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WO2002059050A1 - Procede et dispositif de mesure dans un processus de fabrication de revetement de verre plat - Google Patents

Procede et dispositif de mesure dans un processus de fabrication de revetement de verre plat Download PDF

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Publication number
WO2002059050A1
WO2002059050A1 PCT/FI2002/000012 FI0200012W WO02059050A1 WO 2002059050 A1 WO2002059050 A1 WO 2002059050A1 FI 0200012 W FI0200012 W FI 0200012W WO 02059050 A1 WO02059050 A1 WO 02059050A1
Authority
WO
WIPO (PCT)
Prior art keywords
substrate
aerosol particles
coating
flame
current measurement
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/FI2002/000012
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English (en)
Other versions
WO2002059050A8 (fr
Inventor
Juha Tikkanen
Jorma Keskinen
Markku Rajala
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Liekki Oy
Original Assignee
Liekki Oy
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Liekki Oy filed Critical Liekki Oy
Publication of WO2002059050A1 publication Critical patent/WO2002059050A1/fr
Anticipated expiration legal-status Critical
Publication of WO2002059050A8 publication Critical patent/WO2002059050A8/fr
Ceased legal-status Critical Current

Links

Classifications

    • 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
    • G02B6/132—Integrated optical circuits characterised by the manufacturing method by deposition of thin films
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00—Other methods of shaping glass
    • C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
    • C03B19/1415—Reactant delivery systems
    • C03B19/1423—Reactant deposition burners
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/30—For glass precursor of non-standard type, e.g. solid SiH3F
    • C03B2207/34—Liquid, e.g. mist or aerosol
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/46—Comprising performance enhancing means, e.g. electrostatic charge or built-in heater

