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WO2004065902A1 - Method and apparatus for the contactless measurement of the thickness of a coating on a substrate - Google Patents

Method and apparatus for the contactless measurement of the thickness of a coating on a substrate Download PDF

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Publication number
WO2004065902A1
WO2004065902A1 PCT/FR2003/003739 FR0303739W WO2004065902A1 WO 2004065902 A1 WO2004065902 A1 WO 2004065902A1 FR 0303739 W FR0303739 W FR 0303739W WO 2004065902 A1 WO2004065902 A1 WO 2004065902A1
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WO
WIPO (PCT)
Prior art keywords
substrate
coating
thickness
ultraviolet radiation
bottle
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/FR2003/003739
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French (fr)
Inventor
Maurice Bourrel
Jean-Michel Chabagno
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Arkema France SA
Arkema SA
Original Assignee
Arkema SA
Atofina SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Arkema SA, Atofina SA filed Critical Arkema SA
Priority to AU2003300621A priority Critical patent/AU2003300621A1/en
Publication of WO2004065902A1 publication Critical patent/WO2004065902A1/en
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01BMEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00Measuring arrangements characterised by the use of optical techniques
    • G01B11/02Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
    • G01B11/06Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material

Definitions

  • the present invention relates to a method and an apparatus for non-contact measurement of the thickness of a coating present on a substrate such as a bottle, in particular, made of glass, or a metal, plastic or ceramic plate.
  • thin layer treatments titanium oxides, titanium oxides, organic lubricating layers, etc.
  • properties such as : mechanical resistance, impact resistance, wear resistance, lubrication, aging, etc.
  • the thin layers which have a thickness of up to a few tens of nanometers, can be made of Sn0 or Ti0 and they are generally deposited at high temperature, that is to say usually between 500 ° C and 600 ° C , just after the bottle is removed from the mold and before entering the annealing arch.
  • the bottle In order for the bottle to have the desired properties, it is important to control the thickness and the homogeneity of the deposits of the oxide layers. In fact, a thickness that is too small does not provide sufficient wear resistance properties and does not allow good adhesion of the subsequent cold treatments. Conversely, too thick, in addition to the fact that it induces excessive use of an expensive product, gives a visible coating, with metallic reflections, which is not acceptable from an aesthetic point of view.
  • the thickness of the thin oxide layers is usually measured in the control laboratory on cold bottles, that is to say at least an hour and a half after the production of the bottle. If the coating does not comply with the specifications, the settings must be modified deposit machine. This results in a loss of production lasting around 1.5 hours.
  • Various methods can be used to measure the thicknesses of thin layers; mention may be made, for example, of optical methods such as infrared reflection measurements, polarized light measurements, spectral analysis methods, ellipsometry, X-ray fluorescence methods, surface analysis methods such as 1 ESCA or SIMS, or methods by optical or mechanical profilometry, or methods of chemical analysis after dissolution of the thin layer in an acid.
  • optical methods such as infrared reflection measurements, polarized light measurements, spectral analysis methods, ellipsometry, X-ray fluorescence methods, surface analysis methods such as 1 ESCA or SIMS, or methods by optical or mechanical profilometry, or methods of chemical analysis after dissolution of the thin layer in an acid.
  • the best known method is that used by the HECM (Hot End Coating Meter) device from the company AGR (American Glass Research, Butler, Pa, USA).
  • This apparatus determines the thickness of the coating by measuring the intensity of the light reflected from the coated glass surface.
  • a fiber-optic system sends infrared light to the surface of the glass and analyzes the reflected ray.
  • This method requires the use of a coupling liquid to adapt the refractive indices: it is a contact method which cannot therefore be used for online measurement. In addition, it cannot be used on a hot bottle. It is therefore only used in the control laboratory.
  • U.S. Patent No. 4,015,127 relates to a method and apparatus for controlling parameters such as the thickness and uniformity of films or coatings on a planar substrate.
  • US Patent No. 5,991,018 relates to an apparatus for inspecting the thickness or the state of deterioration of a coating layer present on the surface of a container such as a bottle. This device determines the thicknesses of the thin layers either by analyzing the spectral distribution (color analysis) of the reflected light or by analyzing the scattered light in the case of measurements by transmission.
  • the object of the invention is to propose a method for measuring the thickness of a coating on a substrate which is simpler than the methods used to date; which allows measurement without contact with the coated substrate and therefore, without having to wait for the coating to be cold, in order to avoid production losses; which is practically indifferent to the temperature of the coating; who performs a measurement in real time; this makes it possible to control the regulation of the coating deposition machine on the substrate to the measurement of the thickness; in this way we can avoid significant production losses; which can be used on a production line; and which gives reliable results, even when, for example in the case of a bottle, the coating is itself covered with an organic lubricating layer.
  • the method according to the invention comprises at least the following steps: an ultraviolet radiation is sent onto the substrate; the reflected radiation is captured; and processing the reflected radiation to determine the thickness of the substrate coating.
  • the invention also aims to provide an apparatus capable of implementing the above method.
  • FIG. 1 represents an apparatus according to the invention
  • FIG. 2 is a graph representing the values of the signal measured by a UN probe as a function of the thickness of a layer of tin oxide
  • FIG. 3 is a graph representing the values of the signal measured by a UV probe as a function of the thickness of a layer of titanium oxide
  • FIG. 1 represents an apparatus according to the invention
  • FIG. 2 is a graph representing the values of the signal measured by a UN probe as a function of the thickness of a layer of tin oxide
  • FIG. 3 is a graph representing the values of the signal measured by a UV probe as a function of the thickness of a layer of titanium oxide
  • FIG. 1 represents an apparatus according to the invention
  • FIG. 2 is a graph representing the values of the signal measured by a UN probe as a function of the thickness of a layer of tin oxide
  • FIG. 3 is a graph representing the values of the signal measured by a UV probe as a function of the thickness of a layer of titanium oxide
  • FIG. 4 is a graph representing the values of the signal measured by a UV probe as a function of the nature of the coating
  • FIG. 5 represents the calibration curve of a UV probe as a function of the thickness of the coating
  • FIG. 6 represents two curves corresponding, for one, to the values of the signal measured with an uncoated bottle and, for the other to the values of the signal measured with the same bottle coated with tin oxide when the bottles pass in front the device
  • FIG. 7 represents the values of the signal measured with a bottle coated with tin oxide, as a function of the probe / bottle distance;
  • FIG. 5 represents the calibration curve of a UV probe as a function of the thickness of the coating
  • FIG. 6 represents two curves corresponding, for one, to the values of the signal measured with an uncoated bottle and, for the other to the values of the signal measured with the same bottle coated with tin oxide when the bottles pass in front the device
  • FIG. 7 represents the values of the signal measured with a bottle coated with tin oxide, as a
  • FIG. 8 represents the values of the signal measured with a bottle coated with tin oxide, as a function of the temperature of the bottle, and the values of the signal measured with a bottle not coated, as a function of the temperature of the bottle;
