Kai Brune

A detailed experimental study of the effects of pre-bond contamination with a hydraulic fluid, thermal degradation, and poor curing on fracture toughness of composite-bonded joints

Adhesive bonding is applied by the aircraft industry both for assembling composite structural parts and implementing composite patch repairs in damaged structural parts. In both applications, there exist several scenarios, related to surface contamination and processing, that could affect bonding quality and thus, degrade bond strength. In this paper, the detailed effects of pre-bond contamination with a hydraulic fluid, thermal degradation of the composite substrate, as well as poor curing (lower curing temperature) on strength of composite-bonded joints were studied experimentally by conducting mode I fracture toughness tests on double-cantilever beam specimens. These three application scenarios are possible to appear in the implementation of a composite patch repair in a damaged composite structural part. The experimental results showed a contradictory effect as the presence of the hydraulic fluid and poor curing degrades the fracture toughness whereas thermal degradation enhances fracture toughness of the composite-bonded joints. These findings are explained by means of extended non-destructive inspection, surface analysis, and evaluation of fracture surfaces.

Quality assurance concepts for adhesive bonding of composite aircraft structures – characterisation of adherent surfaces by extended NDT

In order to ensure the performance of adhesively joined load-critical composite structures, suitable technologies are needed to steadily monitor adherent surfaces prior to bonding and to detect adhesion properties of bonded components. A novel class of non-destructive testing (NDT) techniques, classified as extended non-destructive testing (ENDT), is required to ascertain selected physicochemical properties which are important for the performance of adhesive bonds in place of detecting material defects like conventional NDT methods do. The European FP7 project, ‘ENCOMB – Extended non-destructive testing of composite bonds’ aims in the identification, development, adaptation and validation of ENDT methods for characterisation of adherent surfaces and adhesive bond quality. Here, recent NDT techniques such as optically stimulated electron emission (OSEE) and aerosol wetting test (AWT) as well as laser-induced breakdown spectroscopy (LIBS) were advanced and applied in field, and without contacting carbon fibre-reinforced polymer (CFRP) surfaces for detecting different contamination layers such as release agent, moisture or hydraulic oil as well as thermal degradation of CFRP adherent surfaces before performing an adhesive bonding process. Sensitivity and accuracy of these techniques allow distinguishing surface states which are suitable for bonding of CFRP adherents from surface states which are unfavourable for bonding. ENDT using OSEE, AWT and LIBS facilitated the detection of layers of release agent as thin as one nanometre and thin layers resulting from hydraulic oil. OSEE investigations of adherent surfaces before adhesive bonding allowed the indication of all surface states of potential CFRP adherents, which according to previous studies, were related to application scenarios reducing the joint strength of resulting adhesive joints by 20–70%.

Surface analytical approaches contributing to quality assurance during manufacture of functional interfaces

Assessing adhesion or strength of composites or adhesive joints in a non-destructive way is highly challenging. Therefore, instead of performing retrospective quality assurance, i.e. investigating manufactured joints, it is advantageous to safeguard performance and quality of each layer and each interface already during manufacture. This approach still is challenging, as it requires a systematic quantitative evaluation of threshold criteria, but appreciably it gets more and more feasible. We present approaches for an inline-capable and non-destructive quality assurance of steps in manufacturing processes used for tailoring the state of substrate surfaces. Benefits from applying techniques for inline surface analysis like Optically Stimulated Electron Emission (OSEE) and Aerosol Wetting Test (AWT) will be detailed. The performed procedures contribute to a novel class of non-destructive testing (NDT) techniques, classified as Extended NDT (ENDT). The principle of ENDT methods is based on the detection of selected physico-chemical properties which are important for the anticipated performance of the functional interfaces in the products to be manufactured.A prerequisite for obtaining reliable composite materials is to reproducibly prepare a suitable surface state of the substrates before the first step of a coating or bonding process. As demonstrative application scenarios, we highlight first an exemplary surface pretreatment process for steel substrates, and second the identification of a surface state for carbon fiber reinforced polymer (CFRP) adherents suitable for joining. Concerning steel substrates we investigated two types of steel both in the as-received state and a state after grinding. We demonstrate that the removal of the topmost material layer comprising the reaction layer and mechanically deformed metal grains strongly affects the properties of the resulting adherent surface. As a consequence, a material-specific time slot for a steel substrate exposure in air after grinding is suggested in which the surface properties probed by OSEE remain unchanged. Moreover, we work out that the sensitivity and accuracy of inline-capable NDT techniques allow distinguishing surface states suitable for bonding of CFRP adherents from surface states unfavourable for adhesive bonding, and we exemplarily verify this statement for bonding processes applying freshly ground CFRP or, respectively, CFRP covered with thin layers of release agents.

