• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    A method of surface annealing a substrate having a coating, said method comprising - moving the substrate (1) carrying the annealing coating (2) under a flash lamp (4), the face of the substrate (1) carrying said coating ( 2) being turned towards the flash lamp (4), - the irradiation of the coating to be annealed by the intense pulsed light emitted by the flash lamp (4) through a mask (3) located between the flash lamp and the coating to be annealed and having a slot whose longitudinal axis is perpendicular to the direction of travel of the substrate, the frequency of the flash lamp and the speed of travel of the substrate being adjusted so that each point of the coating to be annealed receives at least one pulse characterized in that the distance between the lower face of the mask and the surface of the coating to be annealed is at most equal to 1 mm, and in that the shape and the extent of the slot are such that the mask obscures the coating to be annealed in all areas where the light intensity which, in the absence of a mask, would arrive at the level of the coating to be annealed is less than a threshold light intensity, hereinafter called the nominal luminous intensity.
    公开号:FR3025936A1
    申请号:FR1458520
    申请日:2014-09-11
    公开日:2016-03-18
    发明作者:Lorenzo Canova；Emmanuel Mimoun；Brice Dubost
    申请人:Saint Gobain Glass France SAS；Compagnie de Saint Gobain SA；
    IPC主号:
    专利说明:

    [0001] The present invention relates to a method and an apparatus for the rapid annealing of thin layers deposited on flat substrates, by means of flash lamps. It is known to carry out local and rapid laser annealing (laser flash heating) of thin coatings deposited on flat substrates. For this purpose, the substrate is scanned with the coating to be annealed under a laser line, or a laser line above the substrate carrying the coating (see, for example, WO2008 / 096089 and WO 2013/156721). Laser annealing is used to heat thin coatings at high temperatures, on the order of several hundred degrees, while preserving the underlying substrate. More recently, it has been proposed to replace, in such a surface annealing process, laser light sources, such as laser diodes, with Intense Pulsed Light (IPL) lamps also known as flash lamps. In the international application WO 2013/026817 there is thus proposed a method of manufacturing a low-emission coating comprising a step of depositing a thin layer based on silver, then a step of rapid surface annealing of said layer in the purpose of decreasing its emissivity and increasing its conductivity. For the annealing step, the substrate coated with the silver layer is scrolled under a set of flash lamps downstream of the deposition station of the layer. In attempting to reproduce this process with Planitherm ONE® glazing (clear glass coated with a stack of thin transparent layers, including some layers of noble metals, deposited by vacuum sputtering), the Applicant has observed inhomogeneities in the appearance of coating after annealing. Figure 1 shows a Planitherm ONE® coating after annealing with flash lamps under the following conditions: 3025936 - 2 - Intensity of each light pulse: 35 J / cm2 Duration of each pulse: 2.7 ms Pulse frequency: 0, 5 Hz Substrate travel speed: 0.78 m / m in 5 Approximate width of the area illuminated by the lamp in the substrate direction: 10 cm Distance between the flash lamp and the substrate: 20 mm Striations are observed Periodic, about 2.6 cm apart, which were absent from the coating directly after depositing the Planitherme® ONE stack. These streaks do not appear either when annealing the coating by running an identical substrate under a laser line generated by laser diodes. The appearance of defects in appearance homogeneity seems to be related to the use of a pulsed light source 15 (flash lamp) to replace a continuous light source (laser diode). After numerous attempts to better understand this undesirable phenomenon, the Applicant has found a solution, quite simple to implement, which makes it possible to considerably reduce, if not completely eliminate, this periodic defect of homogeneity of the annealed substrate. This solution consists in interposing between the flash lamp and the coating to anneal an opaque mask having an irradiation slot. In order for the use of such a mask to result in the reduction or elimination of inhomogeneities in the annealed coating, the following conditions must be met: the mask and the irradiation slot must have a fixed position by relative to the flash lamp, - The frequency of the flash lamp and the speed of travel of the substrate 30 must be such that each point of the coating receives at least one light pulse, - The mask must be positioned as close as possible