  • FIG. 9 represents an assembly used to compare the results given by an apparatus according to the prior art and the apparatus according to the invention;
  • FIG. 10 represents the curves obtained by measuring the signals supplied by the apparatus according to the prior art and the apparatus according to the invention, during the rotation of a bottle coated with tin oxide; and
  • Figures 11 and 12 show arrangements used to measure the thickness of the coating at various points on a bottle.
  • the method according to the invention therefore comprises at least the following steps: ultraviolet radiation is sent onto said substrate; the reflected radiation is captured; and processing the reflected radiation to determine the thickness of the substrate coating.
  • An interesting feature of the method according to the invention is that the incident ultraviolet radiation sent to the substrate does not need to be polarized. It is therefore advantageous to dispense with the use of a polarizer.
  • the incident radiation and the reflected radiation are substantially parallel.
  • the incident and reflected radiation are substantially perpendicular to the surface of the substrate where the radiation is absorbed.
  • the method according to the invention can be implemented on all kinds of coated substrates. These substrates can be made of various materials and be of various shapes. As examples of substrates, mention may be made of flat articles, bottles or flasks of glass, ceramic or plastic.
  • the coating whose thickness is to be measured can consist, for example, of various oxides, such as tin oxide, titanium oxide, zinc oxide, or mixtures of oxides, nitrides such than aluminum nitride and in general any coating applied in a thin layer on the substrate capable of reflecting light in the UN 280-400 nm range.
  • various oxides such as tin oxide, titanium oxide, zinc oxide, or mixtures of oxides, nitrides such than aluminum nitride and in general any coating applied in a thin layer on the substrate capable of reflecting light in the UN 280-400 nm range.
  • the method according to the invention finds a very useful application in the measurement of the thickness of coatings of tin or titanium oxide on glass bottles.
  • the method according to the invention makes it possible to measure thicknesses ranging from 0.001 to 0.1 ⁇ m.
  • Apparatus according to the invention makes it possible to measure thicknesses ranging from 0.001 to 0.1 ⁇ m.
  • the apparatus according to the invention is illustrated in FIG. 1. It comprises at least: a source 1 of ultraviolet radiation; a first optical guide 2, which directs the ultraviolet radiation emitted by said source of ultraviolet radiation towards the substrate 11 (incident radiation); a second optical guide 4 which collects and directs the reflected radiation towards means 5, preferably electronic, for detecting and processing the reflected radiation in order to determine the thickness of the coating.
  • any source of ultraviolet radiation can be used.
  • a UV lamp there may be mentioned a UV lamp.
  • it is a source of non-polarized ultraviolet radiation.
  • the power of the radiation is generally from 50 to 250 Watts, but this is not limiting.
  • the incident and reflected radiation are perpendicular (or at least as perpendicular as possible) to the surface of the substrate where the radiation is absorbed.
  • the first and second optical guides 2,4 are substantially coaxial or else substantially parallel. This means that they send and receive light beams (respectively emitted and received), which are substantially parallel to each other.
  • the means for detecting and processing the reflected radiation may comprise a photomultiplier 6 connected to an acquisition card 7 itself connected to a computer 8.
  • the thickness of the coating can be determined by these detection means and for processing the reflected radiation, preferably electronic, in particular the computer, by comparison with a preset calibration curve located in the memory of the computer.
  • the apparatus further comprises a bandpass filter 9 installed at the outlet of the ultraviolet radiation source 1 and / or a second bandpass filter 10 installed at the inlet of the photomultiplier 6.
  • This preferred embodiment has the advantage of being indifferent to the surrounding ambient light which, thus, does not disturb the measurements made.
  • This or these band-pass filters 9, 10 are centered on a wavelength preferably between 310 and 350 nm, advantageously centered on about 330 nm.
  • the first and second optical guides 2,4 are generally placed at a distance ranging from a few O 2004/065902
  • the thickness of the oxide layers can be expressed in CTU
  • Coating Thickness Unit in French: coating thickness unit.
  • 1 CTU corresponds approximately to a thickness of 0.25 nm for coatings based on Sn0 2 or Ti0 2 .
  • the apparatus according to the invention can advantageously be used in a continuous production line for glass bottles 11 provided with a coating.
  • the apparatus according to the invention can also be used as a control apparatus for studying the homogeneity of thin layer coatings on a bottle. To do this, it suffices, for example, either to move the probe (that is to say the two optical guides) along a generator of the bottle ( Figure 11), or to have several probes along 'a generator ( Figure 12), which allows to simultaneously control several areas of the bottle.
  • the probe was about 4 mm from the surface of the glass.
  • FIGS. 2 and 3 show the values of the signal obtained by the UN probe (in mV) as a function of the thickness of the oxide layers expressed in CTU. O 2004/065902
  • Example 2 Using the assembly used in Example 1, the thicknesses of the coatings of Sn0 2 deposited on a green bottle and a brown bottle were measured, using the same bottles (green and brown) not as reference. coated. The probe was about 4 mm from the surface of the bottle. The results are shown in the following table:
  • the 80 CTU layer provides a 50% increase in signal compared to the uncoated bottle.
  • Example 2 Using the assembly used in Example 1, the thicknesses of various coatings deposited on glass bottles were measured: layer of Sn0 alone, organic lubricating layer (based on polyethylene waxes) alone.
  • the lubricating layer practically does not alter the measurement of the thickness of the tin oxide layer. This constitutes one of the advantages of this device compared to the other techniques for measuring the thicknesses of the thin layers mentioned above.
  • the assembly illustrated in FIG. 1 has been used, using a probe with 2 parallel light guides of 4 mm in diameter, which have the advantage of being much more sensitive than the fibers of 400 ⁇ m in diameter.
  • Glass plates coated with SnO 2 placed 20 cm from the probe, were subjected to thickness measurements. The results are shown in Figure 5.
  • the calibration curve in FIG. 5 makes it possible to determine the sensitivity of the probe to the thickness of the coating of Sn0 2 .
  • the sensitivity is of the order of 29 mV / CTU.
  • Example 4 Using the assembly used in Example 4, the thickness of a coating of SnO 2 of 50 CTU was measured on a 1 liter glass bottle, in comparison with the same uncoated bottle. To do this test, the bottles were scrolled in front of the probe. The minimum probe / bottle distance was 20 cm. The results are shown in FIG. 6, in which, to represent the results obtained, the origin of the abscissas for the uncoated bottle has been shifted, so as to facilitate the comparison of the two curves.
  • the response of the UV probe is almost linear as a function of the distance with a slope of approximately 260 mV / cm, whatever the thickness of the coating.
  • the graph in Figure 8 shows the comparative results of a bottle coated with 50 CTU of Sn0 2 and an uncoated bottle, in the temperature range from room temperature to 180 ° C.
  • the UV probe of the device according to the invention was placed (according to the assembly described in the example 1) about 12 mm from a bottle placed on the turntable of the HECM device, as illustrated in Figure 9.
  • the graph in Figure 10 shows the signals obtained by the two probes when the bottle is rotated.
  • the abscissa scale represents the angular position and the ordinate scale corresponds to the (calibrated) CTU values of the HECM device (dotted curve). Values data by the UV probe are calibrated against the C TU values for the abscissa point 0, and, therefore, also expressed in CTU ( continuous curve).