Qualität prozessintergiert sichern

In Hochtechnologiebereichen zählt das Kleben zu den bevorzugt eingesetzten Fügetechniken. Allerdings gilt es nach DIN EN ISO 9001 als „spezieller Prozess“, dessen Ergebnis nicht umfassend zerstörungsfrei geprüft werden kann. Um eine qualitativ hochwertige Klebverbindung gewährleisten zu können, müssen deshalb alle erforderlichen Prozessschritte ausreichend überwacht und dokumentiert werden beginnend mit der Entwicklung einer Klebverbindung bis hin zum fertigen Produkt. Ein gutes Beispiel für die Entwicklung eines Qualitätssicherungskonzeptes ist der Schienenfahrzeugbau seit der Einführung der DIN 6701 im Jahre 2007. Dabei werden die Qualitätsstandards klebtechnischer Anwenderbetriebe festgelegt, Konstruktionsvorgaben gemacht sowie Ausführungsregeln und die Qualitätssicherung von Klebprozessen festgeschrieben [1]. Schwerpunkt ist hier die Qualifikation der am Prozess beteiligten Mitarbeiter [2]. Um nun die Qualitätsanforderungen auch für andere Anwendungsgebiete in der klebtechnischen Fertigung festzulegen, wird die DIN 2304 eingeführt. Sie legt die Anforderungen für die qualitätsgerechte Ausführung von Klebverbindungen entlang der Prozesskette Kleben von der Entwicklung über die Instandhaltung fest und deckt zwei Anwendungsbereiche ab. Der erste Teil erläutert allgemeine organisatorische, vertragliche und fertigungstechnische Grundlagen für die Herstellung klebtechnischer Verbindungen mit der Hauptfunktion einer Übertragung mechanischer Lasten. Sein Inhalt bezieht sich auf alle Klebstoffklassen, Werkstoffkombinationen und Branchen. Der zweite Teil legt spezielle Anforderungen an die klebtechnische Ausführung für Materialien aus Faserverbundkunststoffen fest. In der DIN 2304 werden die Klebungen hier in Sicherheitsklassen unterteilt, wobei der verantwortliche Konstrukteur bzw. Bauteilverantwortliche die Einstufung vornehmen muss [3].

Optical Riblet Sensor: Beam Parameter Requirements for the Probing Laser Source.

Beam parameters of a probing laser source in an optical riblet sensor are studied by considering the high demands on a sensors’ precision and reliability for the determination of deviations of the geometrical shape of a riblet. Mandatory requirements, such as minimum intensity and light polarization, are obtained by means of detailed inspection of the optical response of the riblet using ray and wave optics; the impact of wavelength is studied. Novel measures for analyzing the riblet shape without the necessity of a measurement with a reference sample are derived; reference values for an ideal riblet structure obtained with the optical riblet sensor are given. The application of a low-cost, frequency-doubled Nd:YVO4 laser pointer sufficient to serve as a reliable laser source in an appropriate optical riblet sensor is discussed.

Study of CFRP adhesive bonds influenced by factors encountered during aircraft operations

Composite materials are commonly used in many branches of industry. One of the effective methods to join CFRP parts is to use adhesives. There is a search of effective methods for quality assurance of bonded parts. There is a need for pre- and post-bond inspection to ensure proper bonding and verify its quality. Research reported here focuses on post-bond inspection of bonded CFRP parts. In this paper we report investigations of samples that were modified in order to simulate the conditions that can be encountered during the bonding repair processes. The modifications were made before adhesive bonding, and their effect on the quality of the bond is studied. The first case was the thermal treatment. It was made by exposure of samples to elevated temperatures. This case accounts for parts that may be exposed to external heat source or lightening impact. Second of the investigated cases was deicing fluid contamination prepared by dip-coating of clean CFRP plates. When cleaning the aircraft for a repair this fluid can be transported to bonding areas and weaken the joint. The third type of modification was faulty curing of the adhesive. It was prepared by local pre-curing of the adhesive. Pre-curing causes irregularities in the curing of the adhesive joint. Apart from single modifications, also mixed cases were studied, as well as scarf bonding. The samples were studied in non-destructive approach. It was shown that for some of the cases the detection is possible.

