WO2001031401A1 - Traitement automatique de composants optiques a diffraction dans des verres sol-gel hybrides - Google Patents

Traitement automatique de composants optiques a diffraction dans des verres sol-gel hybrides Download PDF

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Publication number
WO2001031401A1
WO2001031401A1 PCT/CA2000/001304 CA0001304W WO0131401A1 WO 2001031401 A1 WO2001031401 A1 WO 2001031401A1 CA 0001304 W CA0001304 W CA 0001304W WO 0131401 A1 WO0131401 A1 WO 0131401A1
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Prior art keywords
film
sol
compound
gel compound
gel
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PCT/CA2000/001304
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English (en)
Inventor
Serge Pelissier
Danièle BLANC PELISSIER
S. Iraj Najafi
Marc P. Andrews
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Mcgill University
Polyvalor, S.E.C.
Centre National De Recherche Scientifique
Lumenon Innovative Lightwave Technology Inc.
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Priority to AU11242/01A priority Critical patent/AU1124201A/en
Publication of WO2001031401A1 publication Critical patent/WO2001031401A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/25—Oxides by deposition from the liquid phase
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
    • C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/02—Surface treatment of glass, not in the form of fibres or filaments, by coating with glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
    • C03C23/002—Other surface treatment of glass not in the form of fibres or filaments by irradiation by ultraviolet light
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0005—Other surface treatment of glass not in the form of fibres or filaments by irradiation
    • C03C23/0025—Other surface treatment of glass not in the form of fibres or filaments by irradiation by a laser beam
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/18—Diffraction gratings
    • G02B5/1847—Manufacturing methods
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B5/00—Optical elements other than lenses
    • G02B5/18—Diffraction gratings
    • G02B5/1847—Manufacturing methods
    • G02B5/1857—Manufacturing methods using exposure or etching means, e.g. holography, photolithography, exposure to electron or ion beams
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
    • G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
    • G02B6/122—Basic optical elements, e.g. light-guiding paths
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
    • G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
    • G02B6/122—Basic optical elements, e.g. light-guiding paths
    • G02B6/124—Geodesic lenses or integrated gratings
    • 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
    • G03F7/0005—Production of optical devices or components in so far as characterised by the lithographic processes or materials used therefor
    • 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
    • G03F7/004—Photosensitive materials
    • G03F7/0042—Photosensitive materials with inorganic or organometallic light-sensitive compounds not otherwise provided for, e.g. inorganic resists
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/213—SiO2
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/23—Mixtures
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/44—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the composition of the continuous phase
    • C03C2217/45—Inorganic continuous phases
    • C03C2217/452—Glass
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/40—Coatings comprising at least one inhomogeneous layer
    • C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
    • C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
    • C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
    • C03C2217/475—Inorganic materials
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/70—Properties of coatings
    • C03C2217/77—Coatings having a rough surface
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/11—Deposition methods from solutions or suspensions
    • C03C2218/113—Deposition methods from solutions or suspensions by sol-gel processes
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/30—Aspects of methods for coating glass not covered above
    • C03C2218/32—After-treatment
    • G—PHYSICS
    • G02—OPTICS
    • G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
    • G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
    • G02B6/10—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type
    • G02B6/12—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings of the optical waveguide type of the integrated circuit kind
    • G02B2006/12083—Constructional arrangements
    • G02B2006/12107—Grating
    • 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
    • G03F7/20—Exposure; Apparatus therefor
    • G03F7/2022—Multi-step exposure, e.g. hybrid; backside exposure; blanket exposure, e.g. for image reversal; edge exposure, e.g. for edge bead removal; corrective exposure

