EP2409128A1 - Indicateur pour détecter la pénétration d'air et/ou d'humidité dans un emballage sous vide, sous pression ou sous gaz protecteur - Google Patents

Indicateur pour détecter la pénétration d'air et/ou d'humidité dans un emballage sous vide, sous pression ou sous gaz protecteur

Info

Publication number
EP2409128A1
EP2409128A1 EP10719528A EP10719528A EP2409128A1 EP 2409128 A1 EP2409128 A1 EP 2409128A1 EP 10719528 A EP10719528 A EP 10719528A EP 10719528 A EP10719528 A EP 10719528A EP 2409128 A1 EP2409128 A1 EP 2409128A1
Authority
EP
European Patent Office
Prior art keywords
indicator
vacuum
vacuum insulation
pressure
air
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Withdrawn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
EP10719528A
Other languages
German (de)
English (en)
Inventor
Hans-Frieder Eberhardt
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.)
Porextherm-Dammstoffe GmbH
Porextherm Daemmstoffe GmbH
Original Assignee
Porextherm-Dammstoffe GmbH
Porextherm Daemmstoffe GmbH
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 Porextherm-Dammstoffe GmbH, Porextherm Daemmstoffe GmbH filed Critical Porextherm-Dammstoffe GmbH
Publication of EP2409128A1 publication Critical patent/EP2409128A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
    • G01M3/042—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point by using materials which expand, contract, disintegrate, or decompose in contact with a fluid
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
    • G01M3/042—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point by using materials which expand, contract, disintegrate, or decompose in contact with a fluid
    • G01M3/045—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point by using materials which expand, contract, disintegrate, or decompose in contact with a fluid with electrical detection means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
    • G01M3/16—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using electric detection means
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators

Definitions

  • Indicator for detecting the ingress of air and / or moisture into a vacuum, pressure or protective gas packaging
  • the invention relates to an indicator for detecting the penetration of air and / or moisture in a vacuum, pressure or inert gas packaging with the preamble features of claim 1.
  • Vacuum packaging and protective gas packaging are used, for example, to protect dry food from spoilage.
  • industrial goods that are to be further processed, for example, in clean environments, for the transport and storage of dust and moisture exposure are protected.
  • the packaging can also prevent moisture and oxygen from entering transported or stored sensitive chemicals.
  • VIP vacuum insulation panels
  • Another branch of application has developed at the same time the reduced thermal conductivity of evacuated solids such.
  • B. in vacuum insulation panels (VIP) exploits. These vacuum insulation panels are used i.a. used in refrigerators and freezers as well as for the thermal insulation of buildings.
  • the insulating core or support body of the vacuum insulation panel consists for example of a nano- or microporous material such.
  • Synthetic silica precipitated silica, fumed silica and / or aerogels, open celled polyurethane foam, open celled polystyrene foam, open celled polyisocyanurate foam, perlites or fiber materials, or mixtures and combinations of these materials.
  • the vacuum insulation panel is formed with a small percolation cross-section and has a mechanical constriction of the heat conduction by gas diffusion to the Knudsen portion, which occurs at geometrical dimensions smaller than the mean free path of the gas molecules.
  • the packaging of the vacuum insulation panel is preferably formed by flexible, all-round welded films, which closely conform to the space-giving support body.
  • multilayer films with metal films or metallized plastic layers are usually used as diffusion barriers, which stably close internal vacua by less than 5 mbar and ensure a functional life of the vacuum insulation panels of up to ten and more years.
  • the thermal conductivity of the support body and the residual gas remaining in the technical vacuum determine the quality of the resulting thermal insulation.
  • the vacuum inside the vacuum insulation panel may be caused by very fine (micro) holes, for example, due to defects in film production, by permeation of gases through the heat seal, and by openings due to mechanical failure Violation of the films or the finished vacuum insulation panel in the production, transport and installation of the vacuum insulation panel at the point of use, be affected.
  • micro holes for example, due to defects in film production, by permeation of gases through the heat seal, and by openings due to mechanical failure
  • Violation of the films or the finished vacuum insulation panel in the production, transport and installation of the vacuum insulation panel at the point of use be affected.
  • it is very easy to detect massive damage to the foil wrapping since the loosening of the foils around the supporting bodies is noticeable visually and haptically.
  • the problem is the finest holes, which lead to a very slow increase in pressure inside the vacuum insulation panels. This pressure increase can often not be noticed over the periods between production / storage and delivery.
  • the heat flow is influenced by the gas pressure-dependent thermal conductivity in an open-pore material (for example a fiber mat) lying between the cladding film and the inner metal plate.
  • an open-pore material for example a fiber mat
  • the required measurement structures are poorly suited, for example, at delivery and handover at a construction site a 100% Testing the vacuum insulation panels to perform.
  • a series-installed switch can interrupt the circuit consisting of the coil and the transponder chip, this state being detected from the outside by means of the recognition / non-recognition of the transponder signal by the reader. From the transponder response can be concluded whether the vacuum insulation panel is vented or still evacuated.
  • a disadvantage of this method is the complex design
  • Another method for controlling the internal gas pressure of a vacuum insulation panel is to place the vacuum insulation panel in a vacuum chamber and to evacuate it until the cover sheet of the vacuum insulation panel noticeably lifts from the support body.
  • the internal pressure in the panel just greater than that
  • PVDF highly polarized polyvinyl fluoride
  • DE 101 17 021 A1 proposes a vacuum insulation panel with a pressure measuring device, which comprises a pressure measuring chamber with a movable piston whose volume is variable depending on the pressure prevailing inside the vacuum insulation panel.
  • a disadvantage is in addition to the complex design of the pressure measuring chamber, the fact that the pressure measuring chamber itself can form a thermal bridge and thus reduces the insulation performance of the Vakuumisoiationpaneei.
  • the film envelope of the vacuum insulation panel must be at least locally formed of a transparent material. This results in requirements for the design and positioning of the film wrapping, which can significantly increase the manufacturing time and cost of the vacuum insulation panel.
  • a disadvantage of the said systems is therefore that the sensors used to increase the cost of vacuum insulation panels considerably and require a comprehensive diagnostic technique. Also, some of the techniques do not permit accurate analysis of the state of the vacuum insulation panel in the installed state.
  • the indicator is particularly suitable for use in a vacuum insulation panel, since the quality of the applied vacuum is of particular relevance to the insulation performance. It is provided that the penetrating air and / or the moisture penetrating with the air causes a change in the physical properties of the indicator.
  • the indicator is characterized in that this one with the penetrating air and / or humidity
