WO2025131402A1 - Lunettes pour modification d'indice local par traitement laser à impulsions ultracourtes et dispositifs les comprenant - Google Patents

Lunettes pour modification d'indice local par traitement laser à impulsions ultracourtes et dispositifs les comprenant Download PDF

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Publication number
WO2025131402A1
WO2025131402A1 PCT/EP2024/081193 EP2024081193W WO2025131402A1 WO 2025131402 A1 WO2025131402 A1 WO 2025131402A1 EP 2024081193 W EP2024081193 W EP 2024081193W WO 2025131402 A1 WO2025131402 A1 WO 2025131402A1
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Prior art keywords
glass
substrate
ppm
glasses
laser
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PCT/EP2024/081193
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English (en)
Inventor
Ulrich Fotheringham
Martin Letz
Jens Ulrich Thomas
Bianca Schreder
Holger Wegener
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Schott AG
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Schott AG
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Classifications

    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/097—Glass compositions containing silica with 40% to 90% silica, by weight containing phosphorus, niobium or tantalum
    • 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
    • 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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
    • C03C3/083—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound
    • C03C3/085—Glass compositions containing silica with 40% to 90% silica, by weight containing aluminium oxide or an iron compound containing an oxide of a divalent metal
    • 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
    • G02B6/13—Integrated optical circuits characterised by the manufacturing method

