に1μm以下の微細形状パターンを有する継ぎ目の無い連続したフィルムの製造方法。
- 請求項24に記載の製造方法によって作製されたことを特徴とする微細形状パターンを有するフィルム。
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Also Published As
Publication number | Publication date |
---|---|
EP2246170A4 (en) | 2012-02-29 |
KR20120088868A (ko) | 2012-08-08 |
CN104076600B (zh) | 2019-02-15 |
TWI417181B (zh) | 2013-12-01 |
US20110027408A1 (en) | 2011-02-03 |
EP2246170B1 (en) | 2017-03-15 |
JP2012158178A (ja) | 2012-08-23 |
CN104076600A (zh) | 2014-10-01 |
JPWO2009093700A1 (ja) | 2011-05-26 |
JP5457487B2 (ja) | 2014-04-02 |
EP2246170A1 (en) | 2010-11-03 |
KR101316469B1 (ko) | 2013-10-08 |
US20160114503A1 (en) | 2016-04-28 |
JP4977212B2 (ja) | 2012-07-18 |
TW200946311A (en) | 2009-11-16 |
KR101220641B1 (ko) | 2013-01-10 |
US10399254B2 (en) | 2019-09-03 |
CN101952093A (zh) | 2011-01-19 |
KR20100106511A (ko) | 2010-10-01 |
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