EP1114312A1 - Method for determining the quality of adhesion in a laminar structure - Google Patents
Method for determining the quality of adhesion in a laminar structureInfo
- Publication number
- EP1114312A1 EP1114312A1 EP99947280A EP99947280A EP1114312A1 EP 1114312 A1 EP1114312 A1 EP 1114312A1 EP 99947280 A EP99947280 A EP 99947280A EP 99947280 A EP99947280 A EP 99947280A EP 1114312 A1 EP1114312 A1 EP 1114312A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- quality
- adhesion
- determining
- time
- laser pulse
- 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- Withdrawn
Links
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000002131 composite material Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000011088 calibration curve Methods 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims 1
- 230000005855 radiation Effects 0.000 claims 1
- 230000001066 destructive effect Effects 0.000 abstract description 5
- 230000002123 temporal effect Effects 0.000 abstract 1
- 239000000853 adhesive Substances 0.000 description 6
- 230000001070 adhesive effect Effects 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 230000007547 defect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 238000000275 quality assurance Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N25/00—Investigating or analyzing materials by the use of thermal means
- G01N25/72—Investigating presence of flaws
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N19/00—Investigating materials by mechanical methods
- G01N19/04—Measuring adhesive force between materials, e.g. of sealing tape, of coating
Definitions
- the invention relates to a method for determining the quality of the adhesion in a layer composite.
- Joining materials for joining dividers are increasingly being used in industry.
- the thermal contact resistance as the measure for the connection of two materials, can now be used with the new correct mathematical model (Dusza L., "Determination of Thermal Contact Resistance with Heat Loss Correction Using the Flash Method”. High Te p.-High Press ( 1995/1996), 27/28, 475 - 483).
- this requires extensive iterative calculations by solving transcendental equations up to the optimal adaptation of the calculated temperature curve to the respectively measured one.
- the object of the invention is to provide a method for determining the quality of the adhesion in a layered composite which is non-destructive and does not require any great mathematical effort.
- the thermal contact resistance is the resistance of the heat transport at an interface.
- a high thermal contact resistance means poor transmission of the heat waves, which indicates poor coupling of the two materials at the interface.
- the thermal contact resistance is accordingly inversely proportional to the adhesion.
- the method according to the invention is based on the knowledge that the thermal contact resistance is proportional to the time interval after a certain percentage of the maximum temperature is reached in the laser flash method. 50% is an optimal value for this percentage. This new non-destructive, non-contact and fast method can be used in industry to determine the adhesive strength or to control the curing or drying process in the connecting medium.
- samples with different connection properties are produced. This can be done by adding different amounts of inert materials to the layer mediating the connection or by different percentage coverage of this layer (for example 20, 40, 60, 80 and 100), the area grid being small, against the expansion of the Irradiation area by the laser.
- the "half-temperature times" of these samples are determined on the one hand and the tensile strengths on the other hand using conventional means. The calibration curve is then generated from this.
- This characteristic change in resistance enables e.g. B. the control or monitoring of a wet coating by the method.
- the thermal contact resistance of an epoxy resin adhesive drops over time. After two hours the falling trend of the determined resistance changes.
- the adhesive begins to crosslink two hours after the two components have been mixed together (information from the manufacturer). The increase in resistance after two hours indicates chemical change within the adhesive. After crosslinking is complete, the contact resistance continues to drop until the final strength is reached.
- the new method Compared to the ultrasound method, the new method not only determines the presence of the defects (as a yes No answer), but the quantitative results react to the subtle changes in the connection.
- the method of thermal contact resistance can be used in production, quality assurance and in development laboratories in areas such as Paint and varnish industry, adhesive industry, manufacturer of coating materials, automotive and aircraft industries.
- the quality of various connection technologies can also be examined, such as soldering, welding or coating with coatings (e.g. from turbines).
Landscapes
- 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)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Materials Using Thermal Means (AREA)
- Lining Or Joining Of Plastics Or The Like (AREA)
Abstract
The aim of the invention is to provide a method which is non-destructive and which is not complicated in terms of the mathematics involved. To this end, one side of the laminar structure is irradiated with a short laser pulse, the temporal temperature profile caused by the laser pulse on the other side of the laminar structure is determined and the time taken to reach a given percentage of the maximum temperature is determined, this time being a measure of the quality of adhesion.
Description
Verfahren zur Bestimmung der Qualität der Haftung in einem SchichtverbundMethod for determining the quality of the adhesion in a layer composite
Die Erfindung betrifft ein Verfahren zur Bestimmung der Qualität der Haftung in einem Schichtverbund.The invention relates to a method for determining the quality of the adhesion in a layer composite.
