Analytische Chemie
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Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (1471)
- 8 Zerstörungsfreie Prüfung (1320)
- 6 Materialchemie (1065)
- 6.1 Oberflächen- und Dünnschichtanalyse (368)
- 6.3 Strukturanalytik (337)
- 8.0 Abteilungsleitung und andere (330)
- 8.2 Zerstörungsfreie Prüfmethoden für das Bauwesen (328)
- 1.1 Anorganische Spurenanalytik (291)
- 1.2 Biophotonik (269)
- 8.4 Akustische und elektromagnetische Verfahren (259)
Paper des Monats
- ja (27)
Vortragstagung "Zerstörungsfreie Materialprüfung" vom 28. bis 30. Mai 1962 in Garmisch-Partenkirchen
(1962)
Die „Gesellschaft zur Förderung Zerstörungsfreier Prüfverfahren e. V.“ und der „Unterausschuß für Zerstörungsfreie Prüfung des Werkstoffausschusses beim Verein Deutscher Eisenhüttenleute“ hatten mit Garmisch-Partenkirchen als Ort für ihre Jahrestagung eine gute Wahl getroffen. Die Aula des Gymnasiums gab den Vorträgen einen Rahmen passender Größe, und Gelegenheiten zum geselligen Beisammensein waren reichlich vorhanden; vor allem die Erinnerung an den gemeinsamen Abend im „Bauerntheater“ wird den meisten Tagungsteilnehmern noch manches Schmunzeln entlocken.
Das Vortragsprogramm enthielt in gut ausgewogener Zusammenstellung Beiträge über Grundlagen und Anwendungen verschiedener Prüfmethoden sowie Erfahrungsberichte. Daß es in mehreren Vorträgen um die Gewinnung objektiver Maßstäbe bei der Deutung von Prüfergebnissen ging, ist besonders hervorzuheben.
Leider waren erst die Exkursionen am 30. 5. nach München zur Fa. Kraus-Maffei (die Reaktorbesichtigung war kurzfristig von Garching aus abgesagt worden) und zum Walchensee-Kraftwerk mit einem Umweg über den Sylvensteinspeicher vom Wetter nicht begünstigt. Vor allem den Damen hätte man für ihr an sich sehr reizvolles Programm wenigstens etwas mehr Wärme und Sonne gewünscht.
Den Organisatoren dieser Tagung gebührt volle Anerkennung für das gelungene Programm. Den vielen Regen und die nötig gewordene Änderung der Exkursionen kann man ihnen nicht zum Vorwurf machen.
Die Prüfprobleme bei Verbundwerkstoffen sind im wesentlichen bestimmt durch die Zweckbestimmung des betreffenden Gegenstandes, die materielle und organisatorische Basis für die Verwirklichung des Vorhabens, die untersuchende und vergleichende Auswahl geeigneter Stoffe und Verarbeitungsverfahren und durch die bestätigende und deshalb meist komplexe Prüfung seiner Funktion mit vorgegebenem Leitwert und darauf bezogenen Variablen bei oft nicht als Konstanten beherrschbaren Parametern.
Die erfolgreiche Lösung einer solchen Aufgabe setzt voraus die ausreichende Kenntnis physikalischer, chemischer, mechanischer und technologischer Eigenschaften von verfügbaren und preiswürdigen Stoffen und Stoffzuständen, deren Beeinflußbarkeit und deren Auswirkungen auf den angestrebten Zweck einschließlich erwünschter belangloser oder auch unerwünschter aber erträglicher oder zusätzlich zu kompensierender Nebenwirkungen. Dafür wiederum braucht man ausreichende qualitative und quantitative Vorstellungen über die mit der angestrebten Funktion zusammenhängenden physikalischen Vorgänge, mechanischen Anstrengungen und chemischen Einwirkungen in dem so bedingten Verbundsystem von Werkstoffen entsprechender Eigenschaften. Aufgaben dieser Art sind z. B. Konstruktionen für die Wandlung, Verteilung, Nutzung oder Abwehr von Energie für die Herstellung, die Verarbeitung und den Transport von Stoffen, für die Darstellung von Wohnung, Kleidung und Nahrung sowie jener materiellen und organisatorischen Voraussetzungen, die dem Menschen als Gesellschaftswesen und über den physischen Bereich hinaus dienen.
