EP0704249A1 - Device for distributing pulverulent solids on the surface of a substrate for coating this substrate - Google Patents

Device for distributing pulverulent solids on the surface of a substrate for coating this substrate Download PDF

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Publication number
EP0704249A1
EP0704249A1 EP95402160A EP95402160A EP0704249A1 EP 0704249 A1 EP0704249 A1 EP 0704249A1 EP 95402160 A EP95402160 A EP 95402160A EP 95402160 A EP95402160 A EP 95402160A EP 0704249 A1 EP0704249 A1 EP 0704249A1
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EP
European Patent Office
Prior art keywords
gas
powder
flow
nozzle
conduits
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Granted
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EP95402160A
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German (de)
French (fr)
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EP0704249B1 (en
Inventor
Jean-François Oudard
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Saint Gobain Vitrage SA
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Saint Gobain Vitrage SA
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05BSPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/14Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas designed for spraying particulate materials
    • B05B7/1404Arrangements for supplying particulate material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05BSPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B12/00Arrangements for controlling delivery; Arrangements for controlling the spray area
    • B05B12/02Arrangements for controlling delivery; Arrangements for controlling the spray area for controlling time, or sequence, of delivery
    • B05B12/04Arrangements for controlling delivery; Arrangements for controlling the spray area for controlling time, or sequence, of delivery for sequential operation or multiple outlets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05BSPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B12/00Arrangements for controlling delivery; Arrangements for controlling the spray area
    • B05B12/08Arrangements for controlling delivery; Arrangements for controlling the spray area responsive to condition of liquid or other fluent material to be discharged, of ambient medium or of target ; responsive to condition of spray devices or of supply means, e.g. pipes, pumps or their drive means
    • B05B12/12Arrangements for controlling delivery; Arrangements for controlling the spray area responsive to condition of liquid or other fluent material to be discharged, of ambient medium or of target ; responsive to condition of spray devices or of supply means, e.g. pipes, pumps or their drive means responsive to conditions of ambient medium or target, e.g. humidity, temperature position or movement of the target relative to the spray apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05BSPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/14Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas designed for spraying particulate materials
    • B05B7/1404Arrangements for supplying particulate material
    • B05B7/1477Arrangements for supplying particulate material means for supplying to several spray apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05BSPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
    • B05B7/00Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
    • B05B7/14Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas designed for spraying particulate materials
    • B05B7/1481Spray pistols or apparatus for discharging particulate material
    • B05B7/1486Spray pistols or apparatus for discharging particulate material for spraying particulate material in dry state