Verbindungswerkstoffe zum Fügen von Teiler, werden in der Industrie in zunehmendem Maß eingesetzt.Joining materials for joining dividers are increasingly being used in industry.
Die meisten praktizierten Prüfverfahren zur Bestimmung der Haftfestigkeit, wie z. B. der Zugtest sind zerstörend. Die wenigen zerstörungsfreien Methoden, wie z. B. die Ultraschalluntersuchung, liefern nur Information über die Fehlstellen, aber nicht über die Güte des Kontakts (Habenicht G., 1997, "Kleben", Springer Verlag). Beim Laserflash-Prinzip (Bräuer G., Dusza L., Schulz B.: "The New Laser Flash Equip ent LFA-427". Interceram 41 7/8, 1992.) wird dem Probekörper an der vorderen Seite kurzzeitig ein Energiepuls zugeführt und die Temperaturänderung an der Rückseite wird gemessen. Die Zeit des Temperaturanstiegs hängt in erster Linie bei homogenen Materialien von der Länge und Temperaturleitfähigkeit der Probe ab. Die Laserflash-Methode wird weltweit zur Bestimmung der Temperaturleitfähigkeit benutzt. Die Ansätze zur Bestimmung des thermischen Kontaktwiderstands mit der Laserflash-Methode waren wegen der unvollständigen mathematischen Lösung nicht erfolgreich (Balageas D.L., Krapez J.C., Cielo P., 1986, "Pulsed photothermal modeling of layered aterial", J.Appl . Phys . , 59 (2) 348 - 57).Most of the test methods used to determine the adhesive strength, such as. B. the tensile test are destructive. The few non-destructive methods, such as B. the ultrasound examination, only provide information about the defects, but not about the quality of the contact (habenicht G., 1997, "Kleben", Springer Verlag). In the laser flash principle (Bräuer G., Dusza L., Schulz B .: "The New Laser Flash Equip ent LFA-427". Interceram 41 7/8, 1992.), a short pulse of energy is supplied to the specimen on the front side and the temperature change on the back is measured. For homogeneous materials, the temperature rise time primarily depends on the length and thermal conductivity of the sample. The laser flash method is used worldwide to determine the temperature conductivity. The approaches to determining the thermal contact resistance using the laser flash method were unsuccessful because of the incomplete mathematical solution (Balageas DL, Krapez JC, Cielo P., 1986, "Pulsed photothermal modeling of layered aterial", J.Appl. Phys., 59 (2) 348-57).
Der thermische Kontakwiderstand, als das Maß für die Verbindung zweier Materialien, kann nun mit der neuen korrekten mathematischen Modell (Dusza L., "Determination of Thermal Contact Resistance with Heat Loss Correction Using the Flash Method" . High Te p.-High Press (1995/1996), 27/28, 475 - 483) bestimmt werden. Dies erfordert jedoch umfangreiche iterative Rechnungen durch Lösen von transzentendalen Gleichungen bis zur optimalen Anpassung der berechneten Temperaturkurve an die jeweils gemessene.
Aufgabe der Erfindung ist es ein Verfahren zur Bestimmung der Qualität der Haftung in einem Schichtverbund zur Verfügung zu stellen, welches zerstörungsfrei ist und ohne größeren mathematischen Aufwand auskommt.The thermal contact resistance, as the measure for the connection of two materials, can now be used with the new correct mathematical model (Dusza L., "Determination of Thermal Contact Resistance with Heat Loss Correction Using the Flash Method". High Te p.-High Press ( 1995/1996), 27/28, 475 - 483). However, this requires extensive iterative calculations by solving transcendental equations up to the optimal adaptation of the calculated temperature curve to the respectively measured one. The object of the invention is to provide a method for determining the quality of the adhesion in a layered composite which is non-destructive and does not require any great mathematical effort.
Gelöst wird diese Aufgabe durch die Merkmale des Patentanspruchs 1. Die Unteransprüche beschreiben vorteilhafte Ausgestaltungen des Verfahrens.This object is achieved by the features of patent claim 1. The subclaims describe advantageous embodiments of the method.