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Length Measuring Devices By Optical Means (AREA)
  • Investigating Or Analysing Materials By Optical Means (AREA)
  • Surface Treatment Of Glass (AREA)

Abstract

The invention relates to a method for the contactless measurement of the thickness of a coating on a substrate (11) such as a bottle (e.g. a glass bottle) or a metal, plastic or ceramic plate. According to the invention, the method comprises at least the following steps consisting in: directing ultraviolet radiation at the substrate (1l), capturing the radiation reflected and processing the reflected radiation in order to determine the thickness of the coating on the substrate (11). The invention also relates to an apparatus which is used to perform the inventive method and to the use of said apparatus in a continuous production line or as a control apparatus in order to examine the homogeneity of the coating on a bottle.

Description

PROCEDE ET APPAREIL POUR LA MESURE SANS CONTACT DE L'EPAISSEUR METHOD AND APPARATUS FOR NON-CONTACT THICKNESS MEASUREMENT

D'UN REVÊTEMENT SUR UN SUBSTRATOF A COATING ON A SUBSTRATE

La présente invention concerne un procédé et un appareil pour la mesure sans contact de l'épaisseur d'un revêtement présent sur un substrat tel qu'une bouteille, notamment, en verre, ou une plaque en métal, plastique ou céramique.The present invention relates to a method and an apparatus for non-contact measurement of the thickness of a coating present on a substrate such as a bottle, in particular, made of glass, or a metal, plastic or ceramic plate.

Dans l'industrie du verre, et en particulier des bouteilles, il est courant d'effectuer des traitements en couche mince (oxydes d'étain, oxydes de titane, couches organiques lubrifiantes, etc) dans le but d'améliorer les propriétés telles que : la résistance mécanique, la résistance à l'impact, la résistance à l'usure, la lubrification, le vieillissement, etc.In the glass industry, and in particular in bottles, it is common to carry out thin layer treatments (tin oxides, titanium oxides, organic lubricating layers, etc.) in order to improve properties such as : mechanical resistance, impact resistance, wear resistance, lubrication, aging, etc.

Les couches minces, qui ont une épaisseur pouvant aller jusqu'à quelques dizaines de nanomètres, peuvent être constituées de Sn0 ou Ti0 et elles sont généralement déposées à haute température, c'est-à-dire habituellement entre 500°C et 600°C, juste après que la bouteille soit sortie du moule et avant l'entrée dans l'arche de recuisson.The thin layers, which have a thickness of up to a few tens of nanometers, can be made of Sn0 or Ti0 and they are generally deposited at high temperature, that is to say usually between 500 ° C and 600 ° C , just after the bottle is removed from the mold and before entering the annealing arch.

Pour que la bouteille possède les propriétés désirées, il est important de maîtriser l'épaisseur et l'homogénéité des dépôts des couches d'oxyde. En effet, une épaisseur trop faible n'apporte pas les propriétés de résistance à l'usure suffisantes et ne permet pas une bonne adhérence des traitements ultérieurs opérés à froid. A l'inverse, une épaisseur trop forte, outre le fait qu'elle induit une utilisation excessive d'un produit coûteux, donne un revêtement visible, avec des reflets métalliques, ce qui n'est pas acceptable du point de vue esthétique.In order for the bottle to have the desired properties, it is important to control the thickness and the homogeneity of the deposits of the oxide layers. In fact, a thickness that is too small does not provide sufficient wear resistance properties and does not allow good adhesion of the subsequent cold treatments. Conversely, too thick, in addition to the fact that it induces excessive use of an expensive product, gives a visible coating, with metallic reflections, which is not acceptable from an aesthetic point of view.

La mesure de l'épaisseur des couches minces d'oxyde est faite habituellement au laboratoire de contrôle sur les bouteilles froides, c'est-à-dire au minimum une heure et demie après la production de la bouteille. Si le revêtement n'est pas conforme aux spécifications, il faut modifier les réglages de la machine de dépôt. Il en résulte une perte de production d'une durée de l'ordre de 1 heure et demie.The thickness of the thin oxide layers is usually measured in the control laboratory on cold bottles, that is to say at least an hour and a half after the production of the bottle. If the coating does not comply with the specifications, the settings must be modified deposit machine. This results in a loss of production lasting around 1.5 hours.

Diverses méthodes peuvent être utilisées pour mesurer les épaisseurs des couches minces ; on peut citer par exemple les méthodes optiques telles que les mesures de réflexion dans l'infrarouge, les mesures en lumière polarisée, les méthodes d'analyse spectrale, 1 ' ellipsométrie, les méthodes par fluorescence X, les méthodes d'analyse de surface comme 1 ' ESCA ou le SIMS, ou les méthodes par profilométrie optique ou mécanique, ou encore les méthodes d'analyse chimique après dissolution de la couche mince dans un acide.Various methods can be used to measure the thicknesses of thin layers; mention may be made, for example, of optical methods such as infrared reflection measurements, polarized light measurements, spectral analysis methods, ellipsometry, X-ray fluorescence methods, surface analysis methods such as 1 ESCA or SIMS, or methods by optical or mechanical profilometry, or methods of chemical analysis after dissolution of the thin layer in an acid.

Au niveau industriel, la méthode la plus connue est celle utilisée par l'appareil HECM (Hot End Coating Meter) de la société AGR (American Glass Research, Butler, Pa, USA) . Cet appareil détermine l'épaisseur du revêtement en mesurant 1 ' intensité de la lumière réfléchie par la surface de verre enduite. Un système à base de fibres optiques permet d'envoyer la lumière infrarouge au niveau de la surface du verre et d'analyser le rayon réfléchi. Cette méthode nécessite l'utilisation d'un liquide de couplage pour adapter les indices de réfraction : c'est une méthode de contact qui ne peut donc pas être utilisée pour une mesure en ligne. En outre, elle ne peut être mise en œuvre sur une bouteille chaude. Elle est par conséquent uniquement employée en laboratoire de contrôle.At the industrial level, the best known method is that used by the HECM (Hot End Coating Meter) device from the company AGR (American Glass Research, Butler, Pa, USA). This apparatus determines the thickness of the coating by measuring the intensity of the light reflected from the coated glass surface. A fiber-optic system sends infrared light to the surface of the glass and analyzes the reflected ray. This method requires the use of a coupling liquid to adapt the refractive indices: it is a contact method which cannot therefore be used for online measurement. In addition, it cannot be used on a hot bottle. It is therefore only used in the control laboratory.