Definitions

  • the present invention relates to a device for distributing powdery solids on the surface of a substrate, in particular glass, in order to coat it with thin layers capable of giving it optical, thermal or electrical properties.
  • This device makes it possible in particular to deposit these thin layers by a technique known as powder pyrolysis consisting in spraying said pulverulent solids (in general organo-metallic compounds), in suspension in a gas, in the direction of a substrate heated to high temperature, so that they decompose (usually in the form of metal oxide) on contact.
  • the substrate can take the form of a continuous ribbon of glass called float, at the exit from the glass float enclosure, the device then usually comprising a nozzle comprising a cavity which passes right through it and which ends in a distribution slot above the ribbon and transversely to its axis of travel, the nozzle being equipped with suitable powder supply means.
  • the float glass ribbon to be covered usually has a width of at least 2 meters, in particular of the order of three to four meters. It is therefore over this width, which is considerable, that the nozzles have to distribute the gas / powder suspension in the most homogeneous manner possible to ensure, at least transversely to the axis of travel of the ribbon, a certain consistency in the quality and / or thickness of the coating deposited.
  • Many studies have already been carried out, aiming either at the very design of the nozzle, or at its mode of supplying powder, to best guarantee this homogeneity.
  • patent EP-B-0 130 919 has developed an efficient distribution means making it possible to fairly uniformly subdivide a vein of powder in suspension conveyed in a single supply duct into a plurality of powder veins conveyed in as many secondary conduits coming to feed the nozzle over its entire width by means of supply members called injectors into which they open. It is however difficult to guarantee that each of the veins has a perfect identity with all the others, in terms of flow rate of powder transported, and that all of the veins will be able to “melt” into a perfectly homogeneous stream of powder at the level of the nozzle distribution slot.
  • Patent EP-B-0 392 902 then proposed a device making it possible to automatically modify the relative positions of the injectors arranged in line at the inlet of the nozzle, by removing or bringing together the injectors concerned as soon as a variation of local thickness in the coating deposited “downstream” from the nozzle.
  • This solution gives interesting results, but is not yet fully optimal, firstly because it may seem a little complicated to implement, then and above all because it tries to compensate for any disparities in the flow of the veins. without really correcting them.
  • the object of the invention is therefore to further improve the operating mode of powder distribution devices of this type, and in particular to achieve optimization of the homogeneity of the flow of the powder-gas suspension in the nozzle without sacrificing too much. simplicity of implementation, in order to obtain quality coatings, particularly in terms of thickness regularity.
  • the subject of the invention is a device for distributing powdery solid suspended in a gas, with a view to depositing a coating, in particular by pyrolysis, on a moving substrate, in particular of the float glass ribbon type.
  • This device includes on the one hand, a dispensing nozzle whose walls define a cavity which ends in a longitudinal dispensing slot. It also comprises a main powder supply pipe provided with a distribution means.
  • a plurality of secondary powder supply conduits connected to this main conduit by means of distribution means makes it possible to supply powder to the cavity of the nozzle over its entire length.
  • at least part of the secondary conduits is equipped with at least one pneumatic means capable of modulating the flow rate of the powder-gas suspension that each of the secondary conduits concerned is intended to convey.
  • each of the conduits is equipped with such a pneumatic means.
  • This solution has two major advantages: on the one hand, being able to modulate the flow rate in each of the conduits will make it possible to genuinely and directly correct any disparities in flow rate between the gas-powder mixture streams that they transport to the nozzle, and thus ensuring a very regular distribution in the powder supply at the nozzle, over the entire length of its cavity.
  • using pneumatic rather than mechanical means to operate these flow modulations is very advantageous.
  • a mechanical means of the valve type operates on the principle of a partial blockage of the conduit, a blockage which, in the case of a flow of powder, causes untimely local accumulations of powder, blockages or blockages which can cause sudden and uncontrolled high pressure losses in the flow.
  • a pneumatic means makes it possible to modulate a flow rate of powder-gas mixture in a fine and controlled manner and can be adjusted with very short response times, with appropriate adjustment means, which can be manual or automated.
  • These means if they are chosen to be automated, can advantageously form part of a regulation loop, under the control of a control unit connected to at least one quality or thickness measurement means on the coating deposited on the substrate, using the dispensing nozzle.
  • the regulation in the powder flow rates of the secondary conduits can be carried out continuously, by very quickly adjusting the flow rate of the appropriate secondary conduit (s) using their pneumatic means. as soon as a variation in transverse thickness is detected in the coating deposited on the strip just downstream of the nozzle.
  • pneumatic means may simply be in the form of auxiliary supply conduits opening into the secondary conduits, auxiliary supply which is advantageously provided with a manual or automated means for regulating gas flow or pressure, using for example valves. Insofar as they only carry gas, this type of mechanical adjustment means does not cause any problems.
  • These feeds thus introduce a flow of gas into the flow of the powder-gas mixture from the secondary conduits, the characteristics of which are controlled in order to create a controlled pressure drop thereby allowing the flow to be more or less reduced when necessary. . Thanks to an appropriate distribution means, the quantity of powder which is no longer conveyed by the conduit due to this induced reduction in flow rate will be able to be distributed homogeneously over all the other secondary conduits.
  • These secondary conduits may advantageously comprise pipes, preferably flexible, connected to the distribution means of the main supply pipe, pipes whose ends opening out at the entrance to the cavity of the nozzle are constituted by supply members called " rigid injectors, preferably metallic.
  • the auxiliary gas supply means can then open into the secondary conduits at any point, either at the level of these (flexible) pipes, “downstream” from the distribution means of the main conduit, either near or in the nozzle, in particular at the pipe-injector junction or at the injector itself. It is this latter configuration which is more favorable, since the rigid injector allows an easy and safe "connection" of the auxiliary gas supply.
  • a preferred embodiment of the invention thus consists of a distribution device, where each of the secondary conduits intended to convey the powder-gas suspensions is provided at its end with an injector, the injectors being regularly arranged in line in the inlet port of the nozzle cavity over its entire length and all being provided with an auxiliary gas supply with variable flow.
  • the nozzle cavity is also provided with means for injecting pressurized gas to drive the powder-gas suspension emitted by the injectors into the cavity, means for injecting preferably arranged symmetrically on either side of the injector line.
  • the invention also relates to the method of implementing the device described above, and in particular the various ways of controlling and regulating the pneumatic means equipping the secondary conduits.
  • these pneumatic means are in the form of auxiliary gas inlets opening into the conduits, it is thus possible to adjust each of the auxiliary gas jet flow rates separately for each of them, and this in a range of flow rates which can range from example between 0 and 100% of a predetermined flow value. It is indeed necessary that these gas jets have a “braking” action on the flow of powder in the conduit, in order to create a pressure drop there and not a depression which would cause an acceleration of the flow.
  • the injection rates, speeds and directions of these auxiliary gas jets relative to those of the powder-gas mixture flow must therefore be carefully selected.
  • a first possibility is to operate "all or nothing". If no local disparity in the flow rates of the conduits, resulting in a local variation in coating thickness, is detected, the flow rate of these jets of auxiliary gas is zero. If a disparity appears, locally causing excess thickness in the coating, the pneumatic means of the secondary conduit or conduits involved intervenes to deliver an auxiliary gas jet of suitable flow rate which cannot exceed a certain value, in order to sufficiently reduce the powder flow rate of the or conduits to remove this excess thickness.
  • a second possibility is to permanently operate all of the pneumatic means, which all emit, when no disparity is detected, an auxiliary gas jet of given flow rate. They therefore all exert a certain permanent “braking” effect on the flows of powder-gas mixture in the conduits, which can be compensated for if necessary by adapting accordingly the flow rate of powder-gas mixture in the main supply conduit. . It is thus possible to regulate the flow rate of the gas jets auxiliary around this given flow value. This operating mode is more flexible and leaves more room for maneuver, since it is possible to correct both local coating thicknesses (by increasing the emission rate of the appropriate auxiliary gas jet) as well as local thickness decreases said coating (this time reducing the emission rate of the appropriate auxiliary gas jet).
  • the flow value around which the flow of each of the auxiliary gas jets is regulated is approximately 20 to 60% of the average gas flow of the powder-gas suspension conveyed by each. secondary ducts.
  • a value of around 50% is chosen, with a regulation of the flow rate of each of the auxiliary gas jets of ⁇ 50% around this value.
  • the term “average” flow is understood to mean their theoretical flow, if no disparity in flow between conduits could exist.
  • the device and method for implementing the latter can be advantageously used in view of depositing coatings based on metal oxide, by pyrolysis on a strip of hot float glass, in particular coatings of doped oxides of SnO2 type: F , for example from a powder of dibutyltin difluoride (DBTF) or of the ITO type from powder of indium formate and tin dibutyloxide.
  • DBTF dibutyltin difluoride
  • ITO indium formate and tin dibutyloxide.
  • the installation as shown as a whole in FIG. 1 makes it possible to regularly distribute pulverulent solids of all kinds on various substrates, especially large dimensions.
  • it is used to distribute a powder of organo-metallic compounds on a ribbon 1 of hot float glass leaving the enclosure of the floating bath, ribbon passing over a bed of rollers 2 according to a axis given at a uniform speed.
  • the powder thus brought into contact with the surface of the hot glass decomposes therein to leave a coating based on metal oxide (s).
  • the installation according to FIG. 1 therefore represents a hopper 3 for storing powder 4 to be distributed, a mixer 5 in which the powder-gas mixture is produced, generally air in order to constitute a suspension as homogeneous as possible of the powder in the gas by means of an air inlet 25 and an endless screw 26 supplied with powder by the hopper 3.
  • a main inlet duct 6 conveys the powder-gas suspension at the outlet of the mixer 5, a distribution means 7 subdividing the single powder-gas suspension stream brought by the pipe 6 into a plurality of secondary streams as uniform as possible, a plurality of flexible secondary pipes 8 conveying these to the nozzle distribution 24.
  • This nozzle is arranged transversely to the axis of travel of the glass ribbon 2 and defines a transverse cavity whose length corresponds to the width of the ribbon to be coated.
  • the secondary conduits 8 open into metal injectors 9 arranged in line at the entrance to this cavity.
  • injectors 9 projecting a stream of gas-powder mixture at the inlet 10 of the cavity 11 defined by the inner walls 12 of the nozzle, flat walls and slightly convergent to the distribution slot 13 located a few millimeters from the surface of the glass ribbon 1.
  • Means for injecting gas under pressure are also provided on either side of the line of injectors 9, in order to facilitate the “curtain” distribution of powder and the driving of the powder-gas suspension jets coming from the injectors 9.
  • These means are formed by a series of chambers 14 located symmetrically in the nozzle body and connected by a ramp 15 to a source of gas, air in general.
  • chambers are interconnected by a partition 16 forming a spacer, provided with a means for passing gas, for example using porous materials, and by orifices 17.
  • the chambers 18 located in the upper part of the nozzle open into the cavity 11 by slots 19 near the injectors 9, so as to inject the gas under pressure substantially parallel to the walls 12, slots limited by lips 20, of suitable configuration.
  • each of the injectors 9 consists schematically of a hollow metal cylinder into which each of the secondary conduits 8 opens in a sealed manner.
  • These injectors further include an air type gas inlet in the form of an auxiliary conduit 22 coming into it, preferably with a configuration such between injector 9 and conduit 22 that the jet of powder-gas mixture in the injector and the gas jet that can emit the conduit 22 in the injector 9 make between them an angle a between 5 and 90 °, preferably about 30 °. It is in fact preferable that this angle remains less than 90 ° in order to avoid any risk of traces of powder seeping into the duct 22, traces which can in particular disturb the proper functioning of the flow control means which equip it .
  • Each auxiliary duct 22 is supplied by a suitable gas source, not shown.
  • Each of the conduits connected to a source of gas, in particular air, external to the nozzle is provided with a flow control means of the solenoid valve type.
  • This adjustment means (for example of the flow meter type associated with a magnetic valve) is controlled by a control unit as a function of the thickness variations detected downstream of the nozzle on the coating 23.
  • This detection can be carried out by continuous or by time interval given using one or more means of thickness measurement of the reflectometers type (either a reflectometer mounted movable above the glass ribbon in order to “sweep” the width of the coating, or several reflectometers arranged in line above the ribbon.
  • the mode of operation of the nozzle 24 is explained with the aid of an implementation example, consisting of depositing a layer of SnO2: F 200 nm thick from a tin dibutyldifluoride powder (DBTF).
  • the mass flow of powder of D.B.T.F. conveyed in the main supply conduit 6 is between 3 and 10 kg / hour / linear meter of nozzle.
  • the volume flow rate of the gas in which it is suspended is between 3 and 80 m3 / hour / linear meter of nozzle.
  • the flow of pressurized gas injected through the slots 19 into the cavity is between 200 and 500 m3 / h / linear meter of nozzle.
  • each secondary conduit would convey a gas stream whose mass flow rates in D.B.T.F. and gas volume would be exactly equal to the ratio of those of the suspension conveyed in the main supply duct to the number of secondary ducts.
  • differences in flow can appear between the jets of powder-gas mixture coming from each of the injectors 9, differences leading to excess thicknesses or, on the contrary, local decreases in the thickness of coating deposited relative to the average thickness of 200 nm sought.
  • These transverse variations in the thickness of the coating are detrimental to its quality, because they can, in particular, cause optical defects, of the iridescence type, which are not very aesthetic.
  • a powder-gas flow coming from the secondary pipe 8 is constantly passing through each of the injectors 9, presenting a gas flow rate of approximately 2 m3 / h and a gas jet emitted by the auxiliary pipe 22 of a volume flow rate in given gas, in particular around 1 m3 / h.
  • the control unit controls the valve of the line (s) 22 of the injectors 9 concerned to reduce the flow rate of the auxiliary gas jet .
  • the flow rate of each of the auxiliary gas jets can vary between for example 0.5 and 1.5 m3 / h.
  • the control unit (or the operator) can use charts giving direct correspondence between thickness variation in the coating and flow variation in the conduits 22, without even having to measure precisely the flow rates of powder which pass in the conduits 8 then the injectors 9.
  • any irregularity in the thickness of the coating can thus be quickly corrected, remotely, manually, automated or semi-automated.
  • the flow control of the powder-gas suspension coming from each of the secondary conduits 8 is regulated by the auxiliary gas jet of each of the conduits 22, without any problem of clogging or clogging of the secondary conduit or of detrimental impact on the supply of other secondary conduits.
  • the powder flow is reduced in the secondary duct 8 adhoc to correct an excess thickness in the coating, the “excess powder” not delivered by the duct, the flow of which has been reduced will be distributed regularly on all the other conduits at the level of the distribution means.
  • the powder supply mode uses the pneumatic means of the invention in order to improve the uniformity in the thickness of the coating deposited. But we could just as easily, without departing from the scope of the invention, use these pneumatic means to create, this time in a voluntary and controlled manner, gradients in the thickness of the coating deposited, at least transversely to the axis substrate travel, if it proved useful or advantageous to manufacture coatings having such characteristics.