Hinweisende Beispiele zeigen, daß die Problematik der Prüfung von Verbundwerkstoffen am zuverlässigsten erfaßt und beherrscht werden kann, wenn die Kenntnis der Eigenschaften von Stoffen und Materialien dem konstruktiv zu behandelnden Funktionszweck entspricht, dadurch eine souveräne Auswahl im Sinne einer weiter reichenden Kombination einzelner hervorragender Eigenschaften möglich ist und das Geplante als geschaffene Wirklichkeit durch den prüfenden Versuch und die beobachtete Bewährung bestätigt wird.
Mit Hilfe der zerstörungsfreien Prüfung (ZfP) sind i.a. verborgene Ungänzen oder Mängel in Werkstoffen, Bauteilen oder Konstruktionen zu finden, und zwar mit Verfahren, deren Anwendung am Prüfobjekt keinesfalls seine Verwendbarkeit schädigende Veränderungen hervorrufen dürfen. Dabei sind Verfahrensauswahl und -anwendung auf das Prüfobjekt, seine Verwendung und das dabei bestehende Sicherheitsbedürfnis so abzustimmen, daß das angestrebte Prüfziel mit ausreichender Zuverlässigkeit bei einem Minimum an Prüfaufwand erreicht wird.
Das Prinzip der Massenspektrometrie wird kurz erläutert. Anwendungsbereich und Grenzen der massenspektrometrischen Strukturuntersuchung werden am Beispiel von Massenspektren reiner Kohlenwasserstoffe demonstriert. Die Strukturgruppenanalyse von Mineralölen - Fragmentpeak-Methode, Molekülpeak-Methode - wird beschrieben.
Number-average molecular weights and inherent viscosities were found for the soluble members of an alkoxy-substituted copolyester series. A liquid-crystalline (high-temperature) phase was distinguisehd by IR and wide-angle X-ray scattering on molten and quenched samples in form of a nematic sanidic phase. In this phase no relationship exists between the orientation of the aromatic polyester backbone and that of the laterally attracted alkoxy groups. Further, it was proven by IR that only the polyester backbone can be aligned by shear stress. If the applied shear stress is very strong, the orientation of the stiff backbone becomes sensitive to disturbance caused by mechanical forces.
The main component of this program is a simultaneous representation of the unit cell and the calculated powder pattern. It allows the manipulation of the Crystal structure by moving selected atoms of the asymmetric unit. The resulting powder pattern can be directly compared to experimental data in order to obtain reliable starting values for further computations in refinement programs.
PowderCell 2.0 for Windows
(1998)
PowderCell contains a comfortable, user friendly visualization and modification tool for crystal structures. It provides on-line calculation of the corresponding powder diffraction patterns simulating a variety of experimental conditions. The common ICSD and Shelx file formats are supported for importing crystal structure information. It has control of automatic cell transformation and also derivation of subgroups. More than 740 different settings of the 230 space-group types are supported. Up to ten crystal structures can be considered simultaneously. A full pattern refinement enables the direct comparison with experimental diffractograms for quantitative phase analysis, lattice parameter refinement, polynomial background estimation, etc.
PowderCell as teaching tool
(1998)
PowderCell represents a user friendly program which supports the solution of scientific problems as well as teaching and education. Especially for the last one the program offers a lot of information regarding the space-group type as well as crystal structure used. Therefore, on some universities the program is used successfully to make students familiar with x-ray crystallography. The quasi-simultaneous diffraction pattern simulation visualized the changes caused by the respective crystal structure. However, it is also possible to vary different diffraction parameters and investigate the resulting changes in the interference intensity or the reflection position. In principle, the aim of the program is the intuitive generation of structure models. Therefore, special tools have been implemented to move (rotate or shift) or transform the crystal structure.