Une autre méthode sans contact par fluorescence X a été proposée par la société Rayonic Sensor Systems GmbH. Cette méthode est cependant peu pratique à mettre en œuvre au niveau industriel à cause de l'équipement lourd qu'elle nécessite. La demande de brevet européen publiée sous le n° 144 115 a trait à un ellipsomètre et à son utilisation pour mesurer les constantes optiques d'une couche mince ou épaisse. Cet ellipsomètre nécessite l'emploi d'un polariseur et d'un spectroscope . La demande de brevet européen publiée sous le n° 661 534 se rapporte à un appareil et un procédé pour la mesure et le contrôle de la densité de réticulation de revêtements sur du verre. Cet appareil, et ce procédé font appel à une lumière polarisée pour s'affranchir de la lumière réfléchie par le substrat .Another non-contact X-ray fluorescence method has been proposed by Rayonic Sensor Systems GmbH. This method is however impractical to implement at the industrial level because of the heavy equipment it requires. European patent application published under No. 144,115 relates to an ellipsometer and its use for measuring the optical constants of a thin or thick layer. This ellipsometer requires the use of a polarizer and a spectroscope. European patent application published under No. 661,534 relates to an apparatus and a method for measuring and monitoring the crosslinking density of coatings on glass. This apparatus, and this method uses polarized light to overcome the light reflected by the substrate.

Le brevet américain n° 4 015 127 a pour objet un procédé et un appareil pour contrôler des paramètres tels que l'épaisseur et l'uniformité de films ou revêtements sur un substrat plan.U.S. Patent No. 4,015,127 relates to a method and apparatus for controlling parameters such as the thickness and uniformity of films or coatings on a planar substrate.

Cet appareil et ce procédé prévoient de diriger un rayonnement sur le film ou revêtement avec angle prédéterminé et ils nécessitent l'emploi d'un polariseur. Le brevet américain n° 5 991 018 concerne un appareil pour l'inspection de l'épaisseur ou de l'état de détérioration d'une couche de revêtement présente sur la surface d'un récipient tel qu'une bouteille. Cet appareil détermine les épaisseurs des couches minces soit par l'analyse de la distribution spectrale (analyse de couleur) de la lumière réfléchie soit par l'analyse de la lumière diffusée dans le cas des mesures par transmission.This apparatus and method provides for directing radiation onto the film or coating with a predetermined angle and requires the use of a polarizer. US Patent No. 5,991,018 relates to an apparatus for inspecting the thickness or the state of deterioration of a coating layer present on the surface of a container such as a bottle. This device determines the thicknesses of the thin layers either by analyzing the spectral distribution (color analysis) of the reflected light or by analyzing the scattered light in the case of measurements by transmission.

L'invention a pour but de proposer un procédé pour la mesure de l'épaisseur d'un revêtement sur un substrat qui soit plus simple que les procédés utilisés jusqu'à ce jour ; qui permette une mesure sans contact avec le substrat revêtu et donc, sans avoir à attendre que le revêtement soit froid, ceci afin d'éviter des pertes de production ; qui soit pratiquement indifférent à la température du revêtement ; qui réalise une mesure en temps réel ; ceci permet d'asservir la régulation de la machine de dépôt de revêtement sur le substrat à la mesure de l'épaisseur ; on peut ainsi de cette manière éviter des pertes importantes de production ; qui puisse être utilisé sur une ligne de production ; et qui donne des résultats fiables, même lorsque, par exemple dans le cas d'une bouteille, le revêtement est lui-même recouvert d'une couche organique lubrifiante. Ainsi, le procédé selon l'invention comprend au moins les étapes suivantes : on envoie un rayonnement ultraviolet sur le substrat ; on capte le rayonnement réfléchi ; et on traite le rayonnement réfléchi en vue de déterminer l'épaisseur du revêtement de substrat.The object of the invention is to propose a method for measuring the thickness of a coating on a substrate which is simpler than the methods used to date; which allows measurement without contact with the coated substrate and therefore, without having to wait for the coating to be cold, in order to avoid production losses; which is practically indifferent to the temperature of the coating; who performs a measurement in real time; this makes it possible to control the regulation of the coating deposition machine on the substrate to the measurement of the thickness; in this way we can avoid significant production losses; which can be used on a production line; and which gives reliable results, even when, for example in the case of a bottle, the coating is itself covered with an organic lubricating layer. Thus, the method according to the invention comprises at least the following steps: an ultraviolet radiation is sent onto the substrate; the reflected radiation is captured; and processing the reflected radiation to determine the thickness of the substrate coating.

L'invention vise également à proposer un appareil apte à la mise en œuvre du procédé précité.The invention also aims to provide an apparatus capable of implementing the above method.

Un tel appareil comprend au moins : une source de rayonnement ultraviolet ; un premier guide optique qui dirige le rayonnement ultraviolet émis par ladite source de rayonnement ultraviolet vers le substrat ; un second guide optique qui capte et dirige le rayonnement réfléchi vers des moyens de détection et de traitement du rayonnement réfléchi en vue de déterminer l'épaisseur du revêtement. D'autres caractéristiques et avantages de l'invention apparaîtront à la lecture de l'exposé qui suit et qui est donné en référence aux dessins dans lesquels : la figure 1 représente un appareil selon l'invention ; la figure 2 est un graphique représentant les valeurs du signal mesuré par une sonde UN en fonction de l'épaisseur d'une couche d'oxyde d'étain ; la figure 3 est un graphique représentant les valeurs du signal mesuré par une sonde UV en fonction de l'épaisseur d'une couche d'oxyde de titane ; la figure 4 est un graphique représentant les valeurs du signal mesuré par une sonde UV en fonction de la nature du revêtement ; la figure 5 représente la courbe de calibration d'une sonde UV en fonction de l'épaisseur du revêtement ; la figure 6 représente deux courbes correspondant, pour l'une, aux valeurs du signal mesuré avec une bouteille non revêtue et, pour l'autre aux valeurs du signal mesuré avec la même bouteille revêtue d'oxyde d'étain lorsque les bouteilles défilent devant l'appareil ; la figure 7 représente les valeurs du signal mesuré avec une bouteille revêtue d'oxyde d'étain, en fonction de la distance sonde/bouteille ; la figure 8 représente les valeurs du signal mesuré avec une bouteille revêtue d'oxyde d'étain, en fonction de la température de la bouteille, et les valeurs du signal mesuré avec une bouteille non revêtue, en fonction de la température de la bouteille ; la figure 9 représente un montage utilisé pour comparer les résultats donnés par un appareil selon l'art antérieur et l'appareil selon l'invention ; la figure 10 représente les courbes obtenues en mesurant les signaux fournis par l'appareil selon l'art antérieur et l'appareil selon l'invention, lors de la rotation d'une bouteille revêtue d'oxyde d'étain ; et les figures 11 et 12 représentent des montages utilisés pour mesurer l'épaisseur du revêtement en divers points d'une bouteille.Such an apparatus comprises at least: a source of ultraviolet radiation; a first optical guide which directs the ultraviolet radiation emitted by said source of ultraviolet radiation towards the substrate; a second optical guide which collects and directs the reflected radiation towards means for detecting and processing the reflected radiation in order to determine the thickness of the coating. Other characteristics and advantages of the invention will appear on reading the description which follows and which is given with reference to the drawings in which: FIG. 1 represents an apparatus according to the invention; FIG. 2 is a graph representing the values of the signal measured by a UN probe as a function of the thickness of a layer of tin oxide; FIG. 3 is a graph representing the values of the signal measured by a UV probe as a function of the thickness of a layer of titanium oxide; FIG. 4 is a graph representing the values of the signal measured by a UV probe as a function of the nature of the coating; FIG. 5 represents the calibration curve of a UV probe as a function of the thickness of the coating; FIG. 6 represents two curves corresponding, for one, to the values of the signal measured with an uncoated bottle and, for the other to the values of the signal measured with the same bottle coated with tin oxide when the bottles pass in front the device; FIG. 7 represents the values of the signal measured with a bottle coated with tin oxide, as a function of the probe / bottle distance; FIG. 8 represents the values of the signal measured with a bottle coated with tin oxide, as a function of the temperature of the bottle, and the values of the signal measured with a bottle not coated, as a function of the temperature of the bottle; FIG. 9 represents an assembly used to compare the results given by an apparatus according to the prior art and the apparatus according to the invention; FIG. 10 represents the curves obtained by measuring the signals supplied by the apparatus according to the prior art and the apparatus according to the invention, during the rotation of a bottle coated with tin oxide; and Figures 11 and 12 show arrangements used to measure the thickness of the coating at various points on a bottle.