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  • Nozzles (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Coating Apparatus (AREA)
  • Details Or Accessories Of Spraying Plant Or Apparatus (AREA)
  • Glanulating (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The distributor consists of a nozzle (24) with its walls forming a cavity which ends in a lengthwise slit, and a powder delivery system with a main feed duct (6), a divider (7) and a series of secondary ducts (8), at least some of which have a pneumatic modulator for the powder/gas flow. The modulator forms part of regulating loop which is linked to a coating quality or thickness monitor, and has an auxiliary gas feed duct to the secondary ducts and equipped with a gas flow or pressure regulator. Each secondary duct ends in an injector (9), the injectors being set at regular intervals along a line in the cavity inlet. The cavity also has a pressurised gas injector.

Description

La présente invention concerne un dispositif de distribution de solides pulvérulents à la surface d'un substrat, notamment en verre, afin de le revêtir de couches minces susceptibles de lui conférer des propriétés optiques, thermiques ou électriques.The present invention relates to a device for distributing powdery solids on the surface of a substrate, in particular glass, in order to coat it with thin layers capable of giving it optical, thermal or electrical properties.

Ce dispositif permet notamment de déposer ces couches minces par une technique dite de pyrolyse de poudre consistant à projeter lesdits solides pulvérulents (en général des composés organo-métalliques), en suspension dans un gaz, en direction d'un substrat chauffé à haute température, de manière à ce qu'ils se décomposent (en général sous forme d'oxyde métallique) à son contact. Le substrat peut prendre la forme d'un ruban de verre continu dit float, au sortir de l'enceinte de flottage du verre, le dispositif comprenant alors usuellement une buse comportant une cavité qui la traverse de part en part et qui se termine en une fente de distribution au-dessus du ruban et transversalement à son axe de défilement, la buse étant équipée de moyens d'alimentation en poudre appropriés.This device makes it possible in particular to deposit these thin layers by a technique known as powder pyrolysis consisting in spraying said pulverulent solids (in general organo-metallic compounds), in suspension in a gas, in the direction of a substrate heated to high temperature, so that they decompose (usually in the form of metal oxide) on contact. The substrate can take the form of a continuous ribbon of glass called float, at the exit from the glass float enclosure, the device then usually comprising a nozzle comprising a cavity which passes right through it and which ends in a distribution slot above the ribbon and transversely to its axis of travel, the nozzle being equipped with suitable powder supply means.

On peut ainsi obtenir, en continu, des couches minces présentant en règle générale une adhérence élevée au substrat et une qualité ainsi qu'une durabilité satisfaisantes.It is thus possible to obtain, continuously, thin layers generally exhibiting high adhesion to the substrate and satisfactory quality and durability.

Cependant, le ruban de verre float à recouvrir (ou tout autre substrat de grandes dimensions que l'on chercherait à recouvrir) présente usuellement une largeur d'au moins 2 mètres, notamment de l'ordre de trois à quatre mètres. C'est donc sur cette largeur, qui est considérable, que les buses ont à répartir la suspension gaz/poudre de la manière la plus homogène possible pour assurer, au moins transversalement à l'axe de défilement du ruban, une certaine constance dans la qualité et/ou l'épaisseur du revêtement déposé. Beaucoup d'études ont déjà été effectuées, visant soit la conception même de la buse, soit son mode d'alimentation en poudre, pour garantir au mieux cette homogénéité.However, the float glass ribbon to be covered (or any other large substrate that one would seek to cover) usually has a width of at least 2 meters, in particular of the order of three to four meters. It is therefore over this width, which is considerable, that the nozzles have to distribute the gas / powder suspension in the most homogeneous manner possible to ensure, at least transversely to the axis of travel of the ribbon, a certain consistency in the quality and / or thickness of the coating deposited. Many studies have already been carried out, aiming either at the very design of the nozzle, or at its mode of supplying powder, to best guarantee this homogeneity.

Ainsi, le brevet EP-B-0 130 919 a mis au point un moyen de répartition efficace permettant de subdiviser de manière assez uniforme une veine de poudre en suspension véhiculée dans un conduit d'amenée unique en une pluralité de veines de poudre véhiculées dans autant de conduits secondaires venant alimenter la buse sur toute sa largeur par l'intermédiaire d'organes d'alimentation appelés injecteurs dans lesquels ils débouchent. Il est cependant difficile de garantir que chacune des veines présente une parfaite identité avec toutes les autres, en terme de débit de poudre transportée, et que l'ensemble des veines va pouvoir se « fondre » en un courant de poudre parfaitement homogène au niveau de la fente de distribution de la buse.Thus, patent EP-B-0 130 919 has developed an efficient distribution means making it possible to fairly uniformly subdivide a vein of powder in suspension conveyed in a single supply duct into a plurality of powder veins conveyed in as many secondary conduits coming to feed the nozzle over its entire width by means of supply members called injectors into which they open. It is however difficult to guarantee that each of the veins has a perfect identity with all the others, in terms of flow rate of powder transported, and that all of the veins will be able to “melt” into a perfectly homogeneous stream of powder at the level of the nozzle distribution slot.

C'est pourquoi les brevets EP-B-0 125 153 et EP-B-0 374 023 ont proposé de compléter ce mode d'alimentation en prévoyant chacun des moyens d'amenée de gaz sous pression dans la cavité visant à faciliter, homogénéiser l'écoulement de la suspension poudre-gaz issue des injecteurs au travers de la buse, sans parvenir encore à supprimer tout risque d'irrégularité d'épaisseur dans la couche déposée et à « corriger » véritablement les éventuelles légères disparités entre les différentes veines de gaz arrivant dans les injecteurs.This is why patents EP-B-0 125 153 and EP-B-0 374 023 have proposed to supplement this mode of supply by each providing means for bringing pressurized gas into the cavity intended to facilitate, homogenize the flow of the powder-gas suspension from the injectors through the nozzle, without yet succeeding in eliminating any risk of irregularity in thickness in the deposited layer and in genuinely "correcting" any slight disparities between the different veins of gas entering the injectors.

Le brevet EP-B-0 392 902 a alors proposé un dispositif permettant de modifier automatiquement les positions relatives des injecteurs disposés en ligne à l'entrée de la buse, en écartant ou rapprochant les injecteurs concernés dès qu'est détectée une variation d'épaisseur locale dans le revêtement déposé en « aval » de la buse. Cette solution donne des résultats intéressants, mais n'est pas encore totalement optimale, d'abord parce qu'elle peut paraître un peu compliquée à mettre en oeuvre, ensuite et surtout parce qu'elle tente de compenser les éventuelles disparités de débit des veines secondaires sans les corriger véritablement.Patent EP-B-0 392 902 then proposed a device making it possible to automatically modify the relative positions of the injectors arranged in line at the inlet of the nozzle, by removing or bringing together the injectors concerned as soon as a variation of local thickness in the coating deposited “downstream” from the nozzle. This solution gives interesting results, but is not yet fully optimal, firstly because it may seem a little complicated to implement, then and above all because it tries to compensate for any disparities in the flow of the veins. without really correcting them.

L'invention a alors pour but d'améliorer encore le mode de fonctionnement des dispositifs de distribution de poudre de ce type, et notamment de parvenir à optimiser l'homogénéité de l'écoulement de la suspension poudre-gaz dans la buse sans trop sacrifier à la simplicité de mise en oeuvre, afin d'obtenir des revêtements de qualité, particulièrement en terme de régularité d'épaisseur.The object of the invention is therefore to further improve the operating mode of powder distribution devices of this type, and in particular to achieve optimization of the homogeneity of the flow of the powder-gas suspension in the nozzle without sacrificing too much. simplicity of implementation, in order to obtain quality coatings, particularly in terms of thickness regularity.