  • the indicator according to the invention is based on the knowledge that the quality of the vacuum in vacuum packaging or vacuum insulation panels should not be measured per se, but instead only one air quality.
  • the indicator is the unique determination of the condition of the appropriately equipped packaging or vacuum insulation panel.
  • the running chemical reaction is irreversible, so that the operation of the indicator is comparable to a 155 burning fuse.
  • the indicator according to the invention can also be used in protective gas packaging, in which case a component of the incoming air / moisture is detected, which is not present in the protective gas in the interior.
  • the components of oxygen or moisture can be used as an indicator of an air leak. Both components are chemically reactive and can easily cause a chemical reaction on a sensitive element, which is preferably in a color change or in the change of an electrically measurable size, for example, the change of
  • the chemically reactive material is formed as a barium layer and has a defined dielectric constant.
  • the barium layer reacts with penetrating moisture and is converted to barium oxide, whereas under the influence of penetrating CO 2 a conversion to barium carbonate
  • Each conversion reaction involves a measurable change in the electrical properties of the layer and associated changes in measurable quantities.
  • the barium layer is part of a remote-quereable system, such as an RF transponder and accompanied by the ongoing chemical reaction, a change in the response of the transponder. In both cases, from the
  • the invention also includes a vacuum, pressure or protective gas packaging and in particular a vacuum insulation panel with evacuated heat insulation body, the one
  • the vacuum, pressure or protective gas packaging according to the invention in particular vacuum insulation panel, comprises the aforementioned indicator or preferred embodiments thereof.
  • a vacuum or compressed gas packaging In connection with a color change as a result of the chemical reaction is a vacuum or compressed gas packaging and in particular
  • the electrical parameters of the indicator can be passively read in an electromagnetic circuit, alternatively, the indicators can also be combined with RFID technology, the indicator preferably as an RF transponder with variable electric
  • the RF transponder is formed with sensor input and / or microcontroller. Furthermore, it is considered favorable if the transmission frequency of the RF transponder is variable by the chemical reaction.
  • the presented indicator for vacuum packaging, inert gas packaging and / or vacuum insulation panels uses a chemical reaction to easily detect a vacuum intrusion and associates this with an optical or electronic readout of the indicator state. In addition to the opportunity to easily examine the indicator revealed
  • the indicator according to the invention advantageously comprises a material with a thin layer, which is modified under the action of components of the air / moisture so that their optical or electrical properties change. This can, in addition to the discoloration also a measurable change in the resistance of the layer between two
  • the changed parameters at the sensor input of an RFID by threshold value switching can be transmitted digitally or as an analog signal.
  • a preferred embodiment of the indicator provides as an indicator material before a thin Metaüfiirn which is oxidizable by Sauerstoffeinvvirkung and whose conductivity or Resistance changes depending on the degree of oxidation.
  • the metal film of aluminum or the so-called. Valve metals tantalum, niobium, manganese, titanium, bismuth, antimony, zinc, cadmium, tin and iron and magnesium, copper or nickel formed, which
  • the metal film 230 be oxidized by penetrating into the packaging / sheath oxygen or moisture.
  • the metal film is applied between two contact electrodes, which ensure the connection to the read-out resonant circuit or to an RF transponder.
  • For the design of the metal film is its optimized Schichtdicken- and morphology choice in terms of tolerated production and introduction process in the packaging
  • Oxide formation on closed metal layers with prolonged exposure to air oxygen plus possible moisture components slows down, for the thickness of the metal film the equivalent thickness of a natural oxide film is the desired value. This results according to the time integral of the exposure time times pressure-dependent oxidation depth.
  • the actual indicator reaction in the event of air ingress can also be mediated by the substrate on which the metal films can be applied.
  • the indicator is preferably at least partially made of diffusible substrates such.
  • Overcome substrate barrier made of PE or PET and oxidize the inward facing part of the not yet oxidized metal layer.
  • the above applies analogously to the oxygen and moisture partial pressures.
  • the increase in electrical resistance is optimal for this detection reaction when, after double-sided oxidation, no conductive
  • the interior of the meta-perfume is left over. As a result of the substrate thickness, the response of the indicator can be adjusted.
  • Another preferred embodiment of the indicator uses a PET film, for example 22 ⁇ m thick, on the connections through shadow masks
  • 275 copper are deposited in the thickness less ⁇ m and subsequently a thinner
  • Aluminum film for example, with a thickness of 12 nm, per sensor is applied. These films are then further processed, for example, for the reasons mentioned above either continuously in a glove box or after nitrogen inlet into the vacuum chamber within a few seconds in the lock of oxygen and moisture-free
  • the indicators Oscillating or RF transponder electrically connected and these indicator units airtight packaged in glove box atmosphere.
  • the indicators can be stored and also in packaging, vacuum insulation panels or inert gas packaging, which are prepared for evacuation or gas filling, are introduced.
  • the indicator package