EXPOSE DETAILLE DE L'INVENTION Procédé selon l'inventionDETAILED DESCRIPTION OF THE INVENTION Process according to the invention

Le procédé selon l'invention comprend donc au moins les étapes suivantes : on envoie un rayonnement ultraviolet sur ledit substrat ; on capte le rayonnement réfléchi ; et on traite le rayonnement réfléchi en vue de déterminer l'épaisseur du revêtement de substrat. Une particularité intéressante du procédé selon l'invention est que le rayonnement ultraviolet incident envoyé sur le substrat n'a pas besoin d'être polarisé. On peut donc avantageusement se passer du recours à un polariseur.The method according to the invention therefore comprises at least the following steps: ultraviolet radiation is sent onto said substrate; the reflected radiation is captured; and processing the reflected radiation to determine the thickness of the substrate coating. An interesting feature of the method according to the invention is that the incident ultraviolet radiation sent to the substrate does not need to be polarized. It is therefore advantageous to dispense with the use of a polarizer.

De préférence, le rayonnement incident et le rayonnement réfléchi sont sensiblement parallèles. Ainsi, cela permet d'éviter d'envoyer et de capter ces rayonnements selon des angles différents et prédéterminés par rapport au revêtement dont l'épaisseur est à déterminer, comme cela est le cas dans les techniques de l'art antérieur. Avantageusement, les rayonnements incident et réfléchi sont sensiblement perpendiculaires à la surface du substrat où le rayonnement est absorbé. O 2004/065902Preferably, the incident radiation and the reflected radiation are substantially parallel. Thus, this makes it possible to avoid sending and picking up this radiation at different and predetermined angles with respect to the coating whose thickness is to be determined, as is the case in the techniques of the prior art. Advantageously, the incident and reflected radiation are substantially perpendicular to the surface of the substrate where the radiation is absorbed. O 2004/065902

66

Comme longueur d'onde du rayonnement ultraviolet, on utilise de préférence une longueur d'onde comprise entre 280 et 400 nm, avantageusement comprise entre 300 et 350 nm, et encore plus avantageusement une longueur d'onde d'environ 330 nm.As the wavelength of the ultraviolet radiation, a wavelength of between 280 and 400 nm, advantageously between 300 and 350 nm, and even more advantageously a wavelength of approximately 330 nm, is preferably used.

Le procédé selon l'invention peut être mis en œuvre sur toutes sortes de substrats revêtus. Ces substrats peuvent être constitués de matières diverses et être de formes diverses. A titre d'exemples de substrats, on peut citer des articles plats, des bouteilles ou des flacons de verre, céramique ou plastique.The method according to the invention can be implemented on all kinds of coated substrates. These substrates can be made of various materials and be of various shapes. As examples of substrates, mention may be made of flat articles, bottles or flasks of glass, ceramic or plastic.

Le revêtement dont on souhaite mesurer l'épaisseur peut être constitué par exemple d'oxydes divers, tels que l'oxyde d'étain, l'oxyde de titane, l'oxyde de zinc, ou des mélanges d'oxydes, des nitrures tels que nitrure d'aluminium et d'une manière générale tout revêtement appliqué en couche mince sur le substrat susceptible de réfléchir la lumière dans le domaine UN 280-400 nm.The coating whose thickness is to be measured can consist, for example, of various oxides, such as tin oxide, titanium oxide, zinc oxide, or mixtures of oxides, nitrides such than aluminum nitride and in general any coating applied in a thin layer on the substrate capable of reflecting light in the UN 280-400 nm range.

Ainsi, le procédé selon l'invention trouve une application fort utile dans la mesure de l'épaisseur de revêtements d'oxyde d'étain ou de titane sur des bouteilles de verre.Thus, the method according to the invention finds a very useful application in the measurement of the thickness of coatings of tin or titanium oxide on glass bottles.

En ce qui concerne l'épaisseur du revêtement, le procédé selon l'invention permet de mesurer des épaisseurs allant de 0,001 à 0,1 μm. Appareil selon l'inventionWith regard to the thickness of the coating, the method according to the invention makes it possible to measure thicknesses ranging from 0.001 to 0.1 μm. Apparatus according to the invention

L'appareil selon l'invention est illustré sur la figure 1. Il comprend au moins : une source 1 de rayonnement ultraviolet ; un premier guide optique 2, qui dirige le rayonnement ultraviolet émis par ladite source de rayonnement ultraviolet vers le substrat 11 (rayonnement incident) ; un second guide optique 4 qui capte et dirige le rayonnement réfléchi vers des moyens 5, de préférence électroniques, de détection et de traitement du rayonnement réfléchi en vue de déterminer l'épaisseur du revêtement. O 2004/065902The apparatus according to the invention is illustrated in FIG. 1. It comprises at least: a source 1 of ultraviolet radiation; a first optical guide 2, which directs the ultraviolet radiation emitted by said source of ultraviolet radiation towards the substrate 11 (incident radiation); a second optical guide 4 which collects and directs the reflected radiation towards means 5, preferably electronic, for detecting and processing the reflected radiation in order to determine the thickness of the coating. O 2004/065902

7 Comme source de rayonnement ultraviolet, on peut utiliser toute source de rayonnement ultraviolet. A titre d'exemple, on peut citer une lampe à UV.7 As a source of ultraviolet radiation, any source of ultraviolet radiation can be used. By way of example, there may be mentioned a UV lamp.

De préférence, il s'agit d'une source de rayonnement ultraviolet non polarisé.Preferably, it is a source of non-polarized ultraviolet radiation.

La puissance du rayonnement est généralement de 50 à 250 Watts, mais ce n'est pas limitatif.The power of the radiation is generally from 50 to 250 Watts, but this is not limiting.