The formation of AlN films prepared by N+2 ion implantation into aluminium was investigated using X-ray and Auger photoelectron spectroscopy ( XPS, AES) as well as cross-sectional transmission electron microscopy (XTEM). After 100-keV N+2 implantation of low doses (1×1017 cm−2), the formation of hexagonal AlN nanocrystals (crystal size <5 nm, Ncrystal=1017 cm−3) was observed. Their orientation is strongly correlated with the aluminium matrix. With the dose increasing to 3×1017 cm−2, crystal growth follows, finally forming a homogeneous AlN-layer. Furthermore, the diffraction patterns show an increasing amount of misorientation with increasing dose. From the crystal size distribution, we conclude that continuous nucleation takes place. Samples implanted with an energy of 3 keV exhibit analogous behaviour. Nitride growth was further investigated using microstructured AlN formed by 3-keV implantation through movable TEM-masks (structure size: 15–150 mm).
In the case of high N+2 doses (D&5×1017 cm−2), AlN is detected by AES in the shielded area at a distance of up to 10 mm from the exposed region. The Diffusion coefficient was calculated to be 10−10 cm2 s−1. The formation of AlN proceeds in two steps.
After a continuous nucleation, diffusion-assisted Crystal growth takes place until a homogeneous AlN layer results.
Platinum does not form any adherent oxides and can be easily wetted by tin-based solders. Platinum is also an available metallization in semiconductor laboratories. Therefore we investigated the diffusion of platinum thin-film metallizations into eutectic tin–lead solder by using a high-resolution secondary ion mass spectroscopy (SIMS) profiling from the back side. It is shown that an intermetallic phase (PtSn4) is formed during soldering, which controls the consumption of platinum during soldering and in operation. The consumption of platinum follows the well-known parabolic diffusion law. The activation energy of this process is 0.63 eV. Even at extended heating cycles of 2 min at 250°C, 190 nm from the original 300 nm of the platinum film remain undissolved. This high stability makes platinum a very attractive thin-film metallization for flip-chip (FC) bonding of new microsystems.
Einsatzbereiche des Meßsystems:
- Ortung von Strukturelementen oder Verdichtungsmängeln in Beton
- Dickenbestimmung von Bauteilen bei einseitiger Zugänglichkeit
- Messung des Haftverbundes bei mehrschichtigen Bauteilen
Auswerteverfahren:
- Prinzip der laufzeitkorrigierten Überlagerung
Vorteile:
- Automatischer Meßablauf durch Array-Technik
- Flexibler Einsatz durch lange Kabelverbindungen zwischen Prüfkopfarray und Meßapparatur
Der große Vorteil der vorgestellten Methode liegt in der quasi on-line Bereitstellung der Ergebnisse und in der Möglichkeit des Einsatzes direkt am Bauwerk. Die vorliegenden Meßergebnisse zeigen den erfolgreichen Einsatz von LIBS zur Messung der Betonzusammensetzung. Eine Unterscheidung von Zementen gelingt durch die Einordnung der Meßwerte ins Dreistoffdiagramm.
Neue kleine Laser, handliche Echellespektrographen und neuartige Lichtleiter lassen sich zu mobilen LIBS-Apparaturen kombinieren, die eine Messung undAuswertung vor Ort ermöglicht.
Our aim is the application of LIBS as a simple, quasi on-line method for the non-destructive testing of concrete. Concrete is naturally inhomogeneous. Therefore we must take into account the local variation of the element composition using a statistical analysis. Depending on how much cement and aggregate is measured with each laser pulse, a scan on the surface of a concrete specimen produces a distribution of points in the Rankin diagram which is used to characterise the concrete.
Die volle Leistung einer auf Reibung basierenden Bremse wird erst nach einem Einlaufvorgang erreicht. Dieser ist notwendig, um auf Belag und Scheibe eine sogenannte Reibschicht aufzubauen. Da diese Zwischenschicht das Reibungsverhalten des Systems maßgeblich bestimmt, ist es wichtig, sich Klarheit über ihre chemische Zusammensetzung, Mikrostruktur und die daraus resultierenden Eigenschaften zu verschaffen.