Definitions

  • the invention refers to glasses which combine suitability for local index modification by ultrashort pulse laser (usp-laser) treatment with a low thermal expansion, advantageously matching especially to that of semiconductor materials such as silicon, i.e. a comparatively low thermal expansion coefficient (CTE), and devices incorporating those glasses, especially devices comprising the glass and a semiconductor element.
  • usp-laser ultrashort pulse laser
  • CTE thermal expansion coefficient
  • the usp-laser treatment will lead, first, to a local melting of the glass in the focal area of the laser, and, second, to a high temperature gradient there.
  • this temperature gradient will give rise to a Soret effect with the heavier ions accumulating in the colder areas and the lighter ones accumulating in the hotter area.
  • This effect makes LAS systems particularly suited for increasing the refractive index that way. Aluminium is lighter than Silicon, Lithium is even very much lighter than Silicon so that a LAS system will separate into a Lithium- and Aluminium-rich zone in the centre of the focal area and a Lithium- and Aluminium-deprived area around it.
  • the goal of the present invention is therefore to provide glass substrates, which are suitable for the following process: by moving the focus of an ultrashort pulse laser through the glass, permanent lines of modifications can be realized inwithin the glass substrate volume, without modifying the volume surrounding the modification line.
  • the material modification of the line can consist of micro voids, optical damages, birefringent nanovoids or density changes that result in a locally higher refractive index.
  • the later modification, the raise of the refractive index is favorable in the context of this invention, because the modification lines can then serve as waveguide cores.
  • the flexibility of “writing” the modification lines freely within the glass substrate volume enables complex 3-dimensional waveguide circuits.
  • Evanescent coupling between waveguides can be achieved to place waveguide cores in close vicinity (so that the evanescent parts of the waveguide modes overlap). Based on this principle coupling from one to N waveguides, therefore waveguide splitters can be achieved. They may optionally be combined by optical elements which may also be generated by a usp-laser, e.g., diffractive optical structures which serve as filters or in-line reflectors (Bragg-Gratings).AIso, the modification lines itself can have a sub-structure, e.g. a periodic or an-periodic modulation along the line or a modification profile across the transversal cross-section.
  • stoichiometric glasses i.e. glasses which exist in the same stoichiometry also as crystals and whose properties can be assumed to be very similar for both glass and crystal because of the identical topology of the assemblies.
  • This theorem can be verified in the literature in many examples by NMR measurements or the like.
  • such stoichiometric glasses are selected whose mixture provide a behavior in the sense of a solution of the object according to the invention attainable.
  • these stoichiometric glasses are also referred to as "constituent phases".
  • the invention relates to a glass having the following combination of constituent phases:
  • the composition is chosen with regard to the phases constituting the glass within the limits described herein.
  • the phases constituting the glass are, of course, not present as such in the glass product in crystalline, but amorphous form. This does not mean, however, that the constituent phases have completely different building units in the amorphous state than in the crystalline state.
  • the topology of the building units is comparable, e.g., the coordination of the cations involved with surrounding oxygen atoms or the interatomic distance resulting from the coordination and the strength of the bond between these cations and surrounding oxygen atoms. Therefore, many properties of the glass of the invention can be well described on the basis of the constituent phases, in particular to illustrate the inventive achievement and the problems overcome by the invention.
  • the glass can be produced not only by using the corresponding crystals, but also by using the usual glass raw materials, as long as only the stoichiometric ratios allow the formation of the corresponding building blocks of the constituent phases.
  • the suitability for local index modification by usp-laser treatment is made sure by the above upper limits for the content of heavy ions (e.g. Potassium, Zinc) containing constituent phases.
  • heavy ions e.g. Potassium, Zinc
  • the position of the thermal expansion coefficient according to ISO 7991 in the target range can also be represented with the aid of a calculation rule taking into account the average bond strength.
  • a mean potential well depth E pot From the composition of a glass comprising or consisting of the constituent phases given above, the numbers of different cations contained in the respective phases, and the potential well depths per cation tabulated above, a mean potential well depth E pot can be calculated:
  • Epotj is the potential well depth tabulated above for the j-th cation type
  • Zj is the number of cations of the j-th type in the i-th constituent phase. The sums overj are tabulated below:
  • the bond strength is inversely proportional to the melting point
  • an inverse proportionality also applies between the melting point and the coefficient of expansion.
  • the melting point is not precisely defined for non-stoichiometric glasses, only a tendential relationship applies between a typical temperature for the melting and hot forming range, e.g., the working point, at which the viscosity is 10 4 dPa s, and the coefficient of expansion.
  • this tendential relationship makes it clear that the combination of low coefficient of thermal expansion and an upper limit for the working point is challenging, especially if the glass is simultaneously supposed to have a high lithium fraction, which favours a low working point but does not favour a low coefficient of thermal expansion.
  • the thermal expansion coefficient of the glass should be made small, preferably as close as possible to the one of silicon in order to suppress any negative effect caused by an expansion mismatch. Therefore, the thermal expansion coefficient (CTE) of the glass is preferred to be at most 8 ppm/K, more preferably at most 7.75 ppm/K, more preferably at most 7.5 ppm/K, more preferably at most 7.25 ppm/K, more preferably at most 7 ppm/K, more preferably at most 6.75 ppm/K, more preferably at most 6.5 ppm/K, more preferably at most 6.25 ppm/K, more preferably at most 6.0 ppm/K, more preferably at most 5.75 ppm/K, more preferably at most 5.5 ppm/K, more preferably at most 5.25 ppm/K, more preferably at most 5.0 ppm/K, more preferably at most 4.75 ppm/K, more preferably at most
