DE102013022032A1 - Method for detecting foreign substances or degradation products in encapsulated systems and its use - Google Patents
Method for detecting foreign substances or degradation products in encapsulated systems and its use Download PDFInfo
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- DE102013022032A1 DE102013022032A1 DE102013022032.7A DE102013022032A DE102013022032A1 DE 102013022032 A1 DE102013022032 A1 DE 102013022032A1 DE 102013022032 A DE102013022032 A DE 102013022032A DE 102013022032 A1 DE102013022032 A1 DE 102013022032A1
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- foreign substances
- degradation products
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- encapsulated systems
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- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
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- 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
- G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
- G01M3/22—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material for pipes, cables or tubes; for pipe joints or seals; for valves; for welds; for containers, e.g. radiators
- G01M3/226—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material for pipes, cables or tubes; for pipe joints or seals; for valves; for welds; for containers, e.g. radiators for containers, e.g. radiators
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/7769—Measurement method of reaction-produced change in sensor
- G01N2021/7786—Fluorescence
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- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Plasma & Fusion (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating, Analyzing Materials By Fluorescence Or Luminescence (AREA)
Abstract
Mit der vorliegenden Erfindung soll ein Verfahren für den besonders empfindlichen Nachweis des Eindringens kleinster Mengen von Fremdstoffen, wie z. B. Wasser oder Sauerstoff, in verkapselte Systeme zum einen, und zum anderen der Entstehung von Degradationsprodukten innerhalb von verkapselten Systemen bereitgestellt werden. Erfindungsgemäß wird in die verkapselten Systeme zumindest eine Indikatorsubstanz eingebracht und anschließend wird die durch die Fremdstoffe oder Degradationsprodukte bewirkte Änderung der Photolumineszenz der Indikatorsubstanz gemessen.The present invention is a method for the particularly sensitive detection of the penetration of minute amounts of foreign substances such. As water or oxygen, in encapsulated systems on the one hand, and on the other, the emergence of Degradationsprodukten be provided within encapsulated systems. According to the invention, at least one indicator substance is introduced into the encapsulated systems and subsequently the change in the photoluminescence of the indicator substance caused by the foreign substances or degradation products is measured.
Description
Die vorliegende Erfindung beschreibt ein Verfahren für den besonders empfindlichen Nachweis des Eindringens kleinster Mengen von Fremdstoffen, wie z. B. Wasser oder Sauerstoff, in verkapselte Systeme zum einen, und zum anderen der Entstehung von Degradationsprodukten innerhalb von verkapselten Systemen.The present invention describes a method for the particularly sensitive detection of the penetration of minute amounts of foreign substances, such. As water or oxygen, in encapsulated systems on the one hand, and on the other the emergence of Degradationsprodukten within encapsulated systems.
Zum Nachweis kleinster Mengen von z. B. eingedrungenen Fremdstoffen in verkapselte Systeme ist spezielle Messtechnik erforderlich. Für die Bestimmung der Sauerstoff- bzw. Wasserdampf-Durchgangsrate durch Hochbarrierefolien ist z. B. ein Nachweis von Sauerstoff bzw. Wasser nötig. Stand der Technik ist hier die Messung mittels Radionuklidmethoden (
Eine ortsaufgelöste Messung mit der erforderlichen Empfindlichkeit unter bauteilüblichen Umgebungsbedingungen oder auch direkt in z. B. organischen Bauelementen bei Normaldruck in einer beliebigen Umgebung mit natürlichem Wasserdampf und Sauerstoff ist mit keiner der oben genannten Messmethoden möglich.A spatially resolved measurement with the required sensitivity under component ambient conditions or directly in z. B. organic components at atmospheric pressure in any environment with natural water vapor and oxygen is not possible with any of the above measurement methods.