to the surface of the The shape and extent of the irradiation slot must be such that the mask intercepts the light of the lamp, that is to say, the coating to be annealed, at most within a few millimeters thereof. to say, occult the substrate, in all the zones where the luminous intensity is lower than a threshold luminous intensity, hereinafter called nominal luminous intensity. In the present application, the term "nominal luminous intensity" is the intensity of a light pulse, of a given duration, beyond which a second pulse of intensity greater than or equal to that of the first pulse and of the same duration as this does not cause a color change in reflection of the coating. The color difference is the difference between two colors (DE *) as defined by the color system CIE L * a * b * (illuminant D65). The CIELab system defines a sphere-shaped color space with an L * axis characterizing clarity, an axis a * red / green and a axis b * blue / yellow. A value greater than 0 corresponds to hues with a red component, a negative a * to hues with a green component, a positive b * value to hues with a yellow component and a negative b * value to hues with a blue component. In the formula above L1, a1 and b1 are the coordinates in the color space CIELab of the first color 25 and L2, a2 and b2 those of the second. When irradiating the coating to be annealed with a first pulse of sufficient intensity, this irradiation causes a change in the color of the coating (AE * 1). Then, when this same irradiation is repeated with a pulse of the same energy (same intensity, same duration), the additional color change caused results in a total color change (AE * 2). When AE2 is substantially equal to DES, that is to say when AE2 - DES is less than or equal to 1, it is considered that the second pulse has not had a significant impact on the color of the coating. and that the intensity of the pulse is greater than or equal to the nominal intensity as defined above. On the other hand, when the second pulse causes a significant color change (AE * 2 - AE * 1> 1), the second pulse is considered to affect the color of the coating and the light intensity is considered to be less than the nominal luminous intensity. The light intensities to be considered are of course those measured at the level of the work plane, that is to say at the level of the coating to be annealed. The light emitted by the flash lamp has, at the level of the working plane, a light intensity profile, also called power density profile, at least one zone where the light intensity is greater than or equal to the intensity nominal as defined above, and other zones, generally on the periphery of the irradiated zone, where the luminous intensity is lower than the nominal luminous intensity.
    [0002] The irradiation mask must be positioned between the lamp and the coating so as to intercept all of the light which, at the level of the coating to be annealed, has a luminous intensity lower than the nominal intensity. The mask may optionally intercept a small portion of the light having an intensity greater than or equal to the nominal intensity. The present invention relates to a method of surface annealing a substrate having a coating, said method comprising: - running the substrate carrying the coating to be annealed under a flash lamp emitting intense pulsed light, the face of the substrate carrying said coating being turned towards the flash lamp, - the irradiation of the coating to be annealed by the intense pulsed light emitted by the flash lamp through a mask located, in a fixed position relative to the flash lamp, between the flash lamp and the coating to be annealed and having a slot whose longitudinal axis is perpendicular to the direction of travel of the substrate, the frequency of the flash lamp and the speed of travel of the substrate being adjusted so that each point of the coating at annealing receives at least one light pulse, characterized in that the distance between the underside of the mask and the surface of the coating The annealing agent is at most equal to 1 mm, preferably at most 500 μm, ideally at most 100 μm, and in that the shape and extent of the slit are such that the mask obscures the a coating to be annealed in all areas where the light intensity which, in the absence of a mask, would arrive at the level of the coating to be annealed is less than a threshold light intensity, hereinafter referred to as the nominal luminous intensity. Whenever mention is made of a "flashlamp" in the present application, this term designates a single flashlamp or a set of flashlamps, for example 5 to 20 lamps, or 8 to 15 lamps. , arranged preferably parallel to each other, and associated with one or more mirrors. Such a set of flash lamps and mirrors is used