Avantageusement, les rayonnements incident et réfléchi sont perpendiculaires (ou du moins le plus perpendiculaires possible) à la surface du substrat où le rayonnement est absorbé. Dans ce cas, les premier et second guides optiques 2,4 sont sensiblement coaxiaux ou bien sensiblement parallèles. Ceci signifie qu'ils envoient et reçoivent des faisceaux lumineux (respectivement émis et reçu) , qui sont sensiblement parallèles l'un à l'autre.Advantageously, the incident and reflected radiation are perpendicular (or at least as perpendicular as possible) to the surface of the substrate where the radiation is absorbed. In this case, the first and second optical guides 2,4 are substantially coaxial or else substantially parallel. This means that they send and receive light beams (respectively emitted and received), which are substantially parallel to each other.

Les moyens de détection et de traitement du rayonnement réfléchi, de préférence électroniques, peuvent comprendre un photomultiplicateur 6 relié à une carte d'acquisition 7 elle- même reliée à un ordinateur 8. L'épaisseur du revêtement peut être déterminée par ces moyens de détection et de traitement du rayonnement réfléchi, de préférence électroniques, en particulier l'ordinateur, par comparaison avec une courbe de calibration préétablie se trouvant dans la mémoire de l'ordinateur. Selon un mode de réalisation préféré de l'invention, l'appareil comprend en outre un filtre passe-bande 9 installé à la sortie de la source de rayonnement ultraviolet 1 et/ou un second filtre passe-bande 10 installé à l'entrée du photomultiplicateur 6. Ce mode de réalisation préféré présente l'avantage d'être indifférent à la lumière ambiante environnante qui, ainsi, ne perturbe pas les mesures effectuées .The means for detecting and processing the reflected radiation, preferably electronic, may comprise a photomultiplier 6 connected to an acquisition card 7 itself connected to a computer 8. The thickness of the coating can be determined by these detection means and for processing the reflected radiation, preferably electronic, in particular the computer, by comparison with a preset calibration curve located in the memory of the computer. According to a preferred embodiment of the invention, the apparatus further comprises a bandpass filter 9 installed at the outlet of the ultraviolet radiation source 1 and / or a second bandpass filter 10 installed at the inlet of the photomultiplier 6. This preferred embodiment has the advantage of being indifferent to the surrounding ambient light which, thus, does not disturb the measurements made.

Ce ou ces filtres passe-bande 9,10 sont centrés sur une longueur d'onde comprise de préférence entre 310 et 350 nm, avantageusement centrée sur environ 330 nm.This or these band-pass filters 9, 10 are centered on a wavelength preferably between 310 and 350 nm, advantageously centered on about 330 nm.

Le premier et le second guides optiques 2,4 sont généralement placés à une distance allant de quelques O 2004/065902The first and second optical guides 2,4 are generally placed at a distance ranging from a few O 2004/065902

8 millimètres à quelques centimètres du substrat portant le revêtement dont l'épaisseur doit être mesurée.8 millimeters to a few centimeters from the substrate carrying the coating, the thickness of which must be measured.

L'épaisseur des couches d'oxyde peut être exprimée en CTUThe thickness of the oxide layers can be expressed in CTU

(Coating Thickness Unit, en français : unité d'épaisseur de revêtement) . Dans le domaine technique des revêtements du verre, il est habituel de considérer que 1 CTU correspond environ à une épaisseur de 0,25 nm pour des revêtements à base de Sn02 ou de Ti02.(Coating Thickness Unit, in French: coating thickness unit). In the technical field of glass coatings, it is usual to consider that 1 CTU corresponds approximately to a thickness of 0.25 nm for coatings based on Sn0 2 or Ti0 2 .

L'appareil selon l'invention peut avantageusement être utilisé dans une ligne de production en continu de bouteilles en verre 11 pourvues d'un revêtement.The apparatus according to the invention can advantageously be used in a continuous production line for glass bottles 11 provided with a coating.

L'appareil selon l'invention peut aussi être utilisé en tant qu'appareil de contrôle pour étudier l'homogénéité des revêtements en couche mince sur une bouteille. Pour ce faire, il suffit, par exemple, soit de déplacer la sonde (c'est-à- dire les deux guides optiques) le long d'une génératrice de la bouteille (figure 11) , soit de disposer plusieurs sondes le long d'une génératrice (figure 12), ce qui permet de contrôler simultanément plusieurs zones de la bouteille.The apparatus according to the invention can also be used as a control apparatus for studying the homogeneity of thin layer coatings on a bottle. To do this, it suffices, for example, either to move the probe (that is to say the two optical guides) along a generator of the bottle (Figure 11), or to have several probes along 'a generator (Figure 12), which allows to simultaneously control several areas of the bottle.

ExemplesExamples

Les exemples suivants sont destinés à illustrer la présente invention sans toutefois en limiter la portée.The following examples are intended to illustrate the present invention without however limiting its scope.

Exemple 1Example 1

Influence de la nature de 1 ' oxyde déposé sur le verreInfluence of the nature of the oxide deposited on the glass

A l'aide de l'appareil illustré sur la figure 1 muni d'une sonde co-axiale à fibres optiques de 400 μm de diamètre, on a soumis à des mesures d'épaisseur une série de plaquettes en verre revêtues de Sn02 et de Ti0 de diverses épaisseursUsing the apparatus illustrated in FIG. 1 fitted with a coaxial fiber optic probe 400 μm in diameter, a series of glass plates coated with Sn0 2 and of Ti0 of various thicknesses

(mesurées précédemment à l'aide de l'appareil HECM de l'art antérieur précité) . La sonde se trouvait à environ 4 mm de la surface du verre.(previously measured using the above-mentioned prior art HECM device). The probe was about 4 mm from the surface of the glass.

Les résultats sont illustrés sur les figures 2 et 3 qui montrent les valeurs du signal obtenu par la sonde UN (en mV) en fonction de l'épaisseur des couches d'oxyde exprimée en CTU. O 2004/065902The results are illustrated in FIGS. 2 and 3 which show the values of the signal obtained by the UN probe (in mV) as a function of the thickness of the oxide layers expressed in CTU. O 2004/065902

Dans les deux cas on constate une bonne linéarité de la réponse du capteur UV 3 (en fonction de l'épaisseur en CTU) .In both cases there is a good linearity of the response of the UV sensor 3 (depending on the thickness in CTU).

Exemple 2Example 2

Influence de la couleur du verreInfluence of glass color

A l'aide du montage utilisé dans l'exemple 1, on a mesuré les épaisseurs des revêtements de Sn02 déposés sur une bouteille de couleur verte et une bouteille de couleur marron, en utilisant comme référence les mêmes bouteilles (verte et marron) non revêtues . La sonde se trouvait à environ 4 mm de la surface de la bouteille. Les résultats figurent dans le tableau suivant :Using the assembly used in Example 1, the thicknesses of the coatings of Sn0 2 deposited on a green bottle and a brown bottle were measured, using the same bottles (green and brown) not as reference. coated. The probe was about 4 mm from the surface of the bottle. The results are shown in the following table:

Figure imgf000011_0001
Figure imgf000011_0001

On constate que dans les deux cas, la couche de 80 CTU apporte une augmentation du signal de 50% par rapport à la bouteille non revêtue.It can be seen that in both cases, the 80 CTU layer provides a 50% increase in signal compared to the uncoated bottle.