Aus dem Stand der Technik sind zum ortsaufgelösten Nachweis von auftretenden Lecks auf Fluoreszenz basierende Leck-Detektoren (
Aufgabe der vorliegenden Erfindung ist es deshalb, die Nachteile aus dem Stand der Technik zu überwinden und ein kontaktloses Verfahren zum qualitativen und quantitativen Nachweis von Fremdstoffen, wie z. B. Wasser und Sauerstoff, die in verkapselte Systeme eingedrungen sind, wobei insbesondere der Eindringungsort der Fremdstoffe ermittelt werden soll, um Schwachstellen in der Verkapselung nachzuweisen. Außerdem soll mit der vorliegenden Erfindung auch der Nachweis von Degradationsprodukten in verkapselten Systemen realisiert werden, die nicht von außen in die Probe eingedrungen, sondern innerhalb der Probe – aber unter Umständen auch durch von außen eingedrungene Substanzen – entstanden sind.Object of the present invention is therefore to overcome the disadvantages of the prior art and a non-contact method for the qualitative and quantitative detection of foreign substances, such. As water and oxygen, which have penetrated into encapsulated systems, in particular, the penetration of the foreign substances to be determined in order to detect weak points in the encapsulation. In addition to the present invention, the detection of degradation products in encapsulated systems to be realized, which did not penetrate from the outside into the sample, but within the sample - but possibly also by externally penetrated substances - have arisen.
Erfindungsgemäß gelingt die Lösung dieser Aufgabe mit den Merkmalen des ersten Patentanspruches. Weitere vorteilhafte Ausgestaltungen des erfindungsgemäßen Verfahrens sind in den Unteransprüchen angegeben.According to the invention, the solution of this problem succeeds with the features of the first claim. Further advantageous embodiments of the method according to the invention are specified in the subclaims.
Mit dem erfindungsgemäßen Verfahren können Fremdstoffe, insbesondere auch Gase und Flüssigkeiten, in verkapselten Systemen, wie z. B. organischen Bauelementen, qualitativ und quantitativ kontaktlos nachgewiesen werden. Dafür werden reaktive Materialien als Indikatoren in das zu untersuchende verkapselte System eingebracht. Diese reaktiven Indikatormaterialien zeigen im Ursprungszustand entweder eine Photolumineszenz, welche durch Kontakt oder Reaktion mit nachzuweisenden, gegebenenfalls eindringenden Substanzen ausgelöscht wird oder keine Photolumineszenz, welche durch Kontakt oder Reaktion mit nachzuweisenden, gegebenenfalls eindringenden Substanzen erst ermöglicht wird. Die Materialeigenschaft der Photolumineszenz wird somit für eine kontaktlose Messung ausgenutzt.With the method according to the invention, foreign substances, in particular gases and liquids, in encapsulated systems, such as. As organic components, qualitatively and quantitatively be detected contactless. For this purpose, reactive materials are introduced as indicators into the encapsulated system to be investigated. These reactive indicator materials in the original state either a photoluminescence, which is extinguished by contact or reaction with detectable, optionally penetrating substances or no photoluminescence, which is made possible by contact or reaction with detectable, optionally penetrating substances. The material property of the photoluminescence is thus utilized for contactless measurement.
Zum Nachweis von Fremdstoffen bzw. Degradationsprodukten werden reaktive Indikatorsubstanzen explizit mit in die zu untersuchende Probe eingebracht. Proben in diesem Sinne können verkapselte Bauelemente oder Bauteile, komplexere Geräte oder auch verpackte Nahrungsmittel oder Medikamente sein, aber nicht ausschließlich. Unter der Bedingung, dass die zu untersuchende Probe mindestens eine wenigstens semitransparente Seite oder Oberfläche besitzt, können mittels einer Photolumineszenzmessung Fremdstoffe oder Degradationsprodukte im Inneren dieser Probe unter verschiedenen Test- bzw. Stressbedingungen nachgewiesen werden.For the detection of foreign substances or degradation products reactive indicator substances are explicitly introduced into the sample to be examined. Samples in this sense can be, but are not limited to, encapsulated devices or components, more complex devices, or packaged foods or medicines. Under the condition that the sample to be examined has at least one at least semitransparent side or surface, by means of a Photoluminescence Measurement Foreign substances or degradation products are detected inside this sample under different test or stress conditions.