L'invention a pour objet un dispositif de distribution de solide pulvérulent en suspension dans un gaz, en vue de déposer un revêtement, notamment par pyrolyse, sur un substrat en défilement, notamment du type ruban de verre float. Ce dispositif comprend d'une part une buse de distribution dont les parois définissent une cavité qui se termine par une fente de distribution longitudinale. Il comprend d'autre part un conduit principal d'amenée de poudre muni d'un moyen de répartition . Une pluralité de conduits secondaires d'amenée de poudre connectés à ce conduit principal à l'aide des moyens de répartition permet d'alimenter en poudre la cavité de la buse sur toute sa longueur. Selon l'invention, au moins une partie des conduits secondaires est équipée d'au moins un moyen pneumatique apte à moduler le débit de la suspension poudre-gaz que chacun des conduits secondaires concerné est destiné à véhiculer. De préférence, chacun des conduits est équipé d'un tel moyen pneumatique. Cette solution présente deux intérêts majeurs : d'une part, pouvoir moduler le débit dans chacun des conduits va permettre de corriger véritablement et directement les éventuelles disparités de débit entre les veines de mélange gaz-poudre qu'ils transportent jusque dans la buse, et ainsi d'assurer une répartition très régulière dans l'alimentation en poudre au niveau de la buse, sur toute la longueur de sa cavité. D'autre part, avoir recours à un moyen pneumatique et non mécanique pour opérer ces modulations de débit est très avantageux. En effet, un moyen mécanique du type vanne fonctionne sur le principe d'une obturation partielle du conduit, obturation qui, dans le cas d'un écoulement de poudre, provoque des accumulations locales intempestives de poudre, des colmatages ou engorgements pouvant provoquer de manière soudaine et incontrôlée de fortes pertes de charge dans l'écoulement.The subject of the invention is a device for distributing powdery solid suspended in a gas, with a view to depositing a coating, in particular by pyrolysis, on a moving substrate, in particular of the float glass ribbon type. This device includes on the one hand, a dispensing nozzle whose walls define a cavity which ends in a longitudinal dispensing slot. It also comprises a main powder supply pipe provided with a distribution means. A plurality of secondary powder supply conduits connected to this main conduit by means of distribution means makes it possible to supply powder to the cavity of the nozzle over its entire length. According to the invention, at least part of the secondary conduits is equipped with at least one pneumatic means capable of modulating the flow rate of the powder-gas suspension that each of the secondary conduits concerned is intended to convey. Preferably, each of the conduits is equipped with such a pneumatic means. This solution has two major advantages: on the one hand, being able to modulate the flow rate in each of the conduits will make it possible to genuinely and directly correct any disparities in flow rate between the gas-powder mixture streams that they transport to the nozzle, and thus ensuring a very regular distribution in the powder supply at the nozzle, over the entire length of its cavity. On the other hand, using pneumatic rather than mechanical means to operate these flow modulations is very advantageous. Indeed, a mechanical means of the valve type operates on the principle of a partial blockage of the conduit, a blockage which, in the case of a flow of powder, causes untimely local accumulations of powder, blockages or blockages which can cause sudden and uncontrolled high pressure losses in the flow.

Un moyen pneumatique, au contraire, permet de moduler un débit de mélange poudre-gaz de manière fine et contrôlée et peut être réglé avec des temps de réponse très brefs, avec des moyens de réglage appropriés, qui peuvent être manuels ou automatisés. Ces moyens, si on les choisit automatisés, peuvent faire avantageusement partie d'une boucle de régulation, sous commande d'une unité de contrôle connectée à au moins un moyen de mesure de qualité ou d'épaisseur sur le revêtement déposé sur le substrat, à l'aide de la buse de distribution. S'il s'agit d'un ruban de verre float, la régulation dans les débits de poudre des conduits secondaires peut être effectuée en continu, en ajustant très rapidement le débit du ou des conduits secondaires appropriés à l'aide de leurs moyens pneumatiques dès qu'est détectée une variation d'épaisseur transversale dans le revêtement déposé sur le ruban juste en aval de la buse. En se servant par exemple d'abaques préétablies indiquant la correspondance entre une variation d'épaisseur locale donnée et une variation de réglage du moyen pneumatique adéquat du conduit secondaire concerné pour la rectifier, on n'a alors même pas besoin de mesurer précisément les débits de mélange poudre-gaz des conduits et leurs éventuels écarts, on peut effectuer seulement une corrélation entre les variations d'épaisseur qui sont la conséquence de ces écarts et les réglages des moyens pneumatiques à effectuer.A pneumatic means, on the contrary, makes it possible to modulate a flow rate of powder-gas mixture in a fine and controlled manner and can be adjusted with very short response times, with appropriate adjustment means, which can be manual or automated. These means, if they are chosen to be automated, can advantageously form part of a regulation loop, under the control of a control unit connected to at least one quality or thickness measurement means on the coating deposited on the substrate, using the dispensing nozzle. In the case of a float glass ribbon, the regulation in the powder flow rates of the secondary conduits can be carried out continuously, by very quickly adjusting the flow rate of the appropriate secondary conduit (s) using their pneumatic means. as soon as a variation in transverse thickness is detected in the coating deposited on the strip just downstream of the nozzle. By using for example pre-established charts indicating the correspondence between a variation of given local thickness and a variation of adjustment of the adequate pneumatic means of the secondary duct concerned for rectify it, we do not even need to precisely measure the powder-gas mixture flow rates of the conduits and their possible deviations, we can only make a correlation between the variations in thickness which are the consequence of these deviations and the settings pneumatic means to be performed.

Ces moyens pneumatiques peuvent se présenter simplement sous la forme de conduits d'amenée auxiliaires débouchant dans les conduits secondaires, amenées auxiliaires que l'on munit avantageusement d'un moyen de régulation manuel ou automatisé de débit ou pression de gaz, utilisant par exemple des vannes. Dans la mesure où elles ne véhiculent que du gaz, ce type de moyen de réglage mécanique n'entraîne aucun problème. Ces amenées introduisent ainsi dans l'écoulement du mélange poudre-gaz des conduits secondaires un jet de gaz dont les caractéristiques sont maîtrisées afin d'y créer une perte de charge contrôlée permettant alors d'en diminuer plus ou moins le débit quand cela est nécessaire. Grâce à un moyen de répartition approprié, la quantité de poudre qui n'est plus véhiculée par le conduit du fait de cette diminution provoquée de débit va pouvoir se répartir homogènement sur tous les autres conduits secondaires.These pneumatic means may simply be in the form of auxiliary supply conduits opening into the secondary conduits, auxiliary supply which is advantageously provided with a manual or automated means for regulating gas flow or pressure, using for example valves. Insofar as they only carry gas, this type of mechanical adjustment means does not cause any problems. These feeds thus introduce a flow of gas into the flow of the powder-gas mixture from the secondary conduits, the characteristics of which are controlled in order to create a controlled pressure drop thereby allowing the flow to be more or less reduced when necessary. . Thanks to an appropriate distribution means, the quantity of powder which is no longer conveyed by the conduit due to this induced reduction in flow rate will be able to be distributed homogeneously over all the other secondary conduits.

Ces conduits secondaires peuvent avantageusement comporter des canalisations, de préférence souples, connectées au moyen de répartition du conduit d'amenée principal, canalisations dont les extrémités débouchant à l'entrée de la cavité de la buse sont constituées par des organes d'alimentation appelés « injecteurs » rigides, et de préférence métalliques. Les moyens d'amenée de gaz auxiliaires peuvent alors déboucher dans les conduits secondaires en tout point, soit au niveau de ces canalisations (souples), en « aval » du moyen de répartition du conduit principal, soit à proximité ou dans la buse, notamment au niveau de la jonction canalisation-injecteur ou au niveau de l'injecteur lui-même. C'est cette dernière configuration qui est plus favorable, car l'injecteur, rigide, permet un « branchement » facile et sûr de l'amenée de gaz auxiliaire.These secondary conduits may advantageously comprise pipes, preferably flexible, connected to the distribution means of the main supply pipe, pipes whose ends opening out at the entrance to the cavity of the nozzle are constituted by supply members called " rigid injectors, preferably metallic. The auxiliary gas supply means can then open into the secondary conduits at any point, either at the level of these (flexible) pipes, “downstream” from the distribution means of the main conduit, either near or in the nozzle, in particular at the pipe-injector junction or at the injector itself. It is this latter configuration which is more favorable, since the rigid injector allows an easy and safe "connection" of the auxiliary gas supply.

Un mode de réalisation préféré de l'invention consiste ainsi en un dispositif de distribution, où chacun des conduits secondaires destinés à véhiculer les suspensions poudre-gaz est muni à son extrémité d'un injecteur, les injecteurs étant régulièrement disposés en ligne dans l'orifice d'entrée de la cavité de la buse sur toute sa longueur et étant tous munis d'une arrivée de gaz auxiliaire à débit variable. En outre, la cavité de la buse est également munie de moyens d'injection de gaz sous pression pour entraîner la suspension poudre-gaz émise par les injecteurs dans la cavité, moyens d'injection de préférence disposés symétriquement de part et d'autre de la ligne d'injecteurs. Ainsi, l'alimentation en poudre de la buse se trouve doublement optimisée. On la corrige d'abord « à la source », grâce aux moyens pneumatiques de l'invention permettant de supprimer ou à tout le moins d'atténuer très significativement toutes les disparités de débit entre les jets de mélange poudre-gaz émis dans la buse par les injecteurs. On l'homogénéise ensuite, dans la buse, grâce à des gaz sous pression qui vont permettre de « transformer » la pluralité de jets de mélange individualisés s'écoulant dans la buse en un « rideau » de poudre uniforme en sortie de la fente transversale.A preferred embodiment of the invention thus consists of a distribution device, where each of the secondary conduits intended to convey the powder-gas suspensions is provided at its end with an injector, the injectors being regularly arranged in line in the inlet port of the nozzle cavity over its entire length and all being provided with an auxiliary gas supply with variable flow. In addition, the nozzle cavity is also provided with means for injecting pressurized gas to drive the powder-gas suspension emitted by the injectors into the cavity, means for injecting preferably arranged symmetrically on either side of the injector line. Thus, the powder supply of the nozzle is doubly optimized. It is first corrected "at the source", by means of the pneumatic means of the invention making it possible to eliminate or at least attenuate very significantly all the disparities in flow between the jets of powder-gas mixture emitted in the nozzle by the injectors. It is then homogenized in the nozzle, using pressurized gases which will make it possible to "transform" the plurality of individualized mixing jets flowing in the nozzle into a "curtain" of uniform powder at the outlet of the transverse slot. .