Der thermische Kontaktwiderstand ist der Widerstand des Wärmetransports an einer Grenzfläche. Ein hoher thermischer Kontaktwiderstand bedeutet schlechte Übertragung der Wärmewellen, was auf eine schlechte Ankopplung der zwei Materialien an der Grenzfläche hinweist. Der thermische Kontaktwiderstand ist dementsprechend umgekehrt proportional zur Adhäsion. Das erfindungsgemäße Verfahren beruht auf der Erkenntnis, daß der thermische Kontaktwiderstand proportional zu dem Zeitintervall ist, nachdem ein bestimmter Prozentsatz der maximalen Temperatur beim Laserflash-Verfahren erreicht wird. 50 % sind ein optimaler wert für diesen Prozentsatz. Dieses neue zerstörungsfreie, berührungslose und schnelle Verfahren kann in der Industrie zur Bestimmung der Haftfestigkeit, bzw. zur Kontrolle des Aushärtungs- oder des Trocknungsprozesses im verbindenden Medium eingesetzt werden.The thermal contact resistance is the resistance of the heat transport at an interface. A high thermal contact resistance means poor transmission of the heat waves, which indicates poor coupling of the two materials at the interface. The thermal contact resistance is accordingly inversely proportional to the adhesion. The method according to the invention is based on the knowledge that the thermal contact resistance is proportional to the time interval after a certain percentage of the maximum temperature is reached in the laser flash method. 50% is an optimal value for this percentage. This new non-destructive, non-contact and fast method can be used in industry to determine the adhesive strength or to control the curing or drying process in the connecting medium.
Mit Hilfe einfacher Zeitmessungen im Temperatur-Zeitdiagramm können also qualitative Aussagen über die Festigkeit von Fügeverbindungen gemacht werden.With the help of simple time measurements in the temperature-time diagram, qualitative statements about the strength of joint connections can be made.
Die Erfindung wird im folgenden näher erläutert. Nach dem Auftreffen eines kurzen Laserimpulses auf eine Probe steigt die Temperatur der Probe auf der dem Laserimpuls abgewandten Seite an, geht durch ein Maximum und fällt dann wieder ab. Dieser Temperaturverlauf wird z. B. mit einem IR-Sensor erfaßt. Die Zeit bis zum Erreichen der Hälfte der Maximaltemperatur ist ein optimaler Parameter für die Festigkeit der Fügeverbindung.
Zeiten bis zum Erreichen eines Wertes von 20 - 90 % der Maximaltemperatur sind auch als Parameter möglich.The invention is explained in more detail below. After a short laser pulse hits a sample, the temperature of the sample on the side facing away from the laser pulse rises, passes through a maximum and then drops again. This temperature curve is z. B. detected with an IR sensor. The time until half of the maximum temperature is reached is an optimal parameter for the strength of the joint connection. Times until a value of 20 - 90% of the maximum temperature is reached are also possible as parameters.
Soll die Messung quantifiziert werden, muß eine Kalibrierkurve aufgenommen werden.If the measurement is to be quantified, a calibration curve must be recorded.
Dazu werden Proben mit verschiedenen Verbindungseigenschaften hergestellt. Das kann durch unterschiedliche Mengenzugaben von inerten Materialien zu der die Verbindung vermittelnden Schicht erfolgen oder durch unterschiedliche prozentuale Flächenbedek- kung dieser Schicht (z. B. 20, 40, 60, 80 und 100 ), wobei die Flächenrasterung klein ist, gegen die Ausdehnung der Bestrahlungfläche durch den Laser. Von diesen Proben werden einerseits die "Halbtemperaturzeiten" und andererseits mit konventionellen Mitteln die Zugfestigkeiten ermittelt. Daraus wird dann die Kalibrierkurve erzeugt.For this purpose, samples with different connection properties are produced. This can be done by adding different amounts of inert materials to the layer mediating the connection or by different percentage coverage of this layer (for example 20, 40, 60, 80 and 100), the area grid being small, against the expansion of the Irradiation area by the laser. The "half-temperature times" of these samples are determined on the one hand and the tensile strengths on the other hand using conventional means. The calibration curve is then generated from this.
Für Trocknungsprozesse zeigt sich eine Zunahme des thermischen Kontaktwiderstands mit der Zeit.For drying processes, there is an increase in the thermal contact resistance over time.
Diese charakteristische Änderung des Widerstands ermöglicht z. B. die Kontrolle oder Überwachung einer feuchten Beschichtung durch das Verfahren.This characteristic change in resistance enables e.g. B. the control or monitoring of a wet coating by the method.
Der thermische Kontaktwiderstand eines Epoxid-Harz-Klebers fällt mit der Zeit ab. Nach zwei Stunden ändert sich der abfallende Trend des ermittelten Widerstandes.The thermal contact resistance of an epoxy resin adhesive drops over time. After two hours the falling trend of the determined resistance changes.