for example in the method disclosed in WO 2013/026817. The function of the mirrors is to direct all the light emitted by the lamps in the direction of the substrate and to impart to the luminous intensity profile a desired truncated bell shape having a central plateau of approximately constant intensity (less than 5%) and lateral flanks where the intensity gradually decreases. These mirrors can be flat mirrors or focusing mirrors. The flashlamps used in the present invention are generally in the form of glass or quartz tubes sealed and filled with a rare gas, provided with electrodes at their ends. Under the effect of a short-term electrical pulse, obtained by discharging a capacitor, the gas ionizes and produces a particularly intense incoherent light. The emission spectrum generally comprises at least two emission lines; it is preferably a continuous spectrum having a maximum emission in the near ultraviolet. The lamp is preferably a xenon lamp. It can also be an argon, helium or krypton lamp. The emission spectrum preferably comprises several lines, especially at wavelengths ranging from 160 to 1000 nm. The duration of the (flash) light pulse is preferably in the range of 0.05 to 20 milliseconds, especially 0.1 to 5 milliseconds. The repetition rate (frequency) is preferably in a range from 0.1 to 5 Hz, in particular from 0.2 to 2 Hz. The lamp, or lamps, is preferably arranged transversely to the longer sides of the substrate. . It has a length preferably of at least 1 m, especially at least 2 m and even at least 3 m, so as to allow the treatment of large substrates. The capacitor is typically charged at a voltage of 500 V to 500 kV. The current density is preferably at least 4000 A / cm 2. The total energy density emitted by the flash lamps relative to the surface of the coating is preferably between 1 and 100 J / cm 2, preferably between 2 and 30 J / cm 2, in particular between 5 and 20 J / cm 2. cm2. The substrate bearing the coating to be annealed is preferably glass or glass ceramic. It is preferably transparent, colorless (clear or extra-clear glass) or colored, for example blue, gray, green or bronze. The glass is preferably of the silico-soda-lime type, but it may also be of borosilicate or alumino-borosilicate type glass. The substrate advantageously has at least one dimension greater than or equal to 1 m, or even 2 m and even 3 m. The thickness of the substrate generally varies between 0.1 mm and 19 mm, preferably between 0.7 and 9 mm, in particular between 1 and 6 mm, and even between 2 and 4 mm. The material of the coating to be annealed can in principle be any material, organic or inorganic, which is not destroyed by the superficial annealing treatment and whose physical properties, and in particular the color, are modified. to this treatment. It is preferably a mineral coating, in particular a coating comprising one or more layers of a metal oxide and / or one or more layers of a metal, preferably a noble metal, with the metallic state. In one embodiment, the coating to be annealed preferably comprises at least one layer of a transparent conductive oxide (TCO). This oxide is preferably selected from indium tin oxide (ITO), indium zinc oxide (IZO), tin oxide doped with antimony or fluorine ( ATO and FTO), zinc oxide doped with aluminum (AZO) and / or gallium (GZO) and / or titanium, niobium and / or tantalum doped titanium oxide, cadmium stannate or zinc.
    [0003] A particularly preferred oxide is tin and indium oxide, frequently referred to as "ITO". The atomic percentage of Sn is preferably in a range from 5 to 70%, especially from 6 to 60%, advantageously from 8 to 12%. Compared to other conductive oxides, such as fluorine-doped tin oxide, ITO is preferred for its high electrical conductivity, allowing the use of low thicknesses to achieve a good emissivity or resistivity. In another embodiment, the coating to be annealed comprises one or more thin layers of a metal, in particular a noble metal, typically silver or gold-based layers, preferably at least one layer. silver. The physical thickness of the coating to be annealed is advantageously at least equal to 30 nm and at most equal to 5000 nm, preferably between 50 nm and 2000 nm. In the method of the present invention, the substrate bearing the coating is conveyed. to anneal under or in front of the flash lamps partially obscured by the irradiation mask. In order to increase the energy efficiency of the process, the flash lamps are preferably close to the coating to be annealed, advantageously located at less than 20 cm, preferably at less than 10 cm and in particular at less than 5 cm. . The lower this distance, the higher the luminous intensity at the level of the work surface (coating to anneal) is important for a given operating power.