Als Basismaterial diente ein phenolharzgebundener Belag Jurid 57-62, der mit verschiedenen Parametern (Flächenpressung und Umdrehungsgeschwindigkeit) gegen eine Stahlscheibe getestet wurde. Es wurden Dauerbremsungen von jeweils einer Stunde bzw. bis zu einem maximalen Belagverschleiß von 1 mm simuliert, wobei die Entwicklung der Reibzahl und die Oberflächentemperatur der Scheibe registriert wurde.
Zur Analyse der Reibschichten auf dem Bremsbelag wurden mehrere Methoden parallel angewandt. So wurden Verschleißpartikel, die aus der Reibschicht stammen, gesammelt bzw. abgekratzt und nach Dispergieren auf Kohlefolien direkt im Transmissionselektronenmikros-kop (TEM) untersucht. Ferner wurden von einigen ausgesuchten Belagproben Mikrotom-schnitte sowie dünne Querschnittsfolien für die TEM-Untersuchung präpariert, um den Verbund Reibschicht-Grundmaterial darstellen zu können. Als Ergänzung wurden ferner oberflächenmorphologische und –analytische Verfahren wie REM/EDX und ESCA eingesetzt.
Die Ergebnisse deuten darauf hin, dass die Reibschicht nanokristallin ist, und dass fast alle anorganischen Bestandteile des Bremsbelags sowie Eisenoxid von der Bremsscheibe in sehr fein verteilter Form vorliegen. Bei Belägen ohne Metallanteil bildet eine Barium-Eisen-Sulfatphase offenbar die Grundstruktur der Reibschicht, während auf eisenhaltigen Belägen Eisenoxid dominierend ist. Die nanokristalline Mikrostruktur entsteht, ähnlich wie beim mechanischen Legieren, durch einen Mahlvorgang von Verschleißpartikeln zwischen den Reibpartnern. Bei Überlastung des Belags tritt Zersetzung der Polymer-Bindephase ein, was zu einem raschen Anstieg der Verschleißrate führt.
Ziel der Untersuchungen ist die Weiterentwicklung der Impuls-Thermografie als quantitatives zerstörungsfreies Prüfverfahren zur Ortung oberflächennaher Inhomogenitäten in Bauteilen und Bauwerken.
Zur Zeit werden Putzablösungen auf Mauerwerk bzw. Beton, Hohlstellen und Kiesnester in Beton, Ablösungen und Hohlstellen bei Spaltklinkern im Dickbettmörtel auf Beton, Verbundprobleme von CFK-Laminaten auf Beton sowie Ablösungen von Bitumen-Abdichtungsbahnen auf Stahl untersucht.
Die Risstiefenbestimmung in Festen Fahrbahnen ist hinsichtlich der Dauerhaftigkeit der Konstruktion von wesentlichem Interesse. Im Rahmen eines gemeinsamen Forschungsvorhabens mit der DB AG wurden aus der Literatur bekannte Ansätze bewertet und darauf aufbauend ein Verfahren zur bildgebenden Rissdarstellung entwickelt. Rissüberbrückende Bewehrung sowie Kontaktstellen zwischen den Rissflanken wirken als Schallbrücken und erschweren die Risscharakterisierung, wie bei einem Einsatz an einer Betriebserprobungsstrecke festgestellt wurde. Ein aus der Literatur bekanntes Verfahren der einfachen Laufzeitmessung erwies sich für die Tiefenbestimmung von realen verunreinigten Rissen als ungeeignet.
Im Rahmen eines FE-Projektes “Inspektion Fester Fahrbahnen“ der BAM und der Deutschen Bahn AG geht es um die Anwendung und weitere Entwicklung zerstörungsfreier Messverfahren zur Beurteilung des Zustandes Fester Fahrbahnen.
Nach ersten Versuchsreihen direkt im Gleis wurden für verschiedene Bauarten die charakteristischen Herstellungsbedingungen simuliert und systematisch untersucht. Die kombinierte Anwendung der drei Messverfahren Ultraschall-Array-, Impakt-Echo- und Impuls-Radar-Verfahren wird hier an dem Beispiel “Betonschwelle in Betoneinbettung” dargestellt.