Die Vernetzung des Klebstoffes begint zwei Stunden nach dem Zusammenmischen der zwei Komponenten (Angabe des Herstellers) . Der Anstieg des Widerstands nach zwei Stunden weist auf (diese) chemische Änderung innerhalb des Klebstoffes hin. Nach abgeschlossener Vernetzung Fällt der Kontaktwiderstand weiter ab, bis zum Erreichen der Endfestigkeit.The adhesive begins to crosslink two hours after the two components have been mixed together (information from the manufacturer). The increase in resistance after two hours indicates chemical change within the adhesive. After crosslinking is complete, the contact resistance continues to drop until the final strength is reached.
Gegenüber den Ultraschall-Verfahren wird mit der neuen Methode nicht nur das Vorhandensein der Fehlstellen ermittelt (als Ja-
Nein-Antwort) , sondern die quantitativen Ergebnisse reagieren auf die feinen Änderungen in der Verbindung.Compared to the ultrasound method, the new method not only determines the presence of the defects (as a yes No answer), but the quantitative results react to the subtle changes in the connection.
Die Methode des thermischen Kontaktwiderstands kann in der Produktion, Qualitätssicherung und in den Entwicklungslabors in den Gebieten wie z.B. Farben- und Lackindustrie, KlebstoffIndustrie, Hersteller von Schichtwerkstoffen, Auto- und Flugzeugindustrie eingesetzt werden. Die Qualität von verschiedenen Verbindungstechniken kann ebenfalls untersucht werden, wie bei Löten, Schweißen oder bei der Beschichtung mit Coatings (z. B. von Turbinen) .
The method of thermal contact resistance can be used in production, quality assurance and in development laboratories in areas such as Paint and varnish industry, adhesive industry, manufacturer of coating materials, automotive and aircraft industries. The quality of various connection technologies can also be examined, such as soldering, welding or coating with coatings (e.g. from turbines).
Claims
1. Verfahren zur Bestimmung der Qualität der Haftung in einem Schichtverbund mit folgenden Verfahrensschritten: a) Bestrahlen einer Seite des Schichtverbundes mit einem kurzen Laserimpuls, b) Erfassen des zeitlichen Temperaturverlaufs, er durch __ diesen Laserimpuls verursacht wird auf der anderen Seite des Schichtverbundes und c) Bestimmen der Zeit, nach der ein bestimmter Prozentsatz der maximalen Temperatur erreicht wird, wobei diese Zeit ein Maß für die Qualität der Haftung ist.1. A method for determining the quality of the adhesion in a layered composite with the following process steps: a) irradiating one side of the layered composite with a short laser pulse, b) detecting the temperature profile over time, which is caused by __ this laser pulse on the other side of the layered composite and c ) Determining the time after which a certain percentage of the maximum temperature is reached, this time being a measure of the quality of the adhesion.
2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß der Prozentsatz der maximalen Temperatur 50% ist.2. The method according to claim 1, characterized in that the percentage of the maximum temperature is 50%.
3. Verfahren nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß der Schichtverbund aus zwei mit einander verklebten Schichten besteht.3. The method according to claim 1 or 2, characterized in that the layer composite consists of two layers bonded together.
4. Verfahren nach einem der Ansprüche 1 bis 3, dadurch gekennzeichnet, daß der Schichtverbund eine Schicht mit einseitiger Beschichtung ist.4. The method according to any one of claims 1 to 3, characterized in that the layer composite is a layer with a one-sided coating.
5. Verfahren nach einem der Ansprüche 1 bis 4, dadurch gekennzeichnet, daß durch ein geeignetes Raster von vielen Bestrah- lungs- und Meßpunkten ein flächiger Schichtverbund erfaßt wird.5. The method according to any one of claims 1 to 4, characterized in that a flat layer composite is detected by a suitable grid of many radiation and measurement points.
6. Verfahren nach einem der Ansprüche 1 bis 5, dadurch gekennzeichnet, daß die Qualität der Haftungen durch Vergleich mit einer Kalibrierkurve quantifiziert wird.