    [0004] The irradiation mask has a slot whose longitudinal axis is perpendicular to the direction of travel of the substrate. The simplest form of the slot guaranteeing a homogeneous irradiation of the coating to be annealed is the rectangle. The slot therefore preferably has a substantially rectangular shape. More complex, less preferred forms, however, are also conceivable and the invention is not limited to the embodiment where the slot is a rectangle. A slot in the form of an arc, a zigzag or a corrugation would be equivalent to a rectangular slot provided that the upstream edge and the downstream edge of the slot are parallel, allowing the perfect juxtaposition (without vacuum) of the irradiation zones. corresponding to the successive light pulses. The substrate carrying the coating to be annealed can be set in scrolling motion using any suitable mechanical conveyor means, for example using strips, rollers, translational trays. The conveying system makes it possible to control and regulate the speed of movement. The rate of travel of the substrate should be adjusted according to the frequency of the pulses and the slot width of the mask so that each point of the coating receives at least one light pulse, ie the speed of scrolling should be lower. or equal to the L / P ratio of the width of the slot (L) to the period (P) separating two pulses. For an irradiation frequency of 1 Hz and a width of the slot of 10 cm, the running speed of the substrate must thus be at most 10 cm / second. When the running speed of the substrate is less than 30 L / P, a certain number of points receive two light pulses (overlap area), which is not very favorable from the point of view of the energy efficiency of the process. The existence of a relatively narrow area of coverage, however, ensures the continuity of the irradiated area in case of small variations in the speed of travel. Therefore, in a preferred embodiment of the method of the present invention the frequency of the flashlamp, the width of the slot and the rate of travel of the substrate are such that at least 90%, preferably at least 95% more preferably at least 98% of the points of the coating to be annealed receive a single light pulse. In other words, at most 10%, preferably at most 5%, and more preferably at most 2% of the points of the coating receive two light pulses. The speed of travel of the substrate is therefore preferably between L / P and 0.9 L / P. The rate of travel of the substrate carrying the coating to be annealed is advantageously between 0.1 and 30 m / minute, preferably between 1 and 20 m / minute, and in particular between 2 and 10 m / minute. The width of the irradiation slot is advantageously between 1 and 50 cm, preferably between 5 and 20 cm. The length of the slot is substantially equal to the width of the coating to be annealed, namely generally at least 1 m, preferably at least 2 m, in particular at least 3 m. As indicated above, the irradiation mask must be as close as possible to the coating to be annealed, that is to say the distance between its underside and the surface of the coating to be annealed must not exceed 1 mm, Preferably, it does not exceed 500 microns, and most preferably is at most 100 microns. Of course, in the context of a continuous process that involves the continuous movement of the substrate under fixed lamps - or the continuous movement of a lamp and a mask relative to a fixed substrate - it is impossible to pose the mask directly in contact with the coating to be annealed. It is essential, to adjust the distance between the mask and the coating to be annealed, to take into account the undulations of the surface of the substrate which have repercussions on the surface of the coating to be annealed. It is therefore important to understand that there is not only a maximum distance between the mask and the surface of the coating but also a minimum distance which must be sufficient to guarantee the absence of contact between the mask and the coating. This minimum distance will of course depend on the flatness of the substrate and / or the roughness of the coating. It may be, for example, 10 μm, even 20 μm, or even 50 μm. The present invention also relates to an apparatus for surface annealing a substrate having a coating to be annealed, particularly suitable for carrying out the process of the present application. The apparatus of the present invention comprises a flash lamp capable of emitting intense pulsed light, a transport means for scrolling a flat substrate having a coating to be annealed in front of the flash lamp, a mask located in a fixed position with respect to the flash lamp between the flash lamp and the conveying means, said mask having a slot whose longitudinal axis is perpendicular to the direction of travel of the substrate and which is positioned so that the light emitted by the flash lamp 20 is projected through the slot towards the flat substrate carrying a coating to be annealed, and further comprises means for adjusting the distance between the mask and the transport means such as the distance between the lower face of the mask and the surface of the coating to be annealed may be adjusted to a value of less than 1 mm, preferably less than 500 μm, in particular less than 100 μm. The mask will preferably be made of a metallic material, typically aluminum or copper. It may be coated with an absorbent layer, or undergo an anodizing treatment that makes it absorbent, to absorb all the light it catches. In this case, the body of the mask will preferably be in contact with a cooling circuit, so as to maintain its temperature below 100 ° C., preferably below 50 ° C.