L'invention a également pour objet le procédé de mise en oeuvre du dispositif précédemment décrit, et notamment les diverses manières de contrôler et réguler les moyens pneumatiques équipant les conduits secondaires. Quand ces moyens pneumatiques se présentent sous la forme d'arrivées de gaz auxiliaires débouchant dans les conduits, on peut ainsi régler chacun des débits de jets de gaz auxiliaire séparément pour chacun d'entre eux, et ceci dans une gamme de débit pouvant aller par exemple entre 0 et 100% d'une valeur de débit prédéterminée. Il faut en effet que ces jets de gaz aient une action de « freinage » de l'écoulement de poudre dans le conduit, afin d'y créer une perte de charge et non une dépression qui provoquerait une accélération de l'écoulement. Les débits, vitesses et directions d'injection de ces jets de gaz auxiliaire par rapport à ceux de l'écoulement de mélange poudre-gaz doivent donc être soigneusement sélectionnés.The invention also relates to the method of implementing the device described above, and in particular the various ways of controlling and regulating the pneumatic means equipping the secondary conduits. When these pneumatic means are in the form of auxiliary gas inlets opening into the conduits, it is thus possible to adjust each of the auxiliary gas jet flow rates separately for each of them, and this in a range of flow rates which can range from example between 0 and 100% of a predetermined flow value. It is indeed necessary that these gas jets have a “braking” action on the flow of powder in the conduit, in order to create a pressure drop there and not a depression which would cause an acceleration of the flow. The injection rates, speeds and directions of these auxiliary gas jets relative to those of the powder-gas mixture flow must therefore be carefully selected.

Une première possibilité est de fonctionner en « tout ou rien ». Si aucune disparité locale des débits des conduits, se traduisant par une variation locale d'épaisseur du revêtement, est détectée, le débit de ces jets de gaz auxiliaire est nul. Si une disparité apparaît, provoquant localement des surépaisseurs dans le revêtement, le moyen pneumatique du ou des conduits secondaires impliqués intervient pour délivrer un jet de gaz auxiliaire de débit adapté ne pouvant dépasser une certaine valeur, afin de diminuer suffisamment le débit de poudre du ou des conduits pour supprimer cette surépaisseur.A first possibility is to operate "all or nothing". If no local disparity in the flow rates of the conduits, resulting in a local variation in coating thickness, is detected, the flow rate of these jets of auxiliary gas is zero. If a disparity appears, locally causing excess thickness in the coating, the pneumatic means of the secondary conduit or conduits involved intervenes to deliver an auxiliary gas jet of suitable flow rate which cannot exceed a certain value, in order to sufficiently reduce the powder flow rate of the or conduits to remove this excess thickness.

Une seconde possibilité est de faire fonctionner en permanence l'ensemble des moyens pneumatiques, qui émettent tous, quand aucune disparité n'est détectée, un jet de gaz auxiliaire de débit donné. Ils exercent donc tous un certain effet de « freinage » permanent sur les écoulements de mélange poudre-gaz dans les conduits, que l'on peut compenser si besoin en adaptant en conséquence le débit de mélange poudre-gaz dans le conduit d'amenée principal. On peut ainsi effectuer la régulation du débit des jets de gaz auxiliaire autour de cette valeur de débit donnée. Ce mode de fonctionnement est plus souple et laisse plus de marge de manoeuvre, puisque l'on peut aussi bien rectifier des surépaisseurs locales de revêtement (en augmentant le débit d'émission du jet de gaz auxiliaire approprié) que des diminutions locales d'épaisseur dudit revêtement (en diminuant cette fois le débit d'émission du jet de gaz auxiliaire approprié).A second possibility is to permanently operate all of the pneumatic means, which all emit, when no disparity is detected, an auxiliary gas jet of given flow rate. They therefore all exert a certain permanent “braking” effect on the flows of powder-gas mixture in the conduits, which can be compensated for if necessary by adapting accordingly the flow rate of powder-gas mixture in the main supply conduit. . It is thus possible to regulate the flow rate of the gas jets auxiliary around this given flow value. This operating mode is more flexible and leaves more room for maneuver, since it is possible to correct both local coating thicknesses (by increasing the emission rate of the appropriate auxiliary gas jet) as well as local thickness decreases said coating (this time reducing the emission rate of the appropriate auxiliary gas jet).

Dans ce mode de fonctionnement, il est avantageux que la valeur de débit autour de laquelle on régule le débit de chacun des jets de gaz auxiliaire soit d'environ 20 à 60% du débit de gaz moyen de la suspension poudre-gaz véhiculée par chacun des conduits secondaires. De préférence, on choisit une valeur d'environ 50%, avec une régulation du débit de chacun des jets de gaz auxiliaire de ± 50% autour de cette valeur. On entend par débit « moyen », leur débit théorique, si aucune disparité de débit entre conduits ne pouvait exister.In this operating mode, it is advantageous that the flow value around which the flow of each of the auxiliary gas jets is regulated is approximately 20 to 60% of the average gas flow of the powder-gas suspension conveyed by each. secondary ducts. Preferably, a value of around 50% is chosen, with a regulation of the flow rate of each of the auxiliary gas jets of ± 50% around this value. The term “average” flow is understood to mean their theoretical flow, if no disparity in flow between conduits could exist.

Comme précédemment mentionné, le plus simple et le plus efficace est de réguler ces débits de jet de gaz auxiliaire non en fonction des écarts évalués quantitativement entre les débits des conduits secondaires, ce qui serait délicat à faire, mais directement en fonction des variations d'épaisseur détectées dans le revêtement « en aval » de la buse de distribution. On corrige ainsi les écarts de débit indirectement.As previously mentioned, the simplest and most effective is to regulate these auxiliary gas jet flow rates not according to the differences evaluated quantitatively between the flow rates of the secondary conduits, which would be difficult to do, but directly according to the variations in thickness detected in the coating “downstream” from the dispensing nozzle. This corrects the flow differences indirectly.

Le dispositif et procédé de mise en oeuvre de ce dernier peuvent être avantageusement utilisés en vu de déposer des revêtements à base d'oxyde métallique, par pyrolyse sur un ruban de verre float chaud, notamment des revêtements d'oxydes dopés du type SnO₂:F, par exemple à partir d'une poudre de difluorure de dibutylétain (D.B.T.F.) ou du type ITO à partir de poudre de formiate d'indium et de dibutyloxyde d'étain.The device and method for implementing the latter can be advantageously used in view of depositing coatings based on metal oxide, by pyrolysis on a strip of hot float glass, in particular coatings of doped oxides of SnO₂ type: F , for example from a powder of dibutyltin difluoride (DBTF) or of the ITO type from powder of indium formate and tin dibutyloxide.

Les détails et caractéristiques avantageuses du dispositif de distribution selon l'invention vont maintenant ressortir d'un mode de réalisation non limitatif illustré à l'aide des figures suivantes :

  • figure 1 : une vue schématique d'ensemble d'une installation de dépôt d'un revêtement par pyrolyse de poudre sur un substrat,
  • figure 2 : une vue en coupe transversale de la buse de distribution de l'installation selon la figure 1.
The details and advantageous characteristics of the dispensing device according to the invention will now emerge from a nonlimiting embodiment illustrated with the aid of the following figures:
  • FIG. 1: an overall schematic view of an installation for depositing a coating by powder pyrolysis on a substrate,
  • FIG. 2: a cross-sectional view of the dispensing nozzle of the installation according to FIG. 1.

L'installation telle que montrée dans son ensemble en figure 1 permet de distribuer de manière régulière des solides pulvérulents de toutes natures sur des substrats divers, notamment de grandes dimensions. Dans le cadre de cet exemple non limitatif, on l'utilise pour distribuer une poudre de composés organo-métalliques sur un ruban 1 de verre float chaud au sortir de l'enceinte du bain flottage, ruban défilant sur un lit de rouleaux 2 selon un axe donné à une vitesse uniforme. La poudre mis ainsi au contact de la surface du verre chaud s'y décompose pour laisser un revêtement à base d'oxyde(s) métallique(s).The installation as shown as a whole in FIG. 1 makes it possible to regularly distribute pulverulent solids of all kinds on various substrates, especially large dimensions. In the context of this nonlimiting example, it is used to distribute a powder of organo-metallic compounds on a ribbon 1 of hot float glass leaving the enclosure of the floating bath, ribbon passing over a bed of rollers 2 according to a axis given at a uniform speed. The powder thus brought into contact with the surface of the hot glass decomposes therein to leave a coating based on metal oxide (s).