Definitions

  • the invention relates to a measurement method in a process for manufacturing a planar glass coating, especially a glass coating suitable for planar waveguides, as presented in the preamble of the appended claim 1.
  • the invention also relates to a device according to the preamble of the appended claim 11 for implementing the aforementioned method.
  • An optical planar waveguide is produced by forming superimposed glass layers with different refractive indexes on the top of a suitable substrate, for example a silicon wafer.
  • a so-called undercladding is first made of glass on top of the silicon wafer, on top of which a core layer having a slightly higher optical refractive index than said undercladding is formed.
  • a desired waveguide pattern is formed for example by means of photolithographic methods.
  • a third layer i.e. a so-called upper cladding having a slightly lower refractive index is formed on top of the core layer.
  • the waveguide structure formed thereby light propagates in the core layer in the same way as in the core of an optical fibre.
  • planar waveguides are at present quite widely used in different kinds of applications.
  • data processing and telecommunications technology as well as different measurement and sensor applications.
  • Planar waveguides enable the packing of optical structures and elements on the same substrate in a small space as a compact entity, which, in addition to the small size, may have advantages such as small optical signal losses and high operating speed.
  • advantages such as small optical signal losses and high operating speed.
  • planar waveguides it is possible to attain advantages similar to the ones attained with conventional integrated circuits, in which only electric components are used within the same substrate.
  • it is, in addition to the optical components and structures also possible to combine electrical components and structures in the same substrate in optical planar waveguides.
  • FHD flame hydrosis deposition
  • US patent 5,622,750 discloses a method of forming the glass layers required in planar waveguides by means of the FHD method.
  • the reactants necessary in the manufacture of glass are mixed together to form a solution, from which solution aerosol droplets are formed which are guided further with a carrier gas to a burner and to a flame.
  • the aerosol droplets form aerosol particles (glass soot) which are further thermophoretically guided on the substrate to be coated, thus forming a glass material coating.
  • the substrate itself can be made of a semiconductor, glass or ceramic material.
  • the substrate is moved back and forth on a plane transverse to the flame during the coating process which may take, for example, about one hour to make one coating layer.
  • the coating layer is sintered to form a dense glass layer by heat-treating the substrate at high temperature.
  • the homogenous quality of the glass layers contained in the planar waveguide has a very central meaning in the optical properties of the planar waveguide and further in the usability of the planar waveguide.
  • the mechanical properties of different glass layers of the planar waveguide for example the thermal expansion properties, must be adapted so that they are suitable for each other to attain durable structures. All the aforementioned factors require a very precise control of the manufacturing process.
  • the control parameters relating to the thermal reactor itself are for example the mixture ratios and flow rates of combustion gases necessary in the production of a flame, or when plasma is used, the electric parameters (for example input current and input voltage determining the electrical power) affecting the flame arc (or the like) as well as the mixture ratios and flow rates of plasma gases.
  • the formation of the glass material itself (aerosol particles) in the thermal reactor is affected by the mixture ratios and feed rates of the gaseous and/or liquid reactants necessary in the formation of the glass as well as by the process used in the formation of the aerosol droplets.
  • the feed rate of the carrier gas/gases used for feeding reactants in the thermal reactor is also a central control parameter in the process, as well as the control of the vapour pressure of the reactants when gaseous reactants are used.
  • the aforementioned vapour pressure is affected for instance by the temperature of the reactants, as well as the prevailing pressure affecting the same.
  • the main purpose of the present invention is to introduce a new realtime (on-line) measurement method to be used during the process of manufacturing a planar glass coating used especially in planar waveguides, which measurement method enables a more accurate control of the manufacturing process and adjustment of the process parameters by means of feedback coupling, when compared to prior art.
  • the method according to the invention is primarily characterized in what will be presented in the characterizing part of the independent claim 1.
  • the device according to the invention is primarily characterized in what will be presented in the characterizing part of the independent claim 11.
  • the invention is essentially based on the idea that the measurement is implemented by means of aerosol particles accumulating on the substrate to be coated, wherein by means of the measurement it is possible to detect the changes possibly occurring both in the formation of the aerosol particles and in the movement of the same on the substrate. According to the invention, this measurement is based on determining the electric charge conveyed to the substrate by the aerosol particles forming the coating by means of sensitive current measurement.
  • the measurement is based on the electric charge attained intrinsically by the aerosol particles during their formation. It is an advantage of this embodiment that a separate charger is not necessary for electrical charging of the aerosol particles.
  • a separate charger for example a so-called corona charger is used for charging the aerosol particles.
  • a separate charger for example a so-called corona charger is used for charging the aerosol particles.
  • the act of determining the electric charge conveyed by the aerosol particles to the substrate according to the invention can take place by connecting a sensitive current measurement means to a substrate galvanically, which substrate is electrically isolated from a base, or the like, supporting the substrate.
  • the measurement can also be conducted in such a manner that the current measurement means detects the charge of the substrate by means of so-called Faraday cage without a galvanic connection to the substrate itself.