    [0005] Another possibility is the use of a diffusing reflective layer for the mask, so that the intercepted light is not absorbed but diffused in order to lower the reflected luminous intensity and thus its dangerousness.
    [0006] The thickness of the mask at the edges of the slot should be as small as possible, preferably less than 500 μm, or even less than 200 μm or even less than 100 μm. In order to ensure the mechanical rigidity of the mask and its cooling, the parts thereof that are farthest away from the slot 10 may be thicker. The edges of the slot can then be made bevel, so that the light is intercepted by the thinnest part. The invention is explained in more detail with reference to the figures. Figure 1 shows a photograph of a substrate bearing a Planitherme® ONE coating irradiated under the conditions as indicated above in the absence of a mask. There are periodic horizontal streaks spaced about 2.6 cm apart. Figure 2 is a photograph of a Planitherme® ONE substrate treated according to the method of the invention. The streaks visible in FIG. 1 have completely disappeared thanks to the interposition of a mask under the conditions according to the invention. Fig. 3 is an explanatory diagram showing the operation of the method of the present invention and, more particularly, the proper positioning of the irradiation mask in relation to the luminous intensity profile of the lamps. In this figure 3 a continuous flat substrate 1 carrying a coating 2 annealing is conveyed by rollers 6 in the direction of travel indicated by the arrow. The annealing coating 2 is irradiated with light emitted by a set of lamps 4 and directed downwards by means of a set of mirrors 5, through a mask 3. The distance between the two parts of the mask 3 corresponds to to the width of the longitudinal slot. The distance between the lower face of the mask 3 and the upper face of the coating to be annealed 2 is less than 1 mm. In the lower part of the figure is represented the intensity profile of a light pulse such as it would exist at the level of the coating to be annealed 2 in the absence of the mask 3. The mask 3 is positioned such that the light having an intensity lower than the nominal intensity is intercepted by the opaque areas of the mask.
    权利要求:
    Claims (9)
    [0001]
    REVENDICATIONS1. A method of surface annealing a substrate having a coating, said method comprising: - moving the substrate (1) carrying the annealing coating (2) under a flash lamp (4) emitting intense pulsed light, the substrate face carrying said coating being turned towards the flash lamp, - the irradiation of the coating to be annealed by the intense pulsed light emitted by the flash lamp through a mask (3) located in a fixed position with respect to the flash lamp, between the flash lamp and the coating to be annealed and having a slot whose longitudinal axis is perpendicular to the direction of travel of the substrate, the frequency of the flash lamp and the speed of travel of the substrate being adjusted so that each point of the coating to anneal receives at least one light pulse, characterized in that the distance between the lower face of the mask and the surface of the coating to be annealed is at most equal to 1 mm, preferably at most equal to 500 μm, ideally at most equal to 100 μm, and in that the shape and extent of the slot are such that the mask conceals the coating to be annealed in all areas where the light intensity which, in the absence of a mask, would arrive at the level of the coating to be annealed is less than a threshold light intensity, hereinafter referred to as the nominal luminous intensity.
    [0002]
    2. Method according to claim 1, characterized in that the slot has a substantially rectangular shape.
    [0003]
    3. Method according to claim 1 or 2, characterized in that the frequency of the flashlamp, the width of the slot and the running speed of the substrate are such that at least 90%, preferably at least 95% more preferably at least 98% of the points of the coating to be annealed receive a single light pulse.