Definitions

  • the present invention is concerned with a process for micro-structuring a surface and fabricating diffractive optical elements in self-processing photo-curable materials, without development following the exposure.
  • the sol-gel glass process is highly versatile for fabricating photonic devices. Moreover, the introduction of organic components in the inorganic network permits further tailoring of chemical and physical properties of the glasses (improved mechanical properties, lower densification temperature, tailored refractive index, etc.). Photo- sensitivity has been demonstrated in acrylate-rich hybrid glasses where light initiates a chemical process that records the incident light pattern as a variation of polymerized and non-polymerized regions. Waveguides and diffractive elements have already been produced in acrylate-rich silica-zirconia compounds with a wet chemical etching step following the irradiation procedure [[H. Krug, and H. Schmidt, "Organic-inorganic nanocomposites for micro optical applications", New J. Chem.
  • An object of the present invention is therefore to provide a simple process for producing controlled surface deformation in sol-gel compounds with applications in the low-cost mass-production of micro-optical elements.
  • a process of fabricating a diffractive optical component comprising coating a substrate with a film of photosensitive sol-gel compound, pre-photoprocessing the film of photosensitive sol-gel compound, and imprinting a surface grating on the pre-photoprocessed film of photosensitive sol-gel compound.
  • Pre-photoprocessing the film of photosensitive sol-gel compound comprises flooding the entire surface of the film of photosensitive sol-gel compound with light, and modifying compressive and tensile stresses at the surface of the film of photosensitive sol-gel compound in response to the flooding light.
  • the photosensitive sol-gel compound is a hybrid sol-gel glass compound
  • the hybrid sol-gel glass compound is an acrylate-rich hybrid sol-gel glass compound
  • the acrylate-rich hybrid sol-gel glass compound is selected from the group consisting of: an acrylate-rich silica-titania compound; and an acrylate-rich silica-zirconia compound;
  • the photosensitive hybrid sol-gel glass compound is doped with at least one metallic element selected from the group consisting of: titanium, vanadium, chromium, niobium, tantalum, tungsten, molybdenum, and zirconium;
  • the substrate is selected from the group consisting of: glass substrates; paper substrates; metal substrates; plastic substrates; wood substrates; dielectric substrates; and semiconductor substrates including silicon wafer substrates;
  • the photosensitive sol-gel compound is an acrylate-rich silica-titania compound, and wherein the process comprises, prior to coating the substrate, preparing the photosensitive sol-gel compound by:
  • preparing a hybrid organosilicate glass comprises: - conducting partial hydrolysis and polycondensation of the methacryloxypropyl-trimethoxysilane; dissolving the titanium (IV) isopropoxide in isopropanol and complexing said titanium (IV) isopropoxide with methacrylic acid before dispersing said titanium (IV) isoproxide into the silicon oxide system; resuming hydrolysis and condensation of remaining silicon alkoxide functionalities and titanium propoxide; adding a photoinitiator to the solution; and filtering and aging said solution;
  • - preparing a hybrid organosilicate glass comprises introducing methacryloxypropyltrimethoxysilane, titanium (IV) isopropoxide, and methacrylic acid in a molar ratio of 10:2.5:2.5;
  • - conducting partial hydrolysis and polycondensation of the methacryloxypropyltrimethoxysilane comprises initiating said partial hydrolysis and polycondensation with 0.75 equivalent of acidified water; - the acidified water is a 0.01 M HCI acidified water.
  • - resuming hydrolysis and condensation of remaining silicon alkoxide functionalities and titanium propoxide comprises resuming the hydrolysis and condensation of the remaining silicon alkoxide functionalities and the titanium propoxide with the remaining equivalent of water, wherein total H 2 O:Si and H 2 O:Ti molar ratios are equal to 1.5;
  • adding a photoinitiator to the solution comprises adding 3 wt % of Bis(2,4,6-trimethylbenzoyl)-phenylphosphineoxide;
  • - aging the solution comprises allowing the solution to age for 24 hours;
  • the diffractive optical component fabricating process further comprises, prior to pre-photoprocessing the film of photosensitive sol-gel compound, drying this film by applying thereto a low power density UV-curing;
  • An advantage of the process according to the invention is that it involves no etching or other type of development method. Also, the obtained diffractive optical components are resistant to changes in amplitude or period caused by changes in temperature or contact with solvents, like alcohols, ketones or water.