  • 285 may be designed so that it automatically opens during the evacuation of the packaging or the vacuum insulation panel by its internal pressure and releases the indicator contained for monitoring the packaging or the vacuum insulation panel.
  • the required small thickness of the metal films makes high demands on the planarity of the 290 substrates used. Their roughness ensures inhomogeneities of the metal film and
  • the material used is thin films of organic semiconductors which change their conductivity upon exposure to oxygen.
  • Suitable 300 materials for this purpose are polypyrrole, polyaniline and polythiophenes such.
  • a suitable arrangement results here, when the vertical reaction profile is placed in the material in the horizontal, resulting in significantly enlarged diffusion paths, which also fits the comparatively higher diffusibility of polymers.
  • a horizontal diffusion profile results if the polymer film additionally with a difficult diffusible
  • This protective layer is coated, whereby horizontally running concentration profiles are enforced.
  • This protective layer may, for example, again be a metal or else a thickly applied (or calendered) polymer having low diffusibility, such as EVOH 1 PA or COC.
  • the Umschiag Vietnamese the in ⁇ ' ikatorantwort is placed in this way on the time at which the last, horizontally inner region of high resistance to atmospheric oxygen
  • cover layer described above is formed as a counterelectrode, a capacitive arrangement results:
  • the materials introduced here can change mechanically, which is achieved, for example, by the swelling of hydrogels when moisture is absorbed. Alternatively, materials such as plasma polymers which alter their moisture permittivity with moisture uptake may also be used. In this
  • Figure 1 is a equipped with a preferred embodiment of the indicator according to the invention support body of a vacuum insulation panel.
  • Fig. 1a and 1 b shows enlarged sections of the metal film of the inventive 325 indicator of FIG. 1;
  • FIG. 2 shows a supporting body of a vacuum insulation panel equipped with a further embodiment of the indicator according to the invention
  • FIG. 3 shows a supporting body of a vacuum insulation panel equipped with a third embodiment of the indicator according to the invention
  • FIG. 3a shows enlarged sections of the protective layer of the invention
  • Fig. 1 shows a support body 11 of a vacuum insulation panel 10 before insertion into a film wrapping (not shown).
  • the vacuum insulation panel 10 is provided with an indicator 20
  • the indicator 20 has in the embodiment of a thin metal film 21 made of aluminum, wherein the metal film 21 of course from the valve metals tantalum, niobium, manganese, titanium, bismuth, antimony, zinc, cadmium, tin and iron and magnesium, copper or nickel formed can be.
  • the metal film 21 is oxidized.
  • the meta-fu 21 is between two Ko ⁇ taktelektroden 22nd applied, via which a connection can be made to a read-out resonant circuit or to an RF transponder.
  • the metal film 21 is only a few nanometers thick and applied to an additional substrate layer 24. Through the thickness of the metal film 21 becomes the electrical starting point and the values that can be detected with the later
  • the indicator 20 can also be integrated into the substrate layer 24.
  • the substrate layer 24 is then formed as a diffusible polymer film with low water absorption.
  • the delayed transfer of gases through the substrate layer 24 is referred to as
  • 355 is used for the loss of the vacuum inside the vacuum insulation panel 10 to be installed.
  • the response of the indicator 20 can thus be adjusted via the thickness of the substrate layer 24.
  • the small thickness of the metal film 21 places high demands on the planarity of the 360 substrate layer 24. Roughness of the substrate layer 24 causes inhomogeneities in the metal film 21 and resulting joints 25, such as in Figs. 1a and 1b partially enlarged for individual metal clusters of the metal film 21 are shown. The inhomogeneities and even more the joints 25 oxidize faster than homogeneous portions of the metal film 21, but still slower than the directly exposed surfaces. The delay of the 365 oxidation at the junctions 25 may alter the response of the indicator 20 and ultimately falsify the measurement result so that the substrate layer 24 should possibly be planar.
  • FIG. 2 shows a further preferred embodiment of the indicator 20, 370 according to the invention, which in turn has been applied to the support body 11 of a vacuum insulation panel 10.
  • the indicator 20 here consists of a designed as a thin film 26 organic semiconductor, which changes its conductivity when exposed to oxygen.
  • the material chosen here is polypyrrole, with polyaniline and polythiophenes such as polyhexylthiopene being equally suitable as a material.
  • the oxygen content of the penetrating air in the case of 375 pure materials usually leads to a reduction in resistance. This is to be considered in the construction of the indicator 20 because the choking effect in the depth of the thin film 26 is eliminated.
  • an arrangement which is more suitable for the intended purpose of detection results if the vertical reaction pro! of the thin film 26 is bent into the horizontal, causing itself give significantly enlarged diffusion paths. This also fits the comparatively higher
  • a suitable horizontal diffusion profile results when the thin film 26 is coated with a hard diffusible protective layer 27, thereby enforcing horizontally extending concentration profiles.
  • This protective layer 27 may, for example, again be a metal or else a thickly applied (or calendered) polymer with low diffusivity such as EVOH, PA or COC.
  • FIG. 3 shows a further embodiment of the indicator 20, wherein the protective layer 26 is designed as a counterelectrode and thus creates a capacitive arrangement.
  • the additional layer 28 introduced between the protective layer 27 and the thin film 26 in the exemplary embodiment of FIG. 3 can change mechanically if it is present
  • the intermediate layer 28 consists of a plasma polymer, which has its dielectric constant with moisture absorption