  • the CTE is at least 2.50 ppm/K, at least 2.75 ppm/K, at least 3.00 ppm/K, at least 3.25 ppm/K, or at least 3.50 ppm/K. This refers to the value CTE, which can be calculated using formula (2) for glasses of this invention.
  • a mixing rule can also be given for viscosity of glass, with which the viscosity is calculated from the viscosities of the constituent phases.
  • TK is the Kauzmann temperature, which according to C.A. Angell, loc. cit., is identified with the Vogel-Fulcher-Tammann temperature To.
  • VFT equation Vogel-Fulcher-Tamman equation
  • A, B, To are the parameters of the VFT equation, which are determined by fit to a measurement curve.
  • the parameters qo and D/Q, which are in the Adam-Gibbs relationship can be calculated from the VFT parameters A, B, To.
  • a mixing rule can be derived that can be used to calculate the VFT parameters of a glass from the VFT parameters of the constituent phases known from measurements.
  • the first approach is:
  • Di or Di/Q refer to the individual constituent phases and are obtained from their VFT parameters Ai, Bi, To,i according to (6).
  • the sum over “i” is from 1 to n, as above.
  • VFT parameters of a glass expressed as a mixture of the constituent phases forming the basic system of the invention. These are:
  • WP ⁇ + T ° ( 1 °) and the annealing point AP according to:
  • the working point is advantageously at most 1400°C, more advantageously at most 1390°C, more advantageously at most 1380°C, more advantageously at most 1370°C, more advantageously at most 1360°C, more advantageously at most 1350°C, more advantageously at most 1340°C, more advantageously at most 1330°C, more advantageously at most 1320°C, more advantageously at most 1310°C, more advantageously at most 1300°C, more advantageously at most 1290°C, more advantageously at most 1280°C, more advantageously at most 1270°C, more advantageously at most 1260°C, more advantageously at most 1250°C.
  • the selection of the constituent phases according to this invention has been performed with respect to their suitability for usp-laser-structuring, expansion coefficient, working point, devitrification and mechanical properties.
  • working point the temperature is addressd where the viscosity value is 10 4 dP s, a typical viscosity for the melting and hot forming range.
  • the role of the individual constituent phases in this invention is discussed in detail.
  • the total Lithium fraction as provided by the two above constituent phases preferably exceeds 4mol%, more preferred 6mol%, more preferred 8mol%, more preferred 10mol%, more preferred 12mol%, more preferred 14mol%, more preferred 16mol%, more preferred 18mol%, more preferred 20mol%, more preferred 22mol%, more preferred 24mol%, more preferred 26mol%, more preferred 28mol%, more preferred 30mol%, more preferred 32mol%.
  • Glassy Spodumene is the other essential constituent phase which addresses the core of the invention disclosed by US 7262144 B2 from 2007. It contains both Lithium (see above) and Aluminium. As the latter is only slightly lighter than Silicon, it is not assumed to significantly contribute to the essential effect of refractive index increase in the centre of the usp-laser focus.
  • Spodumene is understood to be one mole of (Li2O Al2O3-4SiO2)/6.
  • Albite is added one of the constituent phases according to the invention to provide an additional degree of freedom concerning the adjustment of the thermal expansion and the working point.
  • Sodium is only slightly ligther than Silicon
  • Albite is assumed to contribute less to the essential effect of refractive index increase in the centre of the usp-laser focus than the Lithium-containg phases.
  • Albite is understood to be one mole of (Na2O Al2O3-6SiO2)/8.
  • Glassy Orthoklas is the potassium analogon of albite and another constituent phase according to the invention.
  • a small amount of Orthoklas may be added to the composition.
  • a Potassium-containing phase is disadvantageous with respect to the essential effect of US 7262144 B2 from 2007.
  • One mole of Orthoklas is understood to be one mole of (K2O Al2O3-6SiO2)/8.
  • Glassy Disodium-Zinco-Silicate is added to the constituent phases according to the invention to provide an additional degree of freedom with respect to adjusting thermal expansion and working point.
  • a Zinc-contain- ing phase is disadvantageous with respect to the essential effect of US 7262144 B2 from 2007.
  • Glassy Cordierite is added as one of the constituent phases according to the invention to provide an additional degree of freedom concerning the adjustment of the thermal expansion and the working point.
  • Cordierite is assumed to contribute less to the essential effect of refractive index increase in the centre of the usp-laser focus than the Lithium-containing phases.
  • glassy SiO2 is essential to push down the coefficient of expansion and thus, on balance, to desired values.
  • glassy B2O3 is also suitable to push down the coefficient of expansion and thus, on balance, to desired values.
  • Diboron trioxide forms boroxol rings as a constituent phase, which have a favourable effect on the mechanical properties.
  • diboron trioxide is unsuitable as a basic system for the glasses according to the invention, it is suitable only as an admixture.
  • Glassy Magnesiummetaphosphate is added as one of the constituent phases according to the invention to provide an additional degree of freedom concerning the adjustment of the thermal expansion and the working point.
  • Magnesium is only slightly lighter than Silicon
  • Magnesiummetaphosphate is assumed to contribute less to the essential effect of refractive index increase in the centre of the usp-laser focus than the Lithium-containing phases.
  • Phosphorous is slightly heavier than Silicon, it may be expected to accumulate in the outside section of the usp-laser-fo- cus. With respect to its ultra-low polarizability, this will not be disadvantageous with respect to the essential effect of US 7262144 B2.
  • Magnesiumetaphosphate is understood to mean one mole of (MgO P 2 O 5 )/2.
  • the glass may contain further constituents, referred to herein as "balance".
  • the proportion of balance in the glass according to the invention is preferably at most 5 mol-%, so as not to disturb the glass properties set by careful selection of suitable base glasses.
  • the proportion of balance in the glass is at most 3 mol%, more preferably at most 2 mol% or at most 1 mol% or at most 0.5 mol%.
  • the balance contains in particular oxides which are not contained in the base glasses mentioned herein.