Die IE-Methode wird seit vielen Jahren zur zerstörungsfreien Prüfung von Betonbauteilen eingesetzt. Bei Anwendung dieses Verfahrens besteht oft das Problem, resultierende Frequenzspektren infolge der vielen Peaks richtig zu interpretieren. Ein wichtiges Bewertungskriterium ist dabei die Amplitudengröße eines Peaks, welche u.a. durch das Anregungsspektrum beeinflusst wird.
Im Rahmen eines FE-Projektes “Inspektion Fester Fahrbahnen“ der BAM und der Deutschen Bahn AG geht es um die Anwendung und weitere Entwicklung zerstörungsfreier Messverfahren zur Beurteilung des Zustandes Fester Fahrbahnen.
Nach ersten Versuchsreihen direkt im Gleis wurden für verschiedene Bauarten die charakteristischen Herstellungsbedingungen simuliert und systematisch untersucht. Die kombinierte Anwendung der drei Messverfahren Ultraschall-Array-, Impakt-Echo- und Impuls-Radar-Verfahren wird hier an dem Beispiel “Betonschwelle in Betoneinbettung” dargestellt.
Die Eignung des Verfahrens der Laser Induzierten Breakdown Spectroscopy (LIBS) zur Kontrolle einer ausreichenden Beschichtung und zur Bestimmung der Schichtdicke von Hydrophobierungsschichten auch im Rahmen wiederholender Messungen sollte untersucht werden. Mit LIBS kann die Elementverteilung orts- und tiefenaufgelöst in oberflächennahen Bereichen quasi on-line bestimmt werden. Es ist keine Probenpräparation notwendig. Wiederholende Messungen würden das vorzeitige Erkennen beschädigter Beschichtungen ermöglichen, wodurch kostspielige Sanierungsmaßnahmen vermieden werden.
In den letzten Jahren hat sich das Impulsradar als zerstörungsfreies Prüfverfahren im Bauwesen insbesondere zur Ortung von metallischen Einbauteilen wie z. B. schlaffer und vorgespannter Bewehrung in Betonbauteilen immer stärker durchgesetzt.
Systematische Laboruntersuchungen und Fallstudien zeigen aber auch, dass das Verfahren sehr gut zur Ortung von Hohlstellen sowohl in Mauerwerk als auch in Betonstrukturen geeignet ist.
Das Radarverfahren arbeitet nach dem Impuls-Echo Prinzip. Dabei wird von der Sendeantenne ein sehr kurzer elektromagnetischer Impuls ausgesendet (ca. 3 Halbwellen), der an Grenzflächen im Material (Änderung der Dielektrizitätskonstanten) und bei nicht zu dicken Bauteilen auch an der Rückseite reflektiert und von der Empfangsantenne detektiert wird. Bei den hier vorgestellten Messergebnissen wurden eine 900 MHz sowie eine 1,5 GHz Antenne in Kombination mit einem kommerziellen Radargerät eingesetzt.
Das Projektziel war die Vermeidung von Schäden bei Erdarbeiten und Ausschachtungen durch Entwicklung eines innovativen Bodenradarsystems mit wesentlicher Verbesserung des räumlichen Auflösungsvermögens bei der zerstörungsfreien Ortung von folgenden Objekten im Untergrund: Gasleitungen, Frisch- und Abwasserleitungen, Leitungen zur Elektrizitäts- und Kommunikationsversorgung aus verschiedenen Materialien und umgeben mit unterschiedlichen Böden mit variierendem Feuchtegehalt. Darüber hinaus ging es um die Reduzierung der Kosten und Erhöhung der Akzeptanz des Verfahrens durch eine schnelle Echtzeit-Interpretation der Messdaten.