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Molecular Biology (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Biochemistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Biophysics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Investigating Or Analyzing Materials By The Use Of Electric Means (AREA)
  • Packages (AREA)

Abstract

L'invention porte sur un indicateur simple (20) pour détecter la pénétration d'air et/ou d'humidité dans un récipient sous vide, sous pression ou sous gaz protecteur, en particulier dans un panneau d'isolation sous vide (10), l'air et/ou l'humidité qui pénètre provoquant une modification des propriétés physiques de l'indicateur (20). Il est prévu que l'indicateur (20) comporte un matériau subissant une réaction chimique avec l'air et/ou l'humidité entrants, et qu'au moins une propriété physique de l'indicateur (20) varie sous l'effet de la réaction chimique. En particulier, le matériau se présente sous forme de couche de baryum à constante diélectrique définie. En outre, il est proposé un emballage correspondant, sous vide, sous pression ou sous gaz protecteur, en particulier pour un panneau d'isolation sous vide (10) comportant un corps calorifuge dans lequel le vide a été fait et une enveloppe, métallisée d'une manière pratiquement imperméable, ladite enveloppe ayant cependant subi une variation, pour permettre la détection des propriétés physiques. Ladite enveloppe se trouve dans la zone de l'indicateur (20) masquée par un masque transparent et est recouverte d'un matériau transparent imperméable à l'air.
EP10719528A 2009-03-17 2010-03-17 Indicateur pour détecter la pénétration d'air et/ou d'humidité dans un emballage sous vide, sous pression ou sous gaz protecteur Withdrawn EP2409128A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE200920003677 DE202009003677U1 (de) 2009-03-17 2009-03-17 Indikator zum Nachweis des Eindringens von Luft- und/oder Feuchte in eine Vakuum-, Druck- oder Schutzgasverpackung
PCT/EP2010/001670 WO2010105811A1 (fr) 2009-03-17 2010-03-17 Indicateur pour détecter la pénétration d'air et/ou d'humidité dans un emballage sous vide, sous pression ou sous gaz protecteur

Publications (1)

Publication Number Publication Date
EP2409128A1 true EP2409128A1 (fr) 2012-01-25

Family

ID=42134329

Family Applications (1)

Application Number Title Priority Date Filing Date
EP10719528A Withdrawn EP2409128A1 (fr) 2009-03-17 2010-03-17 Indicateur pour détecter la pénétration d'air et/ou d'humidité dans un emballage sous vide, sous pression ou sous gaz protecteur

Country Status (3)

Country Link
EP (1) EP2409128A1 (fr)
DE (1) DE202009003677U1 (fr)
WO (1) WO2010105811A1 (fr)

Families Citing this family (5)

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EP2810039A4 (fr) * 2012-02-03 2015-09-09 Caralon Global Ltd Systèmes de contrôle de qualité de panneaux d'isolation sous vide et procédés les utilisant
EP2671708B1 (fr) * 2012-06-08 2017-02-01 Airbus Operations GmbH Procédé et système de détection de fuite dans une mise en sachet sous vide
SG11201807642XA (en) * 2016-03-29 2018-10-30 Basf Se Transport container with remote surveillance capability
DE102017001865A1 (de) * 2017-03-01 2018-09-06 Va-Q-Tec Ag Verfahren zur Überprüfung der Funktionstüchtigkeit der Wärmeisolation eines Transportbehälters
US20240027385A1 (en) * 2022-07-18 2024-01-25 Temptime Corporation Capacitance-based humidity and gas sensing rfid tags

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Also Published As

Publication number Publication date
WO2010105811A1 (fr) 2010-09-23
DE202009003677U1 (de) 2010-04-29

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