  • the balance in particular does not contain SiC>2, B2O3, AI2O3, ZnO, MgO, l_i2O, Na2O or K2O.
  • the glass according to this invention will preferably be provided as sheet or endless sheet, with a medium thickness of 30pm to 3mm.
  • Forming the glass may comprise a drawing process or a floating process. Cooling may involve active cooling using a coolant, such as a cooling fluid, or passive cooling.
  • a coolant such as a cooling fluid
  • a corresponding glass has a thermal expansion coefficient CTE that is at most 8 ppm/K or which ranges especially from 2.5 ppm/K to 8 ppm/K and wherein preferably the working point is at most 1400°C.
  • the Lithium fraction is at least 4.0 mol%.
  • the Lithium fraction is calculated by a matrix represented by aforesaid table 7 of this description.
  • the invention also covers a substrate comprising the glass described above, wherein the glass contains an inscribed waveguide and/or wherein the substrate is mounted to a semiconductor device, or the semiconductor device is mounted to a substrate areas comprising the aforesaid glass.
  • the invention relates to an electronic or optoelectronic device as well which comprises the glass or the substrate described above.
  • the electronic or optoelectronic device according to the invention comprises a semiconductor device or substrate which has a CTE from 2.6 to 3.4 ppm/K and preferably the glass has a CTE from 2.5 to 3.6 ppm/K.
  • the method of inscribing a waveguide into a substrate comprising the steps of providing a usp-laser source and directing a focused laser beam from said usp-laser source onto the substrate, whereas the substrate is selected from a glass described above, is also subject to the invention.
  • Suitable lasers for waveguide inscription are ultra short pulse lasers, thus lasers that emit their power as pulse trains, where the temporal distance between the pulses is 1/R, with R being the repetition rate of the laser.
  • the repetion rate can be in the range from 1 Hz to 100 GHz, but preferred, 1 kHz, 10 kHz, 50 kHz, 100 kHz, 500 kHz, 1 MHz.
  • the pulse duration (FWHM, full width, half max) of these lasers is typically between 30 fs up to 20 ps.
  • the preferred duration is 80 fs to 300 fs, most preferred 100 fs.
  • the center wavelengths can also be 200 nm, 355 nm, 400 nm, 515 nm, 532 nm,
  • the spectral bandwidth can be 1 nm an up to 100 nm.
  • the output beam parameter of the collimated laser beam is usualle 3 to 5 mm (1/e 2 ), but can also be increased with telescope setup to 10 mm or 20 mm.
  • Some of these lasers can not only emit their energy single pulses, but also divide the energy in sub-pulse trains, so-called “burst”, where the inter-subpulse distance At P is much smaller than 1/R, typically in the range of 1-200 ns, most preferred to be 20 ns - 30 ns.
  • burst consist of 2 to 50 sub pulses.
  • Preferred bursts of 2 to 4 or 3 to 7 sub pulses.
  • the ouput power P of the lasers is typically between 1 W and 500 W.
  • the pulse energy or burst energy is P/R.
  • the translation velocity is the velocity the focus of the objective is moved relative to the glass substrate. This can be achieved by translating the sample via a motion controlled stage or by moving the laser focus, e.g. with a mirror ensemble that ensures that the laser beam is still incident on the input aperture of the objective, when the objective is move with a mechanical axis.
  • Another implementation is the integration of deformable mirror or a spatial light modulator (SLM) before the objective; thus translating the spot by imprinting a defocus and/or a tilt on the wavefront of the incident beam.
  • SLM spatial light modulator
  • a combination of both of the translation mechanisms can be favorable, e.g. for achieving precicion for longer modification lines.
  • the preferred An is in the range of 0.0001 to 0.002, mostly preferred 0.0005 to 0.005.
  • the An can be continuously altered. This can be done during inscription, so that An varies along the modification line of length L.
  • the variation of can be linear or non-linear function of the modification line coordinate I, 0 ⁇ l ⁇ L. It can also be periodic or an-periodic.
  • the transversal refractive index profile of the modification line is relevant.
  • the local coordinate vectors x and y which are both perpendicular to the modification line vector z and centered at the modification line.
  • ⁇ w y /2 and An 0 elsewhere.
  • w x and w y are the transversal widths of the waveguides, which are typically 0.2 pm to 100 pm, most preferred 0.5 to 20 pm, mostly preferred 1 -15 pm, more mostly preferred 2-12pm.
  • This profile can also be altered along the modification line. In this case we relate to the FWHM definition of the waveguide width along the local x and y axis.
  • the waveguides lines of this invention have low losses for light at the wavelength of 1550 nm, namely below 1 dB/cm, preferably 0.5 dB/cm, most preferred smaller than 0.3 dB/cm, mostly preferred below 0.1 dB/cm.
  • Also provided herein is a method of manufacturing an electronic or optoelectronic device, comprising the steps of mounting a semiconductor element to an element comprising the glass according to this description.
  • the invention is represented in a method of manufacturing an electronic or optoelectronic device comprising a semiconductor element and a glass substrate, comprising the steps of determining the CTE of the semiconductor element, then selecting the CTE of glass of the glass substrate by selecting a composition range of the glass according to this description.
  • composition in constituent phases is given in the following normalized form for the purpose of conversion:
  • composition in mol% with respect to the constituent phases is multiplied as a column vector from the right to the matrix:
  • the thermal expansion coefficient calculated according to (2) amounts to 9.45 ppm/K.
  • the working point calculated according to (10) amounts to 1169.99°C.
  • the first example is a glass with the composition:
  • the calculated properties are:
  • the thermal expansion coefficient calculated according to (2) amounts to 5.91 ppm/K.
  • the calculated properties are:
  • the thermal expansion coefficient calculated according to (2) amounts to 5.96 ppm/K.
  • the next example is a glass with the composition:
  • the calculated properties are:
  • the thermal expansion coefficient calculated according to (2) amounts to 6.63 ppm/K.
  • the working point calculated according to (10) amounts to 1224°C.
  • the next example is a glass with the composition:
  • the thermal expansion coefficient calculated according to (2) amounts to 7.9 ppm/K.
  • the next example is a glass with the composition:
  • the calculated properties are: 1 .
  • the thermal expansion coefficient calculated according to (2) amounts to 4.63 ppm/K.