6. The method according to any one of claims 1 to 5, characterized in that the quality of the bonds is quantified by comparison with a calibration curve.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE19841969 | 1998-09-14 | ||
| DE19841969A DE19841969C1 (en) | 1998-09-14 | 1998-09-14 | Method for determining the quality of the adhesion in a layer composite |
| PCT/EP1999/006566 WO2000016079A1 (en) | 1998-09-14 | 1999-09-07 | Method for determining the quality of adhesion in a laminar structure |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP1114312A1 true EP1114312A1 (en) | 2001-07-11 |
Family
ID=7880875
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP99947280A Withdrawn EP1114312A1 (en) | 1998-09-14 | 1999-09-07 | Method for determining the quality of adhesion in a laminar structure |
Country Status (5)
| Country | Link |
|---|---|
| US (1) | US20010005392A1 (en) |
| EP (1) | EP1114312A1 (en) |
| JP (1) | JP3346558B2 (en) |
| DE (1) | DE19841969C1 (en) |
| WO (1) | WO2000016079A1 (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7690840B2 (en) * | 1999-12-22 | 2010-04-06 | Siemens Energy, Inc. | Method and apparatus for measuring on-line failure of turbine thermal barrier coatings |
| DE10013172C2 (en) * | 2000-03-17 | 2002-05-16 | Wagner Internat Ag Altstaetten | Method and device for the photothermal analysis of a material layer, in particular for measuring the layer thickness |
| WO2003008938A2 (en) * | 2001-07-16 | 2003-01-30 | Siemens Aktiengesellschaft | Method for determining the adhesiveness of a coating on a component |
| US7425093B2 (en) * | 2003-07-16 | 2008-09-16 | Cabot Corporation | Thermography test method and apparatus for bonding evaluation in sputtering targets |
| US7432505B2 (en) * | 2006-05-04 | 2008-10-07 | Siemens Power Generation, Inc. | Infrared-based method and apparatus for online detection of cracks in steam turbine components |
| DE102007051688A1 (en) * | 2007-10-26 | 2009-04-30 | BLZ Bayerisches Laserzentrum Gemeinnützige Forschungsgesellschaft mbH | Method for process monitoring when applying laser to two joining partners |
| US20100171518A1 (en) * | 2008-12-16 | 2010-07-08 | University Of New Brunswick | Method and apparatus for non-destructive detection of defects in composite laminate structures |
| EP2950085A1 (en) * | 2014-05-28 | 2015-12-02 | BAE Systems PLC | Improved structural health monitoring |
| EP3149462A1 (en) | 2014-05-28 | 2017-04-05 | BAE Systems PLC | Improved structural health monitoring |
Family Cites Families (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4126033A (en) * | 1977-06-23 | 1978-11-21 | The United States Of America As Represented By The Secretary Of The Navy | Determination of thermal conductances of bonding layers in infrared photoconductor arrays |
| FI64465C (en) * | 1982-03-15 | 1983-11-10 | Mauri Luukkala | FOERFARANDE OCH APPARAT FOER ATT MAETA YTORNAS EGENSKAPER AV FASTA TILLSTAONDETS MATERIALER |
| IT1185661B (en) * | 1984-09-04 | 1987-11-12 | Gen Electric | METHOD AND APPARATUS FOR REVALING AND CONTROL OF ADHESION OF COATINGS |
| US4928254A (en) * | 1988-04-28 | 1990-05-22 | Knudsen Arne K | Laser flash thermal conductivity apparatus and method |
| US5344236A (en) * | 1992-01-23 | 1994-09-06 | Fishman Iiya M | Method for evaluation of quality of the interface between layer and substrate |
| JP3568271B2 (en) * | 1995-03-27 | 2004-09-22 | 株式会社超高温材料研究所 | Method and apparatus for measuring thermal constant using laser flash method |
| JP3568304B2 (en) * | 1995-12-06 | 2004-09-22 | 株式会社超高温材料研究所 | Analysis method of thermal constant using laser flash method |
-
1998
- 1998-09-14 DE DE19841969A patent/DE19841969C1/en not_active Expired - Fee Related
-
1999
- 1999-09-07 JP JP2000570565A patent/JP3346558B2/en not_active Expired - Fee Related
- 1999-09-07 WO PCT/EP1999/006566 patent/WO2000016079A1/en not_active Application Discontinuation
- 1999-09-07 EP EP99947280A patent/EP1114312A1/en not_active Withdrawn
-
2001
- 2001-02-22 US US09/790,097 patent/US20010005392A1/en not_active Abandoned
Non-Patent Citations (1)
| Title |
|---|
| See references of WO0016079A1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| US20010005392A1 (en) | 2001-06-28 |
| JP3346558B2 (en) | 2002-11-18 |
| WO2000016079A1 (en) | 2000-03-23 |
| JP2002525571A (en) | 2002-08-13 |
| DE19841969C1 (en) | 2000-05-11 |
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