Cette installation est une optimisation de celle décrite dans le brevet européen EP-B-0 130 919 précité dans la mesure où elle comporte en plus les moyens pneumatiques 22 spécifiques de la présente invention.This installation is an optimization of that described in the aforementioned European patent EP-B-0 130 919 insofar as it additionally comprises the specific pneumatic means 22 of the present invention.

La buse 24 de l'installation représentée en figure 2 est de la même manière une optimisation de celle décrite dans le brevet EP-0 374 023. On s'attache ci-après à décrire plus particulièrement les caractéristiques ayant spécifiquement trait à l'invention. Pour plus de renseignements concernant le fonctionnement de l'installation en général et de la buse en particulier, on se rapportera donc avantageusement à ces deux brevets, ainsi qu'aux autres brevets précédemment cités.The nozzle 24 of the installation shown in FIG. 2 is in the same way an optimization of that described in patent EP-0 374 023. We will endeavor below to describe more particularly the characteristics relating specifically to the invention . For more information concerning the operation of the installation in general and of the nozzle in particular, reference will therefore advantageously be made to these two patents, as well as to the other patents cited above.

L'installation selon la figure 1 représente donc une trémie 3 de stockage de poudre 4 à distribuer, un mélangeur 5 dans lequel est réalisé le mélange poudre-gaz, en général de l'air en vue de constituer une suspension aussi homogène que possible de la poudre dans le gaz à l'aide d'une arrivée d'air 25 et d'une vis sans fin 26 alimentée en poudre par la trémie 3. Un conduit principal d'admission 6 achemine la suspension poudre-gaz à la sortie du mélangeur 5, un moyen de répartition 7 subdivisant la veine unique de suspension poudre-gaz amenée par le conduit 6 en une pluralité de veines secondaires aussi uniformes que possible, une pluralité de conduits secondaires 8 souples véhiculant celles-ci jusqu'à la buse de distribution 24. Cette buse est disposée transversalement à l'axe de défilement du ruban de verre 2 et définit une cavité transversale dont la longueur correspond à la largeur du ruban à revêtir. Les conduits secondaires 8 débouchent dans des injecteurs métalliques 9 disposés en ligne à l'entrée de cette cavité.The installation according to FIG. 1 therefore represents a hopper 3 for storing powder 4 to be distributed, a mixer 5 in which the powder-gas mixture is produced, generally air in order to constitute a suspension as homogeneous as possible of the powder in the gas by means of an air inlet 25 and an endless screw 26 supplied with powder by the hopper 3. A main inlet duct 6 conveys the powder-gas suspension at the outlet of the mixer 5, a distribution means 7 subdividing the single powder-gas suspension stream brought by the pipe 6 into a plurality of secondary streams as uniform as possible, a plurality of flexible secondary pipes 8 conveying these to the nozzle distribution 24. This nozzle is arranged transversely to the axis of travel of the glass ribbon 2 and defines a transverse cavity whose length corresponds to the width of the ribbon to be coated. The secondary conduits 8 open into metal injectors 9 arranged in line at the entrance to this cavity.

Si on se reporte à la figure 2, on voit effectivement l'un de ces injecteurs 9 venant projeter une veine de mélange gaz-poudre à l'entrée 10 de la cavité 11 définie par les parois 12 intérieures de la buse, parois planes et légèrement convergentes jusqu'à la fente de distribution 13 située à quelques millimètres de la surface du ruban de verre 1. Des moyens d'injection de gaz sous pression sont par ailleurs prévus de part et d'autre de la ligne des injecteurs 9, afin de faciliter la répartition en « rideau » de poudre et l'entraînement des jets de suspension poudre-gaz issus des injecteurs 9. Ces moyens sont formés par une série de chambres 14 situées symétriquement dans le corps de buse et reliées par une rampe 15 à une source de gaz, de l'air en général. Ces chambres sont reliées entre elles par une cloison 16 formant entretoise, munie d'un moyen de passage du gaz par exemple à l'aide de matériaux poreux et par des orifices 17. Les chambres 18 situées en partie supérieure de la buse débouchent dans la cavité 11 par des fentes 19 à proximité des injecteurs 9, de manière à injecter le gaz sous pression sensiblement parallèlement aux parois 12, fentes limitées par des lèvres 20, de configuration appropriée.If we refer to FIG. 2, we actually see one of these injectors 9 projecting a stream of gas-powder mixture at the inlet 10 of the cavity 11 defined by the inner walls 12 of the nozzle, flat walls and slightly convergent to the distribution slot 13 located a few millimeters from the surface of the glass ribbon 1. Means for injecting gas under pressure are also provided on either side of the line of injectors 9, in order to facilitate the “curtain” distribution of powder and the driving of the powder-gas suspension jets coming from the injectors 9. These means are formed by a series of chambers 14 located symmetrically in the nozzle body and connected by a ramp 15 to a source of gas, air in general. These chambers are interconnected by a partition 16 forming a spacer, provided with a means for passing gas, for example using porous materials, and by orifices 17. The chambers 18 located in the upper part of the nozzle open into the cavity 11 by slots 19 near the injectors 9, so as to inject the gas under pressure substantially parallel to the walls 12, slots limited by lips 20, of suitable configuration.

Selon l'invention, chacun des injecteurs 9 est constitué schématiquement d'un cylindre métallique creux dans lequel débouche chacun des conduits secondaires 8 de manière étanche. Ces injecteurs comprennent en outre une arrivée de gaz du type air sous forme d'un conduit auxiliaire 22 venant y déboucher, avec de préférence une configuration telle entre injecteur 9 et conduit 22 que le jet de mélange poudre-gaz dans l'injecteur et le jet de gaz que peut émettre le conduit 22 dans l'injecteur 9 fassent entre eux un angle a compris entre 5 et 90°, de préférence d'environ 30°. Il est en effet préférable que cet angle reste inférieur à 90° afin d'éviter tout risque de voir des traces de poudre s'infiltrer dans le conduit 22, traces pouvant notamment perturber le bon fonctionnement des moyens de réglage de débit qui l'équipent. Chaque conduit auxiliaire 22 est alimenté par une source de gaz appropriée non représentée.According to the invention, each of the injectors 9 consists schematically of a hollow metal cylinder into which each of the secondary conduits 8 opens in a sealed manner. These injectors further include an air type gas inlet in the form of an auxiliary conduit 22 coming into it, preferably with a configuration such between injector 9 and conduit 22 that the jet of powder-gas mixture in the injector and the gas jet that can emit the conduit 22 in the injector 9 make between them an angle a between 5 and 90 °, preferably about 30 °. It is in fact preferable that this angle remains less than 90 ° in order to avoid any risk of traces of powder seeping into the duct 22, traces which can in particular disturb the proper functioning of the flow control means which equip it . Each auxiliary duct 22 is supplied by a suitable gas source, not shown.

On peut moduler le débit de jet de gaz véhiculé par chacun des conduits 22 dans l'écoulement poudre-gaz de chacun des injecteurs, de manière individualisée, à l'aide de boucle de régulation. Chacun des conduit relié à une source de gaz, notamment de l'air, extérieure à la buse, est munie d'un moyen de réglage de débit du type électrovanne. Ce moyen de réglage, (par exemple du type débit-mètre associé à une vanne magnétique) est commandé par une unité de contrôle en fonction des variations d'épaisseur détectées en aval de la buse sur le revêtement 23. Cette détection peut être réalisée en continu ou par intervalle de temps donné à l'aide d'un ou plusieurs moyens de mesure d'épaisseur du type réflectomètres (soit un réflectomètre monté mobile au-dessus du ruban de verre afin de « balayer » la largeur du revêtement, soit plusieurs réflectomètres disposés en ligne au-dessus du ruban.One can modulate the gas jet flow conveyed by each of the conduits 22 in the powder-gas flow of each of the injectors, individually, using a regulation loop. Each of the conduits connected to a source of gas, in particular air, external to the nozzle, is provided with a flow control means of the solenoid valve type. This adjustment means (for example of the flow meter type associated with a magnetic valve) is controlled by a control unit as a function of the thickness variations detected downstream of the nozzle on the coating 23. This detection can be carried out by continuous or by time interval given using one or more means of thickness measurement of the reflectometers type (either a reflectometer mounted movable above the glass ribbon in order to “sweep” the width of the coating, or several reflectometers arranged in line above the ribbon.