Entstehen im Probeninneren Degradationsprodukte oder gelangen in das Innere der präparierten Probe Fremdstoffe, wird dies erfindungsgemäß durch Änderung des Emissionsspektrums bzw. der Emissionsintensität des Indikators kontaktlos gemessen. Die Beobachtung der Zunahme, Abnahme, Verschiebung oder mehrerer Änderungen zugleich des Emissionsspektrums z. B. mittels Photolumineszenz ermöglicht eine sehr hohe Auflösung, da gegebenenfalls zum vollständigen Auslöschen der lokalen Photolumineszenz bereits wenige Volumenprozent an Anregungslöschern oder -aktivierern ausreichen können. Dabei ist eine Verwendung mehrerer, in ihren Reaktionspartnern und Änderungen der optischen Eigenschaften unterschiedlicher, Indikatoren für den Nachweis unterschiedlicher Fremdstoffe oder Degradationsprodukte generell möglich, so dass diese gleichzeitig beobachtet und unterschieden werden können.If degradation products occur in the interior of the sample or if foreign substances enter the interior of the prepared sample, this is measured according to the invention by changing the emission spectrum or the emission intensity of the indicator without contact. The observation of the increase, decrease, shift or several changes at the same time the emission spectrum z. B. by means of photoluminescence allows a very high resolution, as may already be sufficient to completely extinguish the local photoluminescence already a few volume percent of excitation extinguishers or activators. In this case, a use of several, in their reactants and changes in the optical properties of different indicators for the detection of different foreign substances or degradation products is generally possible, so that they can be observed and distinguished simultaneously.
Mit dem erfindungsgemäßen Verfahren ist der Nachweis von Reaktionsprodukten innerhalb einer Probe, die z. B. bei der Aushärtung von Klebern oder bei der Degradation der zur Probe gehörenden Stoffe frei werden, durch eine kontaktlose optische Messung möglich. Voraussetzung für die Durchführung des erfindungsgemäßen Verfahrens jedoch ist, dass die Probe an der Seite oder Oberfläche, an der die Indikatorsubstanzen eingebracht werden, zumindest semitransparent ist. Werden in einer bevorzugten Ausführungsform des erfindungsgemäßen Verfahrens die Indikatorsubstanzen in der Probenverkapselung eingeschlossen, kann damit die gesamte Verkapselung einschließlich Probe und Versiegelung evaluiert wird.With the method according to the invention, the detection of reaction products within a sample, the z. B. in the curing of adhesives or in the degradation of the sample belonging substances are free, possible by a non-contact optical measurement. However, a prerequisite for carrying out the method according to the invention is that the sample is at least semitransparent on the side or surface on which the indicator substances are introduced. If the indicator substances are included in the sample encapsulation in a preferred embodiment of the method according to the invention, the entire encapsulation, including the sample and the seal, can be evaluated.
Bestandteil einer bevorzugten Ausführungsform des erfindungsgemäßen Mess- und Nachweisverfahrens ist die bildgebende Charakterisierung mittels einer hochempfindlichen Kamera, welche die Photolumineszenz über mehrere Größenordnungen der Intensität hinweg beobachten kann. Als Anregungslichtquelle wird vorzugsweise monochromatisches Licht verwendet. Durch die Nutzung bildgebender Verfahren zur Beobachtung der Photolumineszenzveränderungen können Fremdstoffe oder Degradationsprodukte lokal im verkapselten System nachgewiesen werden und damit insbesondere lokale Defekte in Barrierefolien oder Verkapselungen oder lokale Degradationserscheinungen beobachtet und somit besser verstanden werden. Dies ermöglicht die Suche von Schwachstellen im Bauelementaufbau oder in der Verpackung von z. B. Nahrungsmitteln, und erlaubt somit gezielte Verbesserungen im Produktaufbau bzw. im Fertigungsprozess oder auch die Bestimmung von Ausfallursachen oder die Überschreitung von Haltbarkeiten. Durch das Einbringen der Indikatorsubstanzen in die Probe ist im Allgemeinen eine Beeinflussung auf dessen Funktion oder der Lebensmittelechtheit auszuschließen. Weiterhin können bestehende Bauteilkomponenten, wie z. B. fluoreszierende Klebesysteme, als Indikator genutzt werden oder Indikatoren in diese integriert werden, um z. B. speziell eine Randversiegelung zu untersuchen.Part of a preferred embodiment of the measurement and detection method according to the invention is the imaging characterization by means of a high-sensitivity camera, which can observe the photoluminescence over several orders of magnitude of intensity. The excitation light source used is preferably monochromatic light. By using imaging techniques to monitor the changes in photoluminescence, foreign substances or degradation products can be detected locally in the encapsulated system and thus, in particular, local defects in barrier films or encapsulations or local degradation phenomena can be observed and thus better understood. This allows the search of vulnerabilities in the component structure or in the packaging of z. As food, and thus allows targeted improvements in product design or in the manufacturing process or even the determination of failure causes or the exceeding of shelf life. By introducing the indicator substances into the sample, it is generally possible to rule out any influence on its function or foodstuff authenticity. Furthermore, existing component components, such. As fluorescent adhesive systems, are used as an indicator or indicators are integrated into these z. B. specifically to investigate an edge seal.