    [0004]
    4. Method according to any one of the preceding claims, characterized in that the length of the slot is substantially equal to the width of the coating to be annealed.
    [0005]
    5. Method according to any one of the preceding claims, characterized in that the width of the coating to be annealed is at least 1 m, preferably at least 2 m, in particular at least 3 m.
    [0006]
    6. Method according to one of the preceding claims, characterized in that the width of the slot is between 1 and 50 cm, preferably between 5 and 20 cm.
    [0007]
    7. Method according to any one of the preceding claims, characterized in that the running speed of the substrate carrying the coating to be annealed is between 0.1 and 30 m / minute, preferably between 1 and 20 m / minute. and in particular between 2 and 10 m / minute.
    [0008]
    8. Method according to any one of the preceding claims, characterized in that the coating to be annealed comprises at least one layer of a metal, preferably a layer of silver, or at least one layer of a conductive oxide transparent.
    [0009]
    9. Apparatus for the surface annealing of a substrate having a coating, comprising - A flash lamp (4) capable of emitting intense pulsed light, - A conveying means (6) for scrolling a flat substrate (1). ) having an annealing coating (2) in front of the flash lamp; - a mask (3) located in a fixed position with respect to the flash lamp between the flash lamp and the conveying means, said mask having a slot, longitudinal axis is perpendicular to the running direction of the substrate and is positioned so that the light emitted by the flash lamp is projected through the slot towards the flat substrate having a coating to be annealed, characterized by the fact that comprises means for adjusting the distance between the mask and the transport means such that the distance between the lower face of the mask and the surface of the coating to be annealed can be adjusted to a value of less than 1 mm, from less than 500 μm, in particular less than 100 μm.
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    CN106605290A|2017-04-26|
    AU2015314079A1|2017-04-13|
    BR112017002958A2|2017-12-05|
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    FR3025936B1|2016-12-02|
    CO2017002325A2|2017-06-20|
    US20170291848A1|2017-10-12|
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    法律状态:
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    2016-03-18| PLSC| Search report ready|Effective date: 20160318 |
    2016-09-22| PLFP| Fee payment|Year of fee payment: 3 |
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    2021-06-11| ST| Notification of lapse|Effective date: 20210506 |
    优先权:
    申请号 | 申请日 | 专利标题
    FR1458520A|FR3025936B1|2014-09-11|2014-09-11|METHOD FOR RECLAIMING FLASH LAMPS|FR1458520A| FR3025936B1|2014-09-11|2014-09-11|METHOD FOR RECLAIMING FLASH LAMPS|
    TW104126704A| TWI663637B|2014-09-11|2015-08-17|Process for annealing by flash lamp|
    MX2017002996A| MX2017002996A|2014-09-11|2015-08-20|Annealing method using flash lamps.|
    PCT/FR2015/052238| WO2016038269A1|2014-09-11|2015-08-20|Annealing method using flash lamps|
    CN201580048670.3A| CN106605290A|2014-09-11|2015-08-20|Annealing method using flash lamps|
    AU2015314079A| AU2015314079A1|2014-09-11|2015-08-20|Annealing method using flash lamps|
    US15/507,883| US20170291848A1|2014-09-11|2015-08-20|Annealing method using flash lamps|
    JP2017513808A| JP2017536689A|2014-09-11|2015-08-20|Annealing method using flash lamp|
    BR112017002958A| BR112017002958A2|2014-09-11|2015-08-20|Annealing process by flash lamps|
    KR1020177006735A| KR20170051447A|2014-09-11|2015-08-20|Annealing method using flash lamps|
    EP15767209.8A| EP3192095A1|2014-09-11|2015-08-20|Annealing method using flash lamps|
    EA201790593A| EA201790593A1|2014-09-11|2015-08-20|LOSS FLASH METHOD|
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    CONC2017/0002325A| CO2017002325A2|2014-09-11|2017-03-09|Flash lamp annealing procedure|
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