Le mode de fonctionnement de la buse 24 est explicité à l'aide d'un exemple de mise en oeuvre, consistant à déposer une couche de SnO₂:F de 200 nm d'épaisseur à partir d'une poudre de dibutyldifluorure d'étain (D.B.T.F.). Le débit massique de poudre de D.B.T.F. véhiculée dans le conduit principal d'amenée 6 est compris entre 3 et 10 kg/heure/mètre linéaire de buse. Le débit volumique du gaz dans lequel elle est en suspension est compris entre 3 et 80 m³/heure/mètre linéaire de buse. Le débit de gaz sous pression injecté par les fentes 19 dans la cavité est compris entre 200 et 500 m³/h/mètre linéaire de buse.The mode of operation of the nozzle 24 is explained with the aid of an implementation example, consisting of depositing a layer of SnO₂: F 200 nm thick from a tin dibutyldifluoride powder ( DBTF). The mass flow of powder of D.B.T.F. conveyed in the main supply conduit 6 is between 3 and 10 kg / hour / linear meter of nozzle. The volume flow rate of the gas in which it is suspended is between 3 and 80 m³ / hour / linear meter of nozzle. The flow of pressurized gas injected through the slots 19 into the cavity is between 200 and 500 m³ / h / linear meter of nozzle.

Si le moyen de répartition 7 et la conception des conduits 6 et 8 étaient parfaits, chaque conduit secondaire véhiculerait une veine gazeuse dont les débits massiques en D.B.T.F. et volumique en gaz seraient exactement égaux au rapport de ceux de la suspension véhiculée dans le conduit principal d'amenée sur le nombre de conduits secondaires. Or il s'avère que des écarts de débit peuvent apparaître entre les jets de mélange poudre-gaz issus de chacun des injecteurs 9, écarts conduisant à des surépaisseurs ou au contraire des diminutions locales de l'épaisseur de revêtement déposé par rapport à l'épaisseur moyenne de 200 nm recherchée. Ces variations transversales dans l'épaisseur du revêtement sont préjudiciables à sa qualité, car elles peuvent, notamment, engendrer des défauts optiques, du type irisations, peu esthétiques.If the distribution means 7 and the design of the conduits 6 and 8 were perfect, each secondary conduit would convey a gas stream whose mass flow rates in D.B.T.F. and gas volume would be exactly equal to the ratio of those of the suspension conveyed in the main supply duct to the number of secondary ducts. However, it turns out that differences in flow can appear between the jets of powder-gas mixture coming from each of the injectors 9, differences leading to excess thicknesses or, on the contrary, local decreases in the thickness of coating deposited relative to the average thickness of 200 nm sought. These transverse variations in the thickness of the coating are detrimental to its quality, because they can, in particular, cause optical defects, of the iridescence type, which are not very aesthetic.

En fonctionnement normal, en l'absence de détection par le ou les réflectomètres d'une variation locale d'épaisseur de revêtement dépassant un seuil de tolérance donné, par exemple pas plus de 3% d'écart par rapport à l'épaisseur moyenne voulue de 200 nm, passe en permanence par chacun des injecteurs 9 un écoulement poudre-gaz provenant du conduit secondaire 8, présentant un débit volumique de gaz d'environ 2 m³/h et un jet de gaz émis par le conduit auxiliaire 22 d'un débit volumique en gaz donné, notamment d'environ 1 m³/h.In normal operation, in the absence of detection by the reflectometer (s) of a local variation in coating thickness exceeding a given tolerance threshold, for example not more than 3% deviation from the desired average thickness of 200 nm, a powder-gas flow coming from the secondary pipe 8 is constantly passing through each of the injectors 9, presenting a gas flow rate of approximately 2 m³ / h and a gas jet emitted by the auxiliary pipe 22 of a volume flow rate in given gas, in particular around 1 m³ / h.

Dès qu'un réflectomètre détecte une diminution locale d'épaisseur franchissant le seuil de 3% prédéfini, l'unité de contrôle commande la vanne du (des) conduit(s) 22 des injecteurs 9 concernés pour diminuer le débit du jet de gaz auxiliaire. Dans le cas où il s'agit d'une surépaisseur, il faudra alors au contraire augmenter ce débit. Ainsi, en partant d'une valeur moyenne de 1 m³/h, le débit de chacun des jets de gaz auxiliaire peut varier entre par exemple 0,5 et 1,5 m³/h. Plus le débit de jet de gaz auxiliaire augmente et plus il va diminuer celui de l'écoulement poudre-gaz, et donc diminuer localement l'épaisseur du revêtement déposé. L'unité de contrôle (ou l'opérateur) peut se servir d'abaques donnant les correspondances directes entre variation d'épaisseur dans le revêtement et variation de débit dans les conduits 22, sans même avoir à mesurer précisément les débits de poudre qui passent dans les conduits 8 puis les injecteurs 9.As soon as a reflectometer detects a local thickness reduction crossing the predefined threshold of 3%, the control unit controls the valve of the line (s) 22 of the injectors 9 concerned to reduce the flow rate of the auxiliary gas jet . In the case where it is an additional thickness, it will then on the contrary be necessary to increase this flow rate. Thus, starting from an average value of 1 m³ / h, the flow rate of each of the auxiliary gas jets can vary between for example 0.5 and 1.5 m³ / h. The more the auxiliary gas jet flow increases, the more it will decrease that of the powder-gas flow, and therefore locally decrease the thickness of the coating deposited. The control unit (or the operator) can use charts giving direct correspondence between thickness variation in the coating and flow variation in the conduits 22, without even having to measure precisely the flow rates of powder which pass in the conduits 8 then the injectors 9.

A noter qu'il est important que ces jets de gaz auxiliaire, au vu des débits envisagés et des diamètres des conduits 22, conservent une vitesse suffisamment peu élevée par rapport à celle de l'écoulement poudre-gaz dans les injecteurs 9 pour éviter de créer une aspiration qui viendrait brutalement l'entraîner au lieu d'en moduler le débit.Note that it is important that these jets of auxiliary gas, in view of the envisaged flow rates and the diameters of the conduits 22, maintain a sufficiently low speed compared to that of the powder-gas flow in the injectors 9 to avoid create an aspiration which would brutally drive it instead of modulating the flow.

Toute irrégularité dans l'épaisseur du revêtement peut ainsi être rapidement corrigée, à distance, de manière manuelle, automatisée ou semi-automatisée. La régulation de débit de l'écoulement de la suspension poudre-gaz provenant de chacun des conduits secondaires 8 s'effectue par le jet de gaz auxiliaire de chacun des conduits 22, sans aucun problème d'engorgement ou colmatage du conduit secondaire ni d'incidence préjudiciable sur l'alimentation des autres conduits secondaires. Ainsi, si, grâce au réglage du jet de gaz auxiliaire on diminue le débit de poudre dans le conduit secondaire 8 adhoc pour rectifier une surépaisseur dans le revêtement, « l'excès de poudre » non délivré par le conduit dont on a diminué le débit va se répartir régulièrement sur tous les autres conduits au niveau du moyen de répartition.Any irregularity in the thickness of the coating can thus be quickly corrected, remotely, manually, automated or semi-automated. The flow control of the powder-gas suspension coming from each of the secondary conduits 8 is regulated by the auxiliary gas jet of each of the conduits 22, without any problem of clogging or clogging of the secondary conduit or of detrimental impact on the supply of other secondary conduits. Thus, if, thanks to the adjustment of the auxiliary gas jet, the powder flow is reduced in the secondary duct 8 adhoc to correct an excess thickness in the coating, the “excess powder” not delivered by the duct, the flow of which has been reduced will be distributed regularly on all the other conduits at the level of the distribution means.

Par ailleurs, il ressort de la description précédente que le mode d'alimentation en poudre utilise les moyens pneumatiques de l'invention en vue d'améliorer l'uniformité dans l'épaisseur du revêtement déposé. Mais on pourrait tout aussi bien, sans sortir du cadre de l'invention, utiliser ces moyens pneumatiques pour créer, cette fois de manière volontaire et contrôlée, des gradients dans l'épaisseur du revêtement déposé, à tout le moins transversalement à l'axe de défilement du substrat, si cela s'avérait utile ou avantageux de fabriquer des revêtements présentant de telles caractéristiques.Furthermore, it emerges from the preceding description that the powder supply mode uses the pneumatic means of the invention in order to improve the uniformity in the thickness of the coating deposited. But we could just as easily, without departing from the scope of the invention, use these pneumatic means to create, this time in a voluntary and controlled manner, gradients in the thickness of the coating deposited, at least transversely to the axis substrate travel, if it proved useful or advantageous to manufacture coatings having such characteristics.