  • the invention also enables an adjustment of the process parameters of the coating process by means of feedback coupling to stabilize the coating conditions, thus making it possible to manufacture for example optical planar waveguides of high quality.
  • the significance of this is emphasized especially in such coating processes, in which the production of a desired coating layer requires a continuous maintenance of the process for a long period of time.
  • Fig. 1 illustrates in principle a preferred embodiment of the invention
  • Fig. 2 illustrates in principle another embodiment of the invention.
  • FIG. 1 shows in principle an embodiment of the invention.
  • the thermal reactor 10 is a flame, which is produced by burning combustible and oxidizing combustion gases 11 by means of a burner 22. It is possible to use for example hydrogen + oxygen or methane + oxygen as combustion gases 11.
  • the reactants 12 necessary in the formation of the glass material are brought to the flame 10 for example in aerosol droplets along with a carrier gas, which said aerosol droplets are in the flame 10 further transformed into aerosol particles 13 necessary in the formation of the glass coating.
  • the reactants 12 necessary in the formation of the glass material can be for example silicon or germanium tetrachloride, or chlorine-free reactants such as TEOS, tetraethylortosilicate or GEOS, tetraethoxygermanium in a suitable format.
  • the reactants 12 can, in addition to the above- mentioned agents, also contain rare earth metals and lanthanides, such as erbium and/or neodymium, as well as aluminium, phosphorus, borium and/or fluorine in a suitable format.
  • the aerosol particles 13 produced from the reactants 12 move from the flame towards a substrate 14, which substrate 14 can be made of silicon, quartz or another semiconductor, glass or ceramic material suitable for the purpose.
  • the substrate 14 is a thin, round wafer, for example a silicon wafer, but it is also possible to use substrates of another shape.
  • the aerosol particles 13 hit the substrate 14, they adhere on the substrate 14, thus forming a coating.
  • the flame 10 By moving the flame 10 with respect to the substrate 14, it is possible to attain either a coating layer with a uniform thickness on the entire surface area of the substrate 14, or the thickness of the coating layer can be adjusted, if necessary, so that it is different in different sections of the surface of the substrate 14.
  • the local properties of the coating layer can also be changed, if necessary, by varying the supply/composition of the reactants 12 when the flame 10 is moved with respect to the substrate 14.
  • the movement between the substrate 14 and the flame 10 can be attained by any suitable solution obvious for anyone skilled in the art, either by arranging the burner 22 or the base 16 of the substrate 14 movable for example by means of a stepper motor driven manipulator.
  • the substrate 14 is attached on top of the base 16. If the base 16 is made of conductive material, the substrate 14 is electrically isolated from the base 16 by means of a non-conductive layer 15.
  • the non-conductive layer 15 can be made of for example aluminium oxide (Al 2 0 3 ), sapphire, quartz, teflon or nylon.
  • the contact between the substrate 14 and the base 16 and the non-conductive layer 15 used therebetween is of such a quality, that a good thermal conductivity is attained between the substrate 14 and the base 16. This is necessary especially in such a case if the base 16 is arranged to be heated and/or cooled to adjust the temperature of the substrate 14 and control the coating process.
  • the electric charge produced on the substrate by the aerosol particles 13 hitting the surface of the substrate 14 is measured during the process to measure the amount of glass material accumulated on the substrate 14, and to monitor/control the coating process in real time.
  • the aforementioned measurement is conducted by means of a sensitive current measurement means 17, a so-called electrometer.
  • the current measurement means 17 is galvanically connected to the substrate 14, said substrate 14 being electrically isolated from the base 16 by means of a non-conductive layer 15.
  • the current measurement means 17 can be implemented by means of any method known as such.
  • One electrometer based on the use of a current-voltage converter is disclosed for example in the doctoral thesis by Mikko Moisio: Real Time Size Distribution Measurement of Combustion Aerosols, published by Tampere University of Technology, ISBN 952-15-0328-9, 1999, pp. 37 to 39.
  • the measurement is based on the electric charge obtained by the aerosol particles 13 during the formation of the particles.
  • the advantage of this embodiment is that a separate charger is not necessary for electrical charging of the aerosol particles 13.
  • the aerosol particles 13 produced in the thermal reactor 10 are always intrinsically electrically charged. This results for example from the free ions occurring in the thermal reactor 10, for example in the flame, which also participate and/or electrically interact with the aerosol particles 13 that are being produced.
  • the different chemical reactions occurring in the thermal reactor also produce charged ions and particles.
  • the charge transfer between ions, particles, etc. can take place either by collisions or as a charge transfer without collisions.
  • Fig. 2 illustrates in principle another embodiment of the invention in which a separate charger 23 is used to electrically charge the aerosol particles 13 formed in the flame 10.
  • the charger 23 can be for example a charger based on a corona discharge, or another known method of charging the aerosol particles that is obvious for anyone skilled in the art.
  • the function of the charger can be based for example on the use of a so-called triode charger.
  • One method based on the use of a corona discharge is disclosed for example in the doctoral thesis by Mikko Moisio: Real Time Size Distribution Measurement of Combustion Aerosols, published by Tampere University of Technology, ISBN 952- 15-0328-9, 1999, pp. 21 to 30.
  • the current measurement means 17 detects the charge of the substrate by means of a so-called Faraday cage 24 without a direct galvanic connection to the substrate 14.
  • the measurement based on the Faraday cage 24 can be understood by considering the cage as an electrically closed chamber, on the wall of which the current measurement means 17 is galvanically connected.
  • the current measurement means 17 attached to the chamber also shows a reading corresponding to the same.