  • Figure 1 is a flow chart showing the different steps of a preferred embodiment of the process according to the invention.
  • Figure 2 is a flow chart showing the different substeps involved in a pre-photoprocessing step of the process of Figure 1 ;
  • Figure 7 is a photograph of the Fraunhofer diffraction pattern from two 4 ⁇ m-period gratings recorded orthogonally to each other in a silica-zirconia sol-gel layer;
  • Figure 8 is an AFM three dimensional view showing the absence of swelling at the edge of the grating when sample was UV- cured with a mercury lamp (3 mW/cm 2 for 5 min) before imprinting;
  • a hybrid organosilicate glass is prepared from methacryloxypropyl- trimethoxysilane, titanium (IV) isopropoxide, and methacrylic acid.
  • methacryloxypropyltrimethoxysilane, titanium (IV) isopropoxide, and methacrylic acid are included in a molar ratio of 10:2.5:2.5. Partial hydrolysis and polycondensation of methacryloxypropyltrimethoxysilane was initiated with 0.75 equivalent of acidified water, for example a 0.01 M
  • the metal is added to modify the structural properties of the glass, including hardness, which is particularly relevant to making Bragg gratings that show increased stability to resist changes in the dimensions of the grating due to the effects of heating or cooling or exposure to solvents.
  • step 3 of Figure 1 drying the film of sol-gel compound (step 3 of Figure 1) with a low power density UV-curing;
  • a UV low power density of 3 mW/cm 2 from a mercury lamp was applied for 5 minutes to at least partially dry the coated substrate.
  • Other processs such as oven-drying and exposure to visible light, infrared radiation or microwave radiation could also be used for drying the sol-gel compound.
  • the surface of the film of photosensitive hybrid sol-gel glass compound is subjected to a pre-photoprocessing step.
  • the purpose of pre-photoprocessing the film of photosensitive hybrid sol-gel glass compound is to modify the compressive and tensile stresses in the film, in particular at the surface of the film, to add control over the peak- to-valley depth of the diffraction grating that is subsequently formed.
  • the pre-photoprocessing step further dries the surface of the film to ensure that this film will not adhere to the photomask when this mask is contacted with the surface of the film during writing of the grating.
  • This pre-photoprocessing step comprises exposing, more specifically flooding the entire surface of the film of photosensitive hybrid sol-gel glass compound with light (step 21 of Figure 2).
  • the power density of the flooding light will be of the order of 10 mW/cm 2 .
  • This light may be in the wavelength range 200-450 nm, preferably in the range 240-400 nm.
  • This pre-photoprocessing step is conducted over a range of time extending from 10 seconds to 10 minutes, depending on the intensity and wavelength of the light and the desired effect. A light-exposure time of 30 seconds is usually preferred.
  • This pre-photoprocessing step may be conducted at or above room temperature.
  • pre- photoprocessing involves parameters such as the power density of the flooding light, the wavelength of the flooding light, the time of exposure of the film to the flooding light, and the temperature which can be selected to modify the compressive and tensile stresses in the film, in particular at the surface of the film (step 22 of Figure 2) as required to obtain the desired control over the peak-to-valley depth of the diffraction grating (step 23 of Figure 2) that is subsequently formed.
  • step e ⁇ an alternative to step e ⁇ is to expose the sample to a UV laser light beam through a phase mask in a proximity mode.
  • UV, visible or infrared laser beam interference can also be used to locally expose the sample and imprint the surface grating.
  • Further available processes comprise, amongst others, exposure of the sample to a laser beam through a grey-scale mask, direct laser writing and other interferometric techniques. Local exposure of the film of photosensitive hybrid sol-gel glass compound to UV light through a mask causes local densification and shrinkage of the illuminated area in order to imprint the desired surface grating of the diffractive optical component.
  • pre-photoprocessing greatly influences the peak-to-valley depth of the grating.
  • the alkoxides for example methacryloxypropyltrimethoxysilane are caused to undergo hydrolysis and polycondensation by acid catalysed decomposition of the silico- alkoxide bond.
  • This polycondensation reaction generates a colloidal suspension called a sol.
  • the sol phase is spin- or dip-coated to make a film.
  • the process of film formation is accompanied by further crosslinking reactions to make silicon-oxygen-siiicon bonds throughout the film.
