EP1738137A1 - Instrument pour mesurer l'epaisseur d'un revetement sur des bouteilles - Google Patents

Instrument pour mesurer l'epaisseur d'un revetement sur des bouteilles

Info

Publication number
EP1738137A1
EP1738137A1 EP05738995A EP05738995A EP1738137A1 EP 1738137 A1 EP1738137 A1 EP 1738137A1 EP 05738995 A EP05738995 A EP 05738995A EP 05738995 A EP05738995 A EP 05738995A EP 1738137 A1 EP1738137 A1 EP 1738137A1
Authority
EP
European Patent Office
Prior art keywords
bottle
thickness
coating
anyone
wavelengths
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.)
Withdrawn
Application number
EP05738995A
Other languages
German (de)
English (en)
Inventor
Daniel Malaise
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.)
OPO sprl
Original Assignee
OPO sprl
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 OPO sprl filed Critical OPO sprl
Publication of EP1738137A1 publication Critical patent/EP1738137A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/90—Investigating the presence of flaws or contamination in a container or its contents
    • G01N21/9081—Inspection especially designed for plastic containers, e.g. preforms
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
    • G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
    • G01B11/0616—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating
    • G01B11/0625—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating with measurement of absorption or reflection
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/59—Transmissivity
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/88—Investigating the presence of flaws or contamination
    • G01N21/90—Investigating the presence of flaws or contamination in a container or its contents
    • G01N21/9072—Investigating the presence of flaws or contamination in a container or its contents with illumination or detection from inside the container
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/84—Systems specially adapted for particular applications
    • G01N21/8422—Investigating thin films, e.g. matrix isolation method
    • G01N2021/8427—Coatings