  • the charge conveyed by the aerosol particles 13 is detected by means of the current measurement means 17, as the particles enter a Faraday cage 24 and adhere on the surface of the substrate 14.
  • the Faraday cage 24 By means of the Faraday cage 24 it is possible to measure the charge also in materials which are electrically non-conductive. In other words, the Faraday cage makes it possible to measure the charge collected on the substrate 14 in a situation in which the substrate 14 and/or the coating formed on the substrate is/are made of electrically non- conductive material/materials.
  • the function of the current measurement means 17 and the possible charger 23 is controlled by means of a control unit 18.
  • the control unit 18 is arranged to determine the amount of glass material brought by the aerosol particles 13 accumulated on the substrate substantially in real time by means of a signal given by the current measurement means 17, and further to adjust for example the movement of the base 16 (control 19 in Figs 1 and 2) and/or the heating of the base 16 (control 20 in Figs 1 and 2) and/or the set parameters of the thermal reactor 10 (for example the mixture ratios and/or flow rates of the combustion gases 11 and/or reactants 12 and/or the amounts of carrier gas/carrier gases in the reactants 12) to attain a coating of a desired quality on the substrate 14.
  • the signal given by the current measurement means 17 is primarily dependent on the amount of aerosol particles 13 accumulated on the substrate 14. Because the charge of single aerosol particles 13 is substantially directly proportional to the size of the aerosol particles 13 when a separate charger 23 is used, the signal given by the current measurement means 17 is thus also proportional to the amount of glass material accumulated on the substrate 14. On the basis of the aforementioned measurement signal it is thus for example possible to control the moving of the substrate 16 in such a manner that the same amount/mass of aerosol particles 13 is attained on different locations in the substrate 14.
  • the variation of the measurement signal given by the current measurement means 17 as a function of time indicates the disturbance/disturbances in the function of the process forming the aerosol particles 13 and/or in the movement of the aerosol particles on the substrate 14.
  • the control unit 18 may attempt to eliminate said disturbance by adjusting the set parameters of the process and/or the control unit 18 can also give an alarm for the user monitoring the process.
  • the formation/growth of the coating layer is terminated either by turning off the flame 10 entirely or by terminating the supply of reactants 12 used in the production of aerosol particles to the flame 10 and/or by moving the substrate aside 14 from underneath the jet of aerosol particles 13.
  • the coating layer on the surface of the substrate 14, which at this stage is still a porous layer composed of particles that have melted together only partly, is sintered to form a dense glass material for example by transferring the substrate 14 to a separate oven, in which the sintering is conducted by means of known methods by increasing the temperature of the substrate 14 in such a manner that the glass material particles accumulated on the substrate melt together, thus forming a homogenous glass layer.
  • the invention is not, of course, restricted solely to the use of a flame as a thermal reactor 10, as presented in the examples above.
  • the thermal reactor 10 can also be any other method obvious for anyone skilled in the art for producing such a high local temperature, in which corresponding reactions that generate aerosol particles are produced. Such possibilities include for example different kinds of plasmas, which can be produced for example by means of an electric current or laser light.
  • the reactants 12 necessary in the production of a glass material can also be introduced to the process in any other way known as such.
  • the thermal reactor 10 together with the substrate 14 can be isolated from the ambient atmosphere inside a chamber or a corresponding arrangement, which is shown in principle by broken lines in Figs 1 and 2.
  • Said chamber or the like enables the act of creating such conditions for the coating process that differ from the ambient atmosphere as far as the composition of the gases and/or temperature and/or pressure is/are concerned.
  • said walls, as well as other parts of the device can be arranged to be heated in sections where necessary for example by means of electric resistors.
  • the aforementioned walls of the chamber can also be equipped with a shielding gas flow to prevent wall contamination, in which shielding gas flow the shielding gas is arranged to flow in a laminar flow in the vicinity of the wall, or the walls of the chamber are for example made of a porous metal or quartz material, the shielding gas discharged through the pores of said wall preventing the aerosol particles 13 from adhering on the walls of the chamber.
  • the thermal reactor 10 is a flame spray gun as disclosed in the Finnish patent No. 98832 and in the international patent application PCT/FI 99/00818, in which flame spray gun some of the reactants 12 necessary in the formation of the glass material can be conveyed to the flame 10 in liquid format in such a manner that said reactant/reactants are atomized into aerosol droplets only in the immediate vicinity of the flame 10, right before they are conveyed to the flame 10.
  • the advantage attained hereby is that the single droplets supplied to the flame 10 contain the different components of the used liquid reactant precisely in the original ratio of said components, because the vapour pressures of these components that differ from each other do not have time to affect the composition of the aerosol droplets through evaporation occurring in a different manner.
  • a further advantage is that in the case of said flame spray gun it is possible to supply larger amounts of components in the flame 10 when compared to such methods in which the aerosol droplets are formed further away from the flame 10 and conveyed to the flame 10 with the carrier gas.
  • the sizes of the aerosol particles tend to grow during the conveying for example as a result of coagulation or agglomeration before the aerosol droplets end up in the flame 10.
  • deposition occurs on the walls of the conveying channel that is being used, for example on the walls of a tubing, and in this way the conveying channel also tends to become contaminated, which makes the control of the process even more difficult.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • General Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Surface Treatment Of Glass (AREA)
  • Coating Apparatus (AREA)