En outre, on observe que la couleur du verre n'influe pas sur le résultat de la mesure.In addition, it is observed that the color of the glass does not influence the result of the measurement.

Exemple 3Example 3

Influence de la présence d'une couche organique sur la couche d' oxydeInfluence of the presence of an organic layer on the oxide layer

A l'aide du montage utilisé dans l'exemple 1, on a mesuré les épaisseurs de divers revêtements déposés sur des bouteilles en verre : couche de Sn0 seule, couche organique lubrifiante (à base de cires de polyéthylène) seuleUsing the assembly used in Example 1, the thicknesses of various coatings deposited on glass bottles were measured: layer of Sn0 alone, organic lubricating layer (based on polyethylene waxes) alone.

(d'épaisseur de l'ordre de 1 μm) , couche de Sn02 + couche organique lubrifiante. La sonde se trouvait à environ 4 mm de la surface de la bouteille.(thickness of the order of 1 μm), layer of Sn0 2 + organic lubricating layer. The probe was about 4 mm from the surface of the bottle.

Les résultats sont représentés sur le graphique de la figure 4. O 2004/065902The results are shown in the graph in Figure 4. O 2004/065902

1010

On peut constater que la couche lubrifiante n'altère pratiquement pas la mesure de l'épaisseur de la couche d'oxyde d'étain. Ceci constitue un des avantages de cet appareil par rapport aux autres techniques de mesure des épaisseurs des couches minces citées plus haut.It can be seen that the lubricating layer practically does not alter the measurement of the thickness of the tin oxide layer. This constitutes one of the advantages of this device compared to the other techniques for measuring the thicknesses of the thin layers mentioned above.

Exemple 4Example 4

Sensibilité à l'épaisseur du revêtementCoating thickness sensitivity

Dans cet exemple, on a utilisé le montage illustré sur la figure 1, en employant une sonde avec 2 guides de lumière parallèles de 4 mm de diamètre, qui ont l'avantage d'être beaucoup plus sensibles que les fibres de 400 μm de diamètre. On a soumis à des mesures d'épaisseur des plaques de verre revêtues de Sn02, disposées à 20 cm de la sonde. Les résultats sont représentés sur la figure 5.In this example, the assembly illustrated in FIG. 1 has been used, using a probe with 2 parallel light guides of 4 mm in diameter, which have the advantage of being much more sensitive than the fibers of 400 μm in diameter. . Glass plates coated with SnO 2 , placed 20 cm from the probe, were subjected to thickness measurements. The results are shown in Figure 5.

La courbe de calibration de la figure 5 permet de déterminer la sensibilité de la sonde à l'épaisseur du revêtement de Sn02. Dans la configuration d'essai du présent exemple, la sensibilité est de l'ordre de 29 mV/CTU.The calibration curve in FIG. 5 makes it possible to determine the sensitivity of the probe to the thickness of the coating of Sn0 2 . In the test configuration of the present example, the sensitivity is of the order of 29 mV / CTU.

Exemple 5Example 5

Détermination de 1 ' épaisseur du revêtement en Sn02 sur une bouteille de verreDetermination of the thickness of the coating in Sn02 on a glass bottle

A l'aide du montage utilisé dans l'exemple 4, on a mesuré l'épaisseur d'un revêtement de Sn02 de 50 CTU sur une bouteille de verre de 1 litre, en comparaison avec la même bouteille non revêtue. Pour faire cet essai, on a fait défiler les bouteilles devant la sonde. La distance minimale sonde/bouteille était de 20 cm. Les résultats sont représentés sur la figure 6, sur laquelle, pour représenter les résultats obtenus, on a décalé l'origine des abscisses pour la bouteille non revêtue, de manière à faciliter la comparaison des deux courbes.Using the assembly used in Example 4, the thickness of a coating of SnO 2 of 50 CTU was measured on a 1 liter glass bottle, in comparison with the same uncoated bottle. To do this test, the bottles were scrolled in front of the probe. The minimum probe / bottle distance was 20 cm. The results are shown in FIG. 6, in which, to represent the results obtained, the origin of the abscissas for the uncoated bottle has been shifted, so as to facilitate the comparison of the two curves.

A partir de ces résultats, on peut déterminer la sensibilité à environ 23 mV/CTU. O 2004/065902From these results, sensitivity can be determined at around 23 mV / CTU. O 2004/065902

11 Exemple 6 Influence de la distance sonde/surface du verre11 Example 6 Influence of the probe / surface distance of the glass

A l'aide du montage utilisé dans l'exemple 4, on a fait des mesures sur des plaques revêtues de Sn02 à 25, 58 et 75 CTU et on a fait varier la distance sonde/surface de verre.Using the assembly used in Example 4, measurements were made on plates coated with SnO 2 at 25, 58 and 75 CTU and the distance between probe and glass surface was varied.

Les résultats sont représentés sur le graphique de la figure 7.The results are shown in the graph in Figure 7.

On constate que, dans le domaine exploré, la réponse de la sonde UV est quasiment linéaire en fonction de la distance avec une pente d'environ 260 mV/cm, quelle que soit l'épaisseur du revêtement.It can be seen that, in the area explored, the response of the UV probe is almost linear as a function of the distance with a slope of approximately 260 mV / cm, whatever the thickness of the coating.

Exemple 7Example 7

Influence de la température A l'aide du montage utilisé dans l'exemple 4, on a fait des mesures sur des bouteilles de 1 litre préalablement chauffées à différentes températures et placées à 20 cm de la sonde.Influence of the temperature Using the assembly used in Example 4, measurements were made on 1 liter bottles previously heated to different temperatures and placed 20 cm from the probe.

Le graphique de la figure 8 montre les résultats comparatifs d'une bouteille revêtue de 50 CTU de Sn02 et d'une bouteille non revêtue, dans la plage de température allant de la température ambiante à 180°C.The graph in Figure 8 shows the comparative results of a bottle coated with 50 CTU of Sn0 2 and an uncoated bottle, in the temperature range from room temperature to 180 ° C.

On peut constater que la température n'a quasiment pas d'influence sur les mesures.We can see that the temperature has almost no influence on the measurements.

Exemple 8Example 8

Comparaison appareil HECM / appareil selon l'inventionComparison of HECM device / device according to the invention

Afin de comparer les résultats donnés par l'appareil HECM de la société AGR précité avec ceux donnés par l'appareil selon l'invention, on a placé la sonde UV de l'appareil selon l'invention (suivant le montage décrit dans l'exemple 1) à environ 12 mm d'une bouteille placée sur le plateau tournant de l'appareil HECM, comme illustré sur la figure 9.In order to compare the results given by the HECM device of the aforementioned company AGR with those given by the device according to the invention, the UV probe of the device according to the invention was placed (according to the assembly described in the example 1) about 12 mm from a bottle placed on the turntable of the HECM device, as illustrated in Figure 9.