  • the material enters a gel phase.
  • one bond to silicon contains an organic substituent (an olefin) that can be caused to polymerize when exposed to light
  • a second crosslinking step can be introduced. This occurs when the olefin polymerizes with other olefin moieties in the film of the glass. In this manner, crosslinks involving silicon-carbon-silicon bonds are obtained in the matrix film.
  • the self-processing operation takes place when the photosensitive hybrid sol-gel glass compound is exposed to light and the film responds by producing a polyolefin within the glass.
  • Pre-photoprocessing of the film was subsequently conducted by flooding the entire surface of the film with light having a wavelength of 313 nm selected by a band-pass filter, and a power density of 10 mW/cm 2 for an exposure time of 5 minutes at room temperature. Then:
  • optical interconnection schemes including but not restricted to planar lightwave circuit (optical chip)-to-planar lightwave circuit coupling, and inter layer coupling of light.
  • this self-processing process requires no etching or other development step, and is therefore a short technological process
  • the corrugation is stable even in the absence of any photo or thermal post-treatment
  • the amplitude of the photo-induced surface corrugation was found to be dependent on the the conditions of UV dose and exposure time in both the pre- photoprocessing and grating writing steps. It varied also with the feature size of the pattern to be imprinted in the film.
  • the amplitude of the corrugation obtained with an UV source in the above described example, typically 90 mW-cm "2 ) could be as large as 800 nm. Amplitude of the 0.56 ⁇ m-period grating obtained with the excimer laser was around 110 nm;
  • the root mean square value of the roughness Rq measured by atomic force microscopy on a 100x100 nm 2 area is smaller than 0.5 nm and can be as low as 0.1 nm, depending on the processing conditions;
  • the localized densification and shrinkage of the sol-gel material corresponds to the illuminated regions through the opening of the mask.
  • the formation of photo-relief in this acrylate-containing hybrid sol-gel glass compound ( Figure 10) differs from grating formation by diffusion of monomer in viscous thick film acrylates, or relief due to trans-cis-trans isomerization in media containing azo chromophores. Densification is caused by C-C bond formation during organic polymer chain growth, which induces collateral structural relaxation and condensation reactions in the metastable silica network
  • the 0.56- ⁇ m-period grating which is given above as an example of application is by no means a limit in feature size; - high transmittance of the material: the material is transparent in the visible-near infrared region and is therefore suitable for various applications within this spectral range. This is not the case of the azo-containing materials which absorb in the green region of the spectrum;
  • the material is compatible with most commonly used substrates, including silicon, glass and metals.
  • the composition of the material can be tuned to vary the refractive index and other physical properties.
  • the photoinitiator can also be changed according to the thickness of the section to be cured or the wavelength used;
  • the components after UV inscription the components are solvent-resistant (water, acetone, isopropanol) and can be heated to temperature as high as 220°C for silica-titania compounds and 180°C for silica-zirconia compounds without any deterioration of the diffraction efficiency. This is not the case of azo- containing materials or of most photopolymers which do not stand so high temperatures. Also, no changes in the diffraction efficiency were measured when the gratings were submitted to post-UV exposure (10 mW/cm 2 for 30 min).
  • Table 1 shows typical experimental and theoretical values of diffraction efficiencies ( ⁇ ) transmitted in the various orders (wavelength is 0.6328 ⁇ m). All gratings were UV-imprinted according to the present invention in silica-titania sol-gel films. Gratings 1 and 2 were imprinted with a mercury lamp through an amplitude chromium mask. Grating 3 was imprinted with an ArF excimer laser through a phase mask. The amplitude of the surface corrugation measured by atomic force microscopy is represented by "h”. Discrepancies between theoretical and experimental values can be explained by the profile of the corrugated grating which is not perfectly sinusoidal.
  • - diffractive optical components as described above, including a surface grating;
  • DOE Diffractive Optical Elements comprising, but not restricted to, focussing elements such as lenses, including Fresnel lenses;
  • - photonic band gap devices such as optical filters (not based on simple grating diffraction);