Definitions

  • the present invention is related to a device and a method for measuring the thickness of a carbon film or a coating deposited inside or outside plastic bottles or containers .
  • the aim of this coating is to produce a barrier against the penetration of oxygen from outside and the escape of C0 2 from inside the container.
  • the instrument built according to this invention is intended to measure the local thickness of any absorbing film deposited on a substrate.
  • Plastic containers especially PET plastic containers, are commonly used for packaging liquid food and beverages.
  • the porosity of this material to common light molecules such as 0 2 and C0 2 causes problems for long term conservation of the product.
  • Another common way of addressing the problem is to flush a thin layer of material such as carbon or Si0 onto the container. Further, the most effective way of obtaining the desired tightness of the container is to deposit a carbon coating inside the bottle.
  • the final tightness depends on the thickness of the coating and on the' " regularity of its thickness .
  • One way to estimate the resulting tightness of the container is to directly measure the leak resulting from a pressurization of the container with an unwanted gas. This method is long and tedious because the leakage to be measured is very low and the unwanted gas is so common that it is difficult to separately measure the gas from the leak and the ambient gas . This is especially true for oxygen. Hence these measurements are expensive, long - several days for one bottle is not unusual- and inaccurate.
  • the present invention aims to provide an instrument intended to prevent the drawbacks of prior art.
  • the invention aims at estimating the tightness of a container by measuring the thickness of a coating deposited on the internal or external surface of the container, using a simple, non- contact, reliable, rapid and non expensive method.
  • An additional goal of the invention is to measure the thickness of said coating using optoelectronics means .
  • An additional goal of the invention is to draw a thickness surface map of the container.
  • a first object of the present invention refers to an apparatus for measuring the thickness of a coating on a container such as a bottle made of a transparent substrate, said coating being located either on the external or on the internal surface of the container, characterised in that said apparatus comprises means for simultaneously measuring light transmission of an incident source beam through essentially a same point of the container, making a test sample, at a plurality of different wavelengths, preferably at two different wavelengths .
  • the bottle receives the status "test passed" or "rejected".
  • FIG.l shows the transmission ratio for a 0.5 mm thick PET bottle covered with a 50 nm carbon coating and a reference bottle of the same thickness, for clear and dark green PET respectively.
  • FIG.2 schematically shows the principle scheme of the optical system according to the present invention.
  • FIG.3 schematically shows a preferred embodiment for a source beam combination according to the present invention.
  • FIG.4 is a perspective illustration of a preferred overall embodiment for the apparatus of the present invention.
  • FIG.5A and 5B show respective elevation and perspective views for the optomechanical part of the apparatus described in FIG.4.
  • FIG.6A and 6B show respective cross-sectional and perspective detailed views of the detection block.
  • infrared 860 or 930 nm were the most commonly used wavelengths in our system
  • a shorter wavelength we commonly used 530, 460, 410 and 370 nm
  • the instrument for measuring the carbon film must take this constraint into account by providing a variety of wavelengths in the measuring source.
  • the short wavelength source allows to measure the cumulated thickness of the substrate and of the carbon film
  • the infrared source allows to measure the substrate thickness alone.
  • the carbon thickness is computed by subtracting the substrate thickness from the total thickness .
  • Carbon coating deposition on a transparent medium can be detected and measured as far as the optical properties, namely bulk absorption, are markedly different for the substrate and for the film, provided that two wavelengths are utilised, a first wavelength in the infrared range and a second, shorter wavelength, suitably chosen according to its dependence on the colour of the substrate.
  • Both curves show the transmission ratio for a carbon coating on a PET bottle as a function of wavelength.
  • the regular curve pertains to the clear PET ; the irregular curve representing the green PET should coincide with the former one at the higher wavelengths or where there are both regular, since it reflects only the properties of the carbon layer.
  • the small but significant difference between both curves where they are regular is due to the fact that we used the external transmissions, which are affected by reflectivity, to compute the curves. With the correction for reflectivity, both curves would reach ordinate 1.00 for wavelengths longer than 800 nm.
  • FIG.l illustrates this situation for the dark green PET commonly used for bottling beer : the regions under 450 nm and between 600 and 725 nm, where the normal transmission is strongly perturbed, as shown by the continuous curve, are the spectral ranges where the green PET is essentially opaque and where no accurate measurement can be obtained.
  • FIG.2 three sources Sir 1, Sxx 2 and Ssh 3 are represented, but virtually as many sources as one wishes could be used ; in a typical preferred embodiment shown in FIG.3, five sources are used: IR (860 nm) , UV
  • Criterion #3 The various signals from the sources have to be measured individually, while they are mixed (multiplexed) on the detector. Separation of the signals can be achieved in different ways: optically, by using dichroic beam splitters in the reverse way they were used for combining the source beams ;
  • the degree of polarisation in the measuring beam be as low as possible.
  • the wall of the bottle can be considered as stretched plastic and could show some degree of birefringence.
  • the dichroic beam splitters are utilised at low incidence angle. In a preferred embodiment, this angle is set at 15° as shown in FIG.3.
  • the secondary mirrors 15 facing each lateral source (R, G, B, uv) and folding the beam towards the beam splitters 16 are aluminised and bring a minimum of polarisation. If the resulting polarisation would cause a problem in very special situations, it would be necessary to correct it by the use of a retarding plate after the collimating lens in each source (or a zero order plate in the resulting beam) .
  • the axial beam is represented horizontal.
  • the IR source is at the left, all other sources are above the parallel beam.
  • the folding aluminised mirrors 15 are at the bottom and the dichroic beam splitters 16 are crossed at 15° incidence by the axial beam. The latter exits horizontally to the right.
  • the sources are ordinary LEDs and not laser diodes because the latter usually show a large degree of polarisation and would require careful retardation of each beam separately.
  • the latter relies oh the fact that the carbon layer is transparent in the IR. This allows to measure the absorption ratio of the bottle substrate at the two wavelengths used for the measurement. This operation has to be performed for each substrate using an uncoated reference bottle.
  • the absorption ratio R can be estimated with very high accuracy. It is used for subtracting, from the measured total absorption at wavelength SH, the part due to the bottle substrate, and to take into account its thickness variations. It is important to notice that, without this, one would not be able to separate the thickness variations of the carbon layer and those of the substrate. All the bottle features would then appear as carbon features.
  • This measurement is used to characterise the optical properties of the PET. It is performed on an uncoated bottle of the same material, but not necessarily the same thickness. Its outcome is the ratio of the absorbing coefficients for the two utilised wavelength bands .
  • the (uncoated) reference bottle is measured and its transmission at the same place for both wavelengths is recorded at a certain number of "normal" points, i.e. points unaffected by letters or shape irregularities.
  • Tr SH ⁇ the internal transmission at the short wavelength SH at point i
  • Tr IR ⁇ the internal transmission IR at the same point i .
  • Each bottle made out of the same material is then measured in the two wavelengths at a number of regularly spaced points identified by their cylindrical co- ordinates ( ⁇ r h) .
  • the ratio between the average and its standard deviation E/ ⁇ E is a very sensitive criterion of the overall quality of the coating. This is because this ratio characterises the inhomogeneity of the layer, i.e. its trend at showing thinner and thicker regions, the first one being liable for leaks and the second one being useless .
  • the internal or bulk transmission is the usual transmission, i.e. the external transmission, corrected for the reflections at both faces of the wall .
  • the reflectivity coefficient is different and should be measured for each wavelength.
  • the reflectivity .coefficients of the uncoated plastic do not vary very much and average coefficients can be used without loss of accuracy.
  • the coefficients for the coated plastic vary with the thickness and the nature of the coating and with the wavelength especially if the thickness is an appreciable fraction of the wavelength. These coefficients have to be measured on a sample of coated plastic of each category. If these corrections are not applied, i.e. if all reflectivity coefficients are set to 0, the coating thickness measurement will indicate a wrong value but the relative thickness of a bottle (its thickness map) will be roughly correct. These corrective coefficients can be calibrated if one has samples of the substrate coated with known thicknesses of carbon in the range to be measured. This calibration should be performed once for all for each substrate.
  • FIG.4 showing the casing of the apparatus and on FIG.5A, 5B and 6A, 6B showing various details of the actual instrument.
  • the whole instrument is contained in two metallic cabinets 100 and 200.
  • Cabinet 100 contains all the opto-mechanical parts and the proximity electronics, while cabinet 200 contains the computer and its accessories.
  • the data acquisition card is a 8x24 bits A/D simultaneous converter clocked at 104 Kcps .
  • the opto-mechanical part inside cabinet 100 is shown in more details on FIG.5A and : 5B.
  • the cabinet 100 comprises a five-source system 20 and a light conducting tube 21 terminated by a lens and folding prism 22.
  • the mobile weight 23 whose base is shaped as a cone in order to centre the mouth of the bottle 24 when the latter is lifted in the measuring area.
  • the bottle 24 is sitting on a turntable 25, mounted on a slide mechanism 26. The latter can move the bottle upwards up to 450 mm by steps of 0.1 mm.
  • the bottle is represented in the lower position ready to start the measurements.
  • the detection block 27 is shown in more details on FIG.6A and 6B. It comprises collecting lenses 28, a detector 29 and a preamplifier board. It also comprises a rotating shutter 30 that, allows measuring a transmission comprised between 0% and 100% for calibration, for instance by steps of 25%. This calibration operation is done automatically before and after measuring each bottle.
  • the number of steps in rotation and in height is programmable.
  • the computer analyses the data in real time and yields at the end of the measurement a chart showing the map of carbon thickness and indications for bottle and process identification, parameters of the measurements and decision about the quality of the coating.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Length Measuring Devices By Optical Means (AREA)