Study of CFRP adhesive bonds influenced by manufacturing-related contaminations

Composite materials are commonly used in many branches of industry. One of the effective methods to join CFRP parts is the adhesive bonding. There is a search of effective methods for quality assurance of bonded parts. There is a need for pre- and post-bond inspection to ensure proper bonding and verify its quality. Research reported here focuses on post-bond inspection of bonded CFRP parts. In this paper we report investigations of samples that were modified with contamination that can be encountered during the manufacturing process of the CFRP parts. The contaminations were introduced before adhesive bonding, and the effect of the contamination on the quality bond is studied. First of the investigated cases was release agent contamination prepared by dip-coating of clean CFRP plates. The release agent is used during the production of composite elements and can contaminate the surface to be bonded. The second case was the moisture contamination. It was obtained by conditioning of the samples in humid conditions. Moisture contamination can be gained from water-coupled ultrasonics or during transportation of unprotected parts. The third type of contamination had more local character. It simulated fingerprints. Artificial sweat was used. The fingerprint contamination can be caused by improper handling of the parts. Apart from single contamination, also mixed contamination cases were studied, as well as curved samples. The samples were studied in non-destructive approach. It was shown that for some of the cases the detection is possible.

Assured Use of Release Agents and Adhesives in the Same Production Process

Structural components made of CFK have proved most effective in motor sport. The implementation of lightweight concepts for all road vehicles using composite materials is possible by intelligent design and the management of reliable joining methods. The use of adhesive bonding processes in the car manufacturing industry is paving the way here, with organisational matters regulated by standards and advanced methods for extended quality assurance testing in the production.

Interfactant action of an amphiphilic polymer upon directing graphene oxide layer formation on sapphire substrates

Quality assured surface pre-treatment may greatly enhance adhesive interactions and, thus, the performance and durability of material joints. This holds true as well for substrates used in coating processes as for adherents introduced into bonding processes. Wettable polymeric wetting agents—shortly called polymeric interfactants—contribute to modifying surfaces and governing the properties of interphases. This is demonstrated for amphiphilic polymers directing the adsorption of graphene oxide (GO) nano-sheets from aqueous dispersion on alumina surfaces. In this contribution, contact angle measurements as well as X-ray photoelectron spectroscopy and scanning force microscopy investigations are applied for the characterization of thin films. GO is adsorbed either from a buffered dispersion on pristine aluminum oxide surfaces or on alumina modified with a few nanometers thin layer of a polymeric interfactant. Laterally extended nanoparticles and GO nano-sheets are preferentially found on interfactant layers whereas on pristine aluminum oxide smaller adsorbates dominate. The driving forces directing the GO attachment are discussed using a phenomenological model based on polymer/substrate interactions governing the sticking probabilities of GO nano-sheets with different sizes.

Nondestructive testing of contaminated CFRP surfaces with the BonNDTinspect® system

Composite materials are already being used in the mass production of structural components in the automotive industry, particularly at the BMW Group. Adhesive bonding is generally considered to be the best technique for joining CFRP (carbon fiber reinforced plastic) light-weight structures. The conventional NDT (nondestructive testing) methods currently being used focus on the detection of material defects, e.g. debonding. These methods give little information about the surface properties or bond quality. A new ENDT (extended nondestructive testing) method is the BonNDTinspect system, based on a patent held by the Fraunhofer IFAM. An ultrasonic atomizer nozzle creates a water-aerosol and the small water droplets are sprayed onto the surface. Depending on the surface properties (surface energy or contamination state), the aerosol will form wide or narrow drops on the surface. We determined a test for certain contaminations, including release agents, oil, and fingerprints, the detection of which is critical to ensure the performance of adhesively joined CFRP structures. The BonNDTinspect system is an inline-capable NDT technique that is suitable for distinguishing surface states for adhesive bonding of CFRP. We verify this statement with destructive tests, including the single-lap shear test. It was found by using an extension of the evaluation criteria that it is possible to detect contamination such as water-soluble release agent, CFRP dust and fingerprints. The investigated contamination with hydraulic oil allows only a clear differentiation between cleaned and contaminated. A contamination with corundum is not detectable by the BonNDTinspect system alone.