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Abstract

L'invention concerne un procédé simple destiné à opérer une déformation de surface régulée dans des composés de verre sol-gel hybride photosensible. Cette invention est destinée à des applications de production en série à faible coût d'éléments micro-optiques. Ledit procédé consiste d'abord à produire des composants optiques à diffraction par phototraitement préliminaire d'un film de composé de verre sol-gel hybride de façon à modifier l'effort de traction et la tension de compression à la surface du film, puis à exposer le film soumis à ce phototraitement préliminaire à une lumière UV par l'intermédiaire d'un masque afin de provoquer localement une densification et un retrait des zones éclairées. Ledit procédé ne comprend pas d'étape d'attaque chimique, les composants à diffraction étant résistants aux effets de la température et des solvants. Les applications commerciales de cette invention relèvent du domaine des télécommunications, de la communication de données et de la détection, et plus particulièrement de la microstructuration de surfaces.
PCT/CA2000/001304 1999-10-26 2000-10-26 Traitement automatique de composants optiques a diffraction dans des verres sol-gel hybrides WO2001031401A1 (fr)

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US60/161,351 1999-10-26

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CN113866875A (zh) * 2021-10-08 2021-12-31 吉林大学 一种带有损耗补偿功能的光栅层间耦合器及其制备方法

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US7081278B2 (en) 2002-09-25 2006-07-25 Asml Holdings N.V. Method for protection of adhesives used to secure optics from ultra-violet light
US9195148B2 (en) 2002-09-25 2015-11-24 Asml Holding N.V. Side seal for wet lens elements
US7781029B2 (en) 2002-09-25 2010-08-24 Asml Holding N.V. Side seal for wet lens elements
EP1413907A1 (fr) * 2002-09-25 2004-04-28 ASML Holding, N.V. Procédé pour protéger des adhesifs fixant une optique de la lumière ultra-violette
GB2454342B (en) * 2005-06-30 2010-02-03 Hoya Corp Optical image stabilizer
GB2454342A (en) * 2005-06-30 2009-05-06 Hoya Corp Optical image stabilizer
US7742672B2 (en) 2005-08-24 2010-06-22 General Electric Company Composition, optical device article, and associated method
US7541391B2 (en) 2005-09-02 2009-06-02 General Electric Company Self-forming polymer waveguide and waveguide material with reduced shrinkage
CN100576070C (zh) * 2005-10-21 2009-12-30 同济大学 一种制备光敏凝胶薄膜以实现光栅图形转移的方法
GB2451595A (en) * 2006-04-28 2009-02-04 Univ Southampton Manufacturing a diffraction grating
GB2451595B (en) * 2006-04-28 2009-06-17 Univ Southampton Diffraction element and method of manufacturing the same
GB2437554B (en) * 2006-04-28 2009-04-15 Univ Southampton Diffraction element and method of manufacturing the same
GB2437554A (en) * 2006-04-28 2007-10-31 Univ Southampton Diffraction element and method of manufacturing the same
JP2007298697A (ja) * 2006-04-28 2007-11-15 Univ Of Southampton 回折素子とその製造方法
WO2008027299A3 (fr) * 2006-08-28 2008-04-24 Corning Inc Articles à dépressions de surface multiples et leur procédé de fabrication
WO2008027299A2 (fr) * 2006-08-28 2008-03-06 Corning Incorporated Articles à dépressions de surface multiples et leur procédé de fabrication
US8420280B2 (en) * 2006-09-01 2013-04-16 Tdk Corporation Hologram recording medium
US8728579B2 (en) 2008-10-31 2014-05-20 University Of Florida Research Foundation, Inc. Transparent inorganic-organic hybrid materials via aqueous sol-gel processing
US9011592B2 (en) 2008-10-31 2015-04-21 University Of Florida Research Foundation, Inc. Transparent inorganic-organic hybrid materials via aqueous sol-gel processing
WO2010062436A1 (fr) * 2008-10-31 2010-06-03 University Of Florida Research Foundation, Inc. Matériaux hybrides inorganiques-organiques transparents obtenus par un traitement sol-gel aqueux
CN107219579A (zh) * 2017-07-10 2017-09-29 扬州大学 多倍频沟槽型周期栅阵制备方法
CN107356997A (zh) * 2017-07-10 2017-11-17 扬州大学 多倍频栅条型周期栅阵制备方法
CN113866875A (zh) * 2021-10-08 2021-12-31 吉林大学 一种带有损耗补偿功能的光栅层间耦合器及其制备方法
CN113866875B (zh) * 2021-10-08 2023-10-10 吉林大学 一种带有损耗补偿功能的光栅层间耦合器及其制备方法

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