Abstract

L'invention concerne un procédé et un dispositif de mesure, destinés à être mis en oeuvre dans le cadre d'un processus de fabrication d'un revêtement de verre plan. Dans ce processus de fabrication, un réacteur thermique (10), par exemple à flamme ou à plasma, est utilisé pour produire des particules d'aérosol (13) à partir de réactants (12), ces particules d'aérosol (13) étant guidées sur la surface d'un substrat (14) pour former un revêtement. Selon l'invention, la charge électrique acheminée sur le substrat (14) par la pénétration des particules d'aérosol (13) est mesurée au moyen d'un dispositif de mesure de courant (17) pendant ledit processus, afin de surveiller le processus d'enduction. Ce dispositif de mesure de courant (17) est disposé de façon à communiquer avec une unité (18) de commande de processus, en vue d'adapter les conditions du processus conformément à une valeur seuil prédéterminée. Dans un mode de réalisation, la mesure est basée sur la charge électrique atteinte de manière intrinsèque par les particules d'aérosol (13) pendant leur formation. Il est également possible, le cas échéant, d'utiliser un chargeur séparé (23), par exemple un chargeur dit chargeur corona, pour charger les particules d'aérosol (13).
PCT/FI2002/000012 2001-01-09 2002-01-08 Procede et dispositif de mesure dans un processus de fabrication de revetement de verre plat Ceased WO2002059050A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FI20010036A FI112648B (fi) 2001-01-09 2001-01-09 Mittausmenetelmä ja -laitteisto tasomaisen lasipinnoitteen valmistusprosessissa
FI20010036 2001-01-09

Publications (2)

Publication Number Publication Date
WO2002059050A1 true WO2002059050A1 (fr) 2002-08-01
WO2002059050A8 WO2002059050A8 (fr) 2003-10-30

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PCT/FI2002/000012 Ceased WO2002059050A1 (fr) 2001-01-09 2002-01-08 Procede et dispositif de mesure dans un processus de fabrication de revetement de verre plat

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FI (1) FI112648B (fr)
WO (1) WO2002059050A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009030234A1 (de) * 2009-06-23 2010-12-30 J-Plasma Gmbh Verfahren zur Herstellung von Glas insbesondere Glaspreform und Smoker zu dessen Herstellung

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5844361A (ja) * 1981-09-11 1983-03-15 Toshiba Corp 粉体の帯電量測定装置
US4816285A (en) * 1984-02-10 1989-03-28 Prazisions-Werkzeuge Ag Method and apparatus for measuring a quantity of particles deposited on a metal body to be coated with powder
US5296255A (en) * 1992-02-14 1994-03-22 The Regents Of The University Of Michigan In-situ monitoring, and growth of thin films by means of selected area CVD

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5844361A (ja) * 1981-09-11 1983-03-15 Toshiba Corp 粉体の帯電量測定装置
US4816285A (en) * 1984-02-10 1989-03-28 Prazisions-Werkzeuge Ag Method and apparatus for measuring a quantity of particles deposited on a metal body to be coated with powder
US5296255A (en) * 1992-02-14 1994-03-22 The Regents Of The University Of Michigan In-situ monitoring, and growth of thin films by means of selected area CVD

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE102009030234A1 (de) * 2009-06-23 2010-12-30 J-Plasma Gmbh Verfahren zur Herstellung von Glas insbesondere Glaspreform und Smoker zu dessen Herstellung

Also Published As

Publication number Publication date
FI112648B (fi) 2003-12-31
FI20010036L (fi) 2002-07-10
FI20010036A0 (fi) 2001-01-09
WO2002059050A8 (fr) 2003-10-30

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