Claims (13)

Dispositif de distribution de solide pulvérulent en suspension dans un gaz, en vue de déposer un revêtement (23), notamment par pyrolyse, sur un substrat en défilement, notamment du type ruban de verre float (1), ce dispositif comprenant une buse de distribution (24) dont les parois (12) définissent une cavité (11) qui se termine par une fente de distribution (13) longitudinale, et un système d'alimentation en poudre de ladite buse comportant un conduit principal d'amenée de poudre (6) muni d'un moyen de répartition (7) et une pluralité de conduits secondaires (8) d'amenée de poudre connectés audit conduit principal à l'aide dudit moyen de répartition et permettant d'alimenter en poudre la cavité (11) sur toute sa longueur, caractérisé en ce qu'au moins une partie des conduits secondaires (8) est équipée d'au moins un moyen pneumatique apte à moduler le débit de la suspension poudre-gaz que chacun des conduits secondaires concernés est destiné à véhiculer.Device for distributing a powdery solid suspended in a gas, with a view to depositing a coating (23), in particular by pyrolysis, on a moving substrate, in particular of the float glass ribbon type (1), this device comprising a dispensing nozzle (24) whose walls (12) define a cavity (11) which ends in a longitudinal distribution slot (13), and a powder supply system of said nozzle comprising a main powder supply duct (6 ) provided with a distribution means (7) and a plurality of secondary conduits (8) for supplying powder connected to said main conduit with the aid of said distribution means and making it possible to supply the cavity (11) with powder its entire length, characterized in that at least a portion of the secondary conduits (8) is equipped with at least one pneumatic means capable of modulating the flow rate of the powder-gas suspension that each of the secondary conduits concerned is intended to convey. Dispositif selon la revendication 1, caractérisé en ce que le moyen pneumatique est apte à générer une perte de charge contrôlée par des moyens de réglage, manuels ou automatisés, dudit moyen pneumatique.Device according to claim 1, characterized in that the pneumatic means is capable of generating a pressure drop controlled by means of adjustment, manual or automated, of said pneumatic means. Dispositif selon la revendication 2, caractérisé en ce que les moyens de réglage du moyen pneumatique font partie d'une boucle de régulation, sous commande d'une unité de contrôle connectée à au moins un moyen de mesure de qualité ou d'épaisseur du revêtement déposé sur le substrat.Device according to claim 2, characterized in that the means for adjusting the pneumatic means form part of a regulation loop, under the control of a control unit connected to at least one means for measuring the quality or thickness of the coating deposited on the substrate. Dispositif selon l'une des revendications précédentes, caractérisé en ce que le moyen pneumatique qui équipe les conduits secondaires (8) comporte au moins un conduit d'amenée de gaz auxiliaire (22) qui débouche dans chacun desdits conduits.Device according to one of the preceding claims, characterized in that the pneumatic means which equips the secondary conduits (8) comprises at least one auxiliary gas supply conduit (22) which opens into each of said conduits. Dispositif selon la revendication 4, caractérisé en ce que chaque conduit d'amenée de gaz auxiliaire (22) est muni d'un moyen de réglage de débit ou pression de gaz.Device according to claim 4, characterized in that each auxiliary gas supply pipe (22) is provided with a means for adjusting the gas flow or pressure. Dispositif selon l'une des revendications précédentes, caractérisé en ce que les conduits secondaires (8) comportent des canalisations, de préférence souples, dont les extrémités débouchant à l'entrée de la cavité de la buse sont constituées par des injecteurs (9) rigides, notamment métalliques.Device according to one of the preceding claims, characterized in that the secondary conduits (8) comprise pipes, preferably flexible, the ends of which open out at the entrance to the cavity of the nozzle consist of rigid injectors (9) , especially metallic. Dispositif selon la revendication 6, caractérisé en ce que les moyens pneumatiques comportent des amenées de gaz auxiliaires (22) qui débouchent dans les conduits secondaires (8) en tout point de la canalisation ou au niveau de la jonction canalisation-injecteur ou au niveau de l'injecteur (9).Device according to claim 6, characterized in that the pneumatic means comprise auxiliary gas supplies (22) which open into the secondary conduits (8) at any point of the pipeline or at the level of the pipeline-injector junction or at the level of the injector (9). Dispositif selon l'une des revendications précédentes, caractérisé en ce que chacun des conduits secondaires (8) destinés à véhiculer la suspension poudre-gaz est muni à son extrémité d'un injecteur (9), les injecteurs des conduits étant régulièrement disposés en ligne dans l'orifice d'entrée de la cavité (11) de la buse sur toute sa longueur et étant tous munis d'une arrivée de gaz auxiliaire (22) à débit de gaz variable et en ce que la cavité (11) de la buse (24) est également munie de moyens d'injection de gaz sous pression (19) pour entraîner la suspension poudre-gaz émise par les injecteurs (9), moyens d'injection de préférence disposés symétriquement de part et d'autre de la ligne d'injecteurs.Device according to one of the preceding claims, characterized in that each of the secondary conduits (8) intended to convey the powder-gas suspension is provided at its end with an injector (9), the injectors of the conduits being regularly arranged in line in the inlet orifice of the cavity (11) of the nozzle over its entire length and being all provided with an auxiliary gas inlet (22) with variable gas flow and in that the cavity (11) of the nozzle (24) is also provided with means for injecting pressurized gas (19) to drive the powder-gas suspension emitted by the injectors (9), injection means preferably arranged symmetrically on either side of the line of injectors. Procédé de mise en oeuvre du dispositif selon l'une des revendications précédentes, caractérisé en ce que les moyens pneumatiques introduisent un jet de gaz dans chacun des conduits secondaires (8) et en ce qu'on règle séparément le débit de chacun desdits jets, ce débit pouvant prendre toute valeur entre 0 et 100% d'un débit donné.Method for using the device according to one of the preceding claims, characterized in that the pneumatic means introduce a gas jet into each of the secondary conduits (8) and in that the flow rate of each of said jets is adjusted separately, this flow can take any value between 0 and 100% of a given flow. Procédé selon la revendication 9, caractérisé en ce que les moyens pneumatiques émettent en permanence un jet de gaz dont on régule le débit autour d'une valeur de débit donnée.Method according to claim 9, characterized in that the pneumatic means continuously emit a jet of gas, the flow of which is regulated around a given flow value. Procédé selon la revendication 10, caractérisé en ce que la valeur de débit autour de laquelle on régule le débit de chacun des jets de gaz émis par les moyens pneumatiques est d'environ 20 à 60%, notamment 50% du débit de gaz moyen de la suspension poudre-air véhiculée par chaque conduit secondaire (8).Method according to claim 10, characterized in that the flow value around which the flow of each of the gas jets emitted by the pneumatic means is regulated is approximately 20 to 60%, in particular 50% of the average gas flow of the powder-air suspension conveyed by each secondary conduit (8). Procédé selon l'une des revendications 9 à 11, caractérisé en ce qu'on régule la valeur de débit pour chacun des jets émis par les moyens pneumatiques en fonction des variations d'épaisseur détectées dans le revêtement (23) déposé en aval de la buse (24) de distribution.Method according to one of Claims 9 to 11, characterized in that the flow value is regulated for each of the jets emitted by the pneumatic means as a function of the thickness variations detected in the coating (23) deposited downstream of the dispensing nozzle (24). Utilisation du dispositif selon l'une des revendications 1 à 8 ou du procédé selon l'une des revendications 9 à 12 pour déposer des revêtements (23) d'oxydes métalliques par pyrolyse sur un ruban de verre float chaud (1), notamment des revêtements d'oxydes dopés du type SnO₂:F à partir de poudre de difluorure de dibutylétain ou du type ITO à partir de poudre de formiate d'indium et de dibutyloxyde d'étain.Use of the device according to one of claims 1 to 8 or the method according to one of claims 9 to 12 for depositing oxide coatings (23) metallic by pyrolysis on a ribbon of hot float glass (1), in particular coatings of doped oxides of SnO₂: F type from dibutyltin difluoride powder or ITO type from indium formate powder and dibutyloxide of tin.
EP95402160A 1994-09-27 1995-09-27 Device for distributing pulverulent solids on the surface of a substrate for coating this substrate Expired - Lifetime EP0704249B1 (en)

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EP0130919A1 (en) 1983-07-04 1985-01-09 Saint Gobain Vitrage International Device for distributing powders suspended in a gas
EP0374023B1 (en) 1988-12-14 1994-05-11 Saint-Gobain Vitrage International Device for coating a moving substrate with a powdery solid material
EP0392902A1 (en) 1989-04-12 1990-10-17 Saint-Gobain Vitrage International Method of modifying the relative positions of a plurality of aligned parts, and device for performing this method

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FR2724853A1 (en) 1996-03-29
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ES2144111T3 (en) 2000-06-01
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DE69514743T2 (en) 2000-07-27
US5795388A (en) 1998-08-18

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