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Abstract

L'invention concerne un verre ou un substrat en verre ayant des phases constitutives qui permettent l'inscription de guides d'ondes par des lasers usp, le coefficient de dilatation thermique étant d'au plus 8 ppm/K, en particulier de 2,5 ppm/K à 8 ppm/K Le verre est donc particulièrement adapté à la combinaison avec des dispositifs semi-conducteurs ou des substrats, par exemple pour la réalisation de dispositifs électroniques ou optoélectroniques.
PCT/EP2024/081193 2023-12-20 2024-11-05 Lunettes pour modification d'indice local par traitement laser à impulsions ultracourtes et dispositifs les comprenant Pending WO2025131402A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
EP23218627 2023-12-20
EP23218627.0 2023-12-20
EP24168585 2024-04-04
EP24168585.8 2024-04-04

Publications (1)

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WO2025131402A1 true WO2025131402A1 (fr) 2025-06-26

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7262144B2 (en) 2003-02-03 2007-08-28 Schott Ag Photostructurable body and process for treating a glass and/or a glass-ceramic
DE102014119594A1 (de) 2014-12-23 2016-06-23 Schott Ag Borosilikatglas mit niedriger Sprödigkeit und hoher intrinsischer Festigkeit, seine Herstellung und seine Verwendung
US20160340228A1 (en) * 2015-05-18 2016-11-24 Schott Ag Sensitized, photo-sensitive glass and its production
US20170210665A1 (en) * 2016-01-26 2017-07-27 Corning Incorporated Photosensitive glasses and glass ceramics and composite glass materials made therefrom
EP3770130A1 (fr) * 2018-10-26 2021-01-27 CDGM Glass Co. Ltd. Verre microcristallin, produit de verre microcristallin et procédé de fabrication associé

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7262144B2 (en) 2003-02-03 2007-08-28 Schott Ag Photostructurable body and process for treating a glass and/or a glass-ceramic
DE102014119594A1 (de) 2014-12-23 2016-06-23 Schott Ag Borosilikatglas mit niedriger Sprödigkeit und hoher intrinsischer Festigkeit, seine Herstellung und seine Verwendung
US20160340228A1 (en) * 2015-05-18 2016-11-24 Schott Ag Sensitized, photo-sensitive glass and its production
US20170210665A1 (en) * 2016-01-26 2017-07-27 Corning Incorporated Photosensitive glasses and glass ceramics and composite glass materials made therefrom
EP3770130A1 (fr) * 2018-10-26 2021-01-27 CDGM Glass Co. Ltd. Verre microcristallin, produit de verre microcristallin et procédé de fabrication associé

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
"Chemical structure, medium range order, and crystalline reference state of multicomponent oxide liquids and glasses", JOURNAL OF NON-CRYSTALLINE SOLIDS, vol. 345-346, 15 October 2004 (2004-10-15), pages 16 - 23
C.A. ANGELL: "Structural Instability and Relaxation in Liquid and Glassy Phases near the fragile liiquid limit", JOURNAL OF NON-CRYSTALLINE SOLIDS, vol. 102, 1988, pages 205 - 221

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