Das erfindungsgemäße Messverfahren stellt eine Methode zur Produktüberwachung dar und erlaubt so zum einen den Produktionsprozess (auch während der Fertigung) zu überwachen oder Tests zur beschleunigten Alterung bzw. Untersuchung von Reklamationsfällen bzw. Schadensfällen durch eine einzige kontaktlose Messung ohne mechanische Arbeiten durchzuführen. Ebenso führt die mit dieser Erfindung einhergehende Vereinfachung im Messaufbau auch zu einer Erhöhung der pro Zeiteinheit zu untersuchenden Proben.The measurement method according to the invention represents a method for product monitoring and thus allows on the one hand to monitor the production process (also during production) or to carry out tests for accelerated aging or investigation of complaints or damage cases by a single contactless measurement without mechanical work. Likewise, the simplification in the measurement setup associated with this invention also leads to an increase in the samples to be examined per unit of time.
ZITATE ENTHALTEN IN DER BESCHREIBUNG QUOTES INCLUDE IN THE DESCRIPTION
Diese Liste der vom Anmelder aufgeführten Dokumente wurde automatisiert erzeugt und ist ausschließlich zur besseren Information des Lesers aufgenommen. Die Liste ist nicht Bestandteil der deutschen Patent- bzw. Gebrauchsmusteranmeldung. Das DPMA übernimmt keinerlei Haftung für etwaige Fehler oder Auslassungen.This list of the documents listed by the applicant has been generated automatically and is included solely for the better information of the reader. The list is not part of the German patent or utility model application. The DPMA assumes no liability for any errors or omissions.
Zitierte PatentliteraturCited patent literature
- US 6909088 B2 [0002] US 6909088 B2 [0002]
- CN 102175624 [0002] CN 102175624 [0002]
- CN 102445438 [0002] CN 102445438 [0002]
- JP 03-248039 A [0002] JP 03-248039 A [0002]
- JP 2003-075282 A [0002] JP 2003-075282 A [0002]
- US 6993956 B2 [0002] US 6993956 B2 [0002]
- JP 2007-101228 A [0004] JP 2007-101228 A [0004]
- JP 2011-185757 A [0004] JP 2011-185757 A [0004]
Zitierte Nicht-PatentliteraturCited non-patent literature
- Dunkel et al. Proc. IEEE, vol. 93, pp. 1478–1482, Aug. 2005 [0002] Dark et al. Proc. IEEE, vol. 93, pp. 1478-1482, Aug. 2005 [0002]
Claims (5)
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DE102013022032.7A DE102013022032A1 (en) | 2013-12-19 | 2013-12-19 | Method for detecting foreign substances or degradation products in encapsulated systems and its use |
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DE102013022032.7A DE102013022032A1 (en) | 2013-12-19 | 2013-12-19 | Method for detecting foreign substances or degradation products in encapsulated systems and its use |
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