Abstract

La présente invention a trait à un appareil et un procédé permettant de mesurer l'épaisseur de revêtement déposé à l'intérieur ou à l'extérieur d'un emballage en matière plastique par la mesure de la transmission interne à deux longueurs d'onde. Une longueur d'onde est dans la gamme d'infrarouge, c'est à dire supérieure à 750 nm, et permet la soustraction de l'absorption du substrat tandis que l'autre longueur d'onde est plus courte et choisie dans une gamme où l'absorption par le revêtement est maximale et l'absorption par le substrat est modérée.
EP05738995A 2004-04-22 2005-04-20 Instrument pour mesurer l'epaisseur d'un revetement sur des bouteilles Withdrawn EP1738137A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US56441404P 2004-04-22 2004-04-22
PCT/BE2005/000050 WO2005103605A1 (fr) 2004-04-22 2005-04-20 Instrument pour mesurer l'epaisseur d'un revetement sur des bouteilles

Publications (1)

Publication Number Publication Date
EP1738137A1 true EP1738137A1 (fr) 2007-01-03

Family

ID=34968043

Family Applications (1)

Application Number Title Priority Date Filing Date
EP05738995A Withdrawn EP1738137A1 (fr) 2004-04-22 2005-04-20 Instrument pour mesurer l'epaisseur d'un revetement sur des bouteilles

Country Status (2)

Country Link
EP (1) EP1738137A1 (fr)
WO (1) WO2005103605A1 (fr)

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FR2902514A1 (fr) * 2006-06-15 2007-12-21 Sidel Sas Procede pour controler l'epaisseur d'un revetement sur un substrat
FR2902513B1 (fr) * 2006-06-15 2008-09-19 Sidel Participations Procede pour mesurer l'epaisseur d'un revetement sur un substrat
ITMI20081439A1 (it) * 2008-08-01 2010-02-02 Maurizio Amicabile Dispositivo misuratore della permeabilita' alla luce di manufatti in materia plastica, particolarmente di preforme in polietilentereftalato e simili.
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US9458536B2 (en) 2009-07-02 2016-10-04 Sio2 Medical Products, Inc. PECVD coating methods for capped syringes, cartridges and other articles
IT1396645B1 (it) * 2009-12-03 2012-12-14 Amicabile Dispositivo misuratore della permeabilita' alla luce di manufatti in materia plastica, particolarmente di preforme in polietilentereftalato e simili.
US11624115B2 (en) 2010-05-12 2023-04-11 Sio2 Medical Products, Inc. Syringe with PECVD lubrication
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JP6095678B2 (ja) 2011-11-11 2017-03-15 エスアイオーツー・メディカル・プロダクツ・インコーポレイテッド 薬剤パッケージ用の不動態化、ｐＨ保護又は滑性皮膜、被覆プロセス及び装置
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CA2890066C (fr) 2012-11-01 2021-11-09 Sio2 Medical Products, Inc. Procedes d'inspection de revetement
EP2920567B1 (fr) 2012-11-16 2020-08-19 SiO2 Medical Products, Inc. Procédé et appareil pour détecter des caractéristiques d'intégrité de revêtement de barrière rapide
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WO2014085346A1 (fr) 2012-11-30 2014-06-05 Sio2 Medical Products, Inc. Corps creux comportant un revêtement intérieur
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Also Published As

Publication number Publication date
WO2005103605A1 (fr) 2005-11-03

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