Le graphique de la figure 10 montre les signaux obtenus par les deux sondes lorsque l'on fait tourner la bouteille. L'échelle des abscisses représente la position angulaire et l'échelle des ordonnées correspond aux valeurs (calibrées) de CTU de l'appareil HECM (courbe en pointillés). Les valeurs données par la sonde UV sont calibrées par rapport aux valeurs CTU pour le point d'abscisse 0, et, donc, exprimées aussi en CTU (courbe continue) .The graph in Figure 10 shows the signals obtained by the two probes when the bottle is rotated. The abscissa scale represents the angular position and the ordinate scale corresponds to the (calibrated) CTU values of the HECM device (dotted curve). Values data by the UV probe are calibrated against the C TU values for the abscissa point 0, and, therefore, also expressed in CTU ( continuous curve).

On observe une excellente corrélation entre les deux courbes . There is an excellent correlation between the two curves.

Claims

O 2004/06590213 REVENDICATIONS O 2004/06590213 CLAIMS 1. Procédé pour la mesure sans contact de l'épaisseur d'un revêtement de substrat (11) , comprenant au moins les étapes suivantes : on envoie un rayonnement ultraviolet sur ledit substrat (11) ; on capte le rayonnement réfléchi ; et on traite le rayonnement réfléchi en vue de déterminer l'épaisseur du revêtement de substrat (11).1. A method for non-contact measurement of the thickness of a substrate coating (11), comprising at least the following steps: an ultraviolet radiation is sent on said substrate (11); the reflected radiation is captured; and processing the reflected radiation to determine the thickness of the substrate coating (11). 2. Procédé selon la revendication 1, caractérisé en ce que le rayonnement ultraviolet incident est non-polarisé .2. Method according to claim 1, characterized in that the incident ultraviolet radiation is non-polarized. 3. Procédé selon la revendication 1 ou la revendication 2, caractérisé en ce que le rayonnement incident et le rayonnement réfléchi sont sensiblement perpendiculaires au substrat (11) et sont parallèles.3. Method according to claim 1 or claim 2, characterized in that the incident radiation and the reflected radiation are substantially perpendicular to the substrate (11) and are parallel. 4. Procédé selon l'une- des revendications 1 à 3, caractérisé en ce que le rayonnement ultraviolet incident présente une longueur d'onde comprise entre 280 et 400 nm, de préférence comprise entre 300 et 350 nm, et en particulier d'environ 330 nm.4. Method according to one of claims 1 to 3, characterized in that the incident ultraviolet radiation has a wavelength between 280 and 400 nm, preferably between 300 and 350 nm, and in particular approximately 330 nm. 5. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que le substrat (11) est une bouteille.5. Method according to one of claims 1 to 4, characterized in that the substrate (11) is a bottle. 6. Procédé selon l'une des revendications 1 à 4, caractérisé en ce que le substrat est un article plat.6. Method according to one of claims 1 to 4, characterized in that the substrate is a flat article. 7. Appareil pour la mesure sans contact de l'épaisseur d'un revêtement de substrat (11) , comprenant au moins : une source (1) de rayonnement ultraviolet ; - un premier guide optique (2) qui dirige le rayonnement ultraviolet émis par ladite source (1) de rayonnement ultraviolet vers le substrat (11) ; un second guide optique (4) qui capte et dirige le rayonnement réfléchi vers des moyens (5) de détection et de traitement du rayonnement réfléchi en vue de déterminer l'épaisseur du revêtement .7. Apparatus for non-contact measurement of the thickness of a substrate coating (11), comprising at least: a source (1) of ultraviolet radiation; - a first optical guide (2) which directs the ultraviolet radiation emitted by said source (1) of ultraviolet radiation towards the substrate (11); a second optical guide (4) which collects and directs the reflected radiation towards means (5) for detecting and processing the reflected radiation in order to determine the thickness of the coating. 8. Appareil selon la revendication 7, caractérisé en ce que la source (1) de rayonnement ultraviolet est une source de rayonnement ultraviolet non-polarisé.8. Apparatus according to claim 7, characterized in that the source (1) of ultraviolet radiation is a source of non-polarized ultraviolet radiation. 9. Appareil selon la revendication 7 ou 8, caractérisé en ce que les premier et second guides optiques (2,4) sont sensiblement coaxiaux.9. Apparatus according to claim 7 or 8, characterized in that the first and second optical guides (2,4) are substantially coaxial. 10. Appareil selon l'une des revendications 7 ou 8, caractérisé en ce que les premier et second guides optiques (2,4) sont sensiblement parallèles.10. Apparatus according to one of claims 7 or 8, characterized in that the first and second optical guides (2,4) are substantially parallel. 11. Appareil selon l'une des revendications 7 à 10, caractérisé en ce que les moyens de détection et de traitement11. Apparatus according to one of claims 7 to 10, characterized in that the detection and processing means (5) sont des moyens électroniques.(5) are electronic means. 12. Appareil selon l'une des revendications 7 à 11, caractérisé en ce que les moyens de détection et de traitement (5) comprennent un photomultiplicateur (6) relié à une carte d'acquisition (7) elle-même reliée à un ordinateur (8) .12. Apparatus according to one of claims 7 to 11, characterized in that the detection and processing means (5) comprise a photomultiplier (6) connected to an acquisition card (7) itself connected to a computer (8). 13. Appareil selon l'une des revendications 7 à 12, caractérisé en ce qu'il comprend en outre un filtre passe- bande (9) installé à la sortie de la source de rayonnement ultraviolet et/ou un second filtre passe-bande (10) installé à l'entrée du photomultiplicateur (6).13. Apparatus according to one of claims 7 to 12, characterized in that it further comprises a bandpass filter (9) installed at the outlet of the source of ultraviolet radiation and / or a second bandpass filter ( 10) installed at the entrance of the photomultiplier (6). 14. Appareil selon la revendication 13, caractérisé en ce que le ou les filtres passe-bande (9,10) sont centrés sur une longueur d'onde d'environ 330 nm. 14. Apparatus according to claim 13, characterized in that the bandpass filter (s) (9,10) are centered on a wavelength of about 330 nm. 15. Utilisation d'un appareil selon l'une des revendications 7 à 14 dans une ligne de production en continu.15. Use of an apparatus according to one of claims 7 to 14 in a continuous production line. 16. Utilisation d'un appareil selon l'une des revendications 7 à 14 en tant qu'appareil de contrôle pour étudier l'homogénéité du revêtement sur une bouteille (11) . 16. Use of an apparatus according to one of claims 7 to 14 as a control apparatus for studying the homogeneity of the coating on a bottle (11).
PCT/FR2003/003739 2002-12-20 2003-12-16 Method and apparatus for the contactless measurement of the thickness of a coating on a substrate Ceased WO2004065902A1 (en)

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FR0216318A FR2849180A1 (en) 2002-12-20 2002-12-20 Non-contact method for measuring the thickness of a coating layer on a substrate, especially a bottle, using ultraviolet radiation transmitted towards a bottle and reflected from it for detection and analysis

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