Die Risstiefenbestimmung in Festen Fahrbahnen ist hinsichtlich der Dauerhaftigkeit der Konstruktion von wesentlichem Interesse. Im Rahmen eines gemeinsamen Forschungsvorhabens mit der DB AG wurden aus der Literatur bekannte Ansätze bewertet und darauf aufbauend ein Verfahren zur bildgebenden Rissdarstellung entwickelt. Rissüberbrückende Bewehrung sowie Kontaktstellen zwischen den Rissflanken wirken als Schallbrücken und erschweren die Risscharakterisierung, wie bei einem Einsatz an einer Betriebserprobungsstrecke festgestellt wurde. Ein aus der Literatur bekanntes Verfahren der einfachen Laufzeitmessung erwies sich für die Tiefenbestimmung von realen verunreinigten Rissen als ungeeignet.
Today's civil engineering NDT needs are for quantitative, fast to apply and easy to interpret methods. They are required on site both for evaluation of existing structures/infrastructure and for quality control in new construction. With this purpose, BAM has carried out in-situ feasibility studies, using radar, impact-echo and ultrasonic-echo methods. Two examples are given of their combined application on different railway slab–track constructions, using high frequency radar, scanning impact-echo and ultrasonic array methods. The aim was to evaluate limitations and advantages, comparability and complementarity of these methods. The on-site measurements demonstrated the possibility to investigate, with good accuracy via NDT, the bonding conditions between sleepers and slab, to locate voids and measure layer thickness. The acoustic and electromagnetic methods used, were found to be complementary.
Das Impaktecho-Verfahren wird seit vielen Jahren zur zerstörungsfreien Untersuchung von Betonbauteilen eingesetzt. Um die Mechanismen der elastischen Wellenausbreitung besser zu verstehen und den Einfluss von Geometrieeffekten auf das Messergebnis herauszuarbeiten, wurden Messungen und numerische Simulationen an einer
Betonplatte mit drei innenliegenden Hüllrohren durchgeführt.
Für die Strukturaufklärung von Betonbauteilen existieren mehrere bildgebende Ultraschallecho-Verfahren, u. a. mit Nutzung des Prinzips der synthetischen Apertur. Die Ergebnisse werden mit unterschiedlichen Verfahren, mit oder ohne Anwendung von Rekonstruktionsrechnungen, ausgewertet und in der Regel als B- bzw. C-Bilder dargestellt.
Ziel ist es, die unterschiedlichen Verfahren anhand von Messreihen an Testkörpern mit bekannten Prüfobjekten in Hinblick auf Ihre Leistungsfähigkeit quantitativ zu fassen und zu vergleichen, um den Einsatz der Prüfverfahren bei Untersuchungen unbekannter Objekte zu optimieren. Dazu wurden drei Kenngrößen definiert. Als erster Schritt erfolgte die Anwendung der Definitionen auf vorliegende Messergebnisse zu einer in einem 50 cm dicken Betontestkörper parallel zur Messfläche eingebrachten Bohrung.
The program PowderCell is a crystallographic tool for visualization of Crystal structures. However, it offers also non-conventional features like the fulautomatical generation of subgroups or the consideration of non-standard settings of space-group types. On the one Hand the program is very useful for non-crystallographers who like to get an impression of the atomic arrangement within the unit cell. But also for crystallographers it is recommendable because it contains a lot of additional information which can be extracted and used like data given in the International Tables for Crystallography, Vol. A. However, the most important advantage of the program is the simultaneous calculation of the X-ray or neutron diffraction powder patterns for a mixture of up to 10 crystalline phases. Between more than 7 different characteristic radiations can be chosen and their influence on the resulting powder pattern can be studied. Furthermore, experimental diffractograms can be analysed using a refinement procedure. The implemented LeBail-algorithm allows the investigation of unknown phases. In combination with the refinement algorithm an interface to Shelx offers the possibility for a step by step ab initio structure analysis. Certainly, the user-friendly shell is one reason that especially users who are not so familar with space-group symmetry, crystal structure data or diffractometry use this powerful tool for the solution of scientific or analytical problems as well as in teaching.
X-ray stress analysis on crystalline materials is based on the determination of elastic lattice strains. The strains described by the shift of peak positions are converted to stresses by the means of theory of elasticity. The development of the sin2ψ-method of X-ray stress analysis introduced an enormous progress in X-ray stress analysis during the last decades. This report outlines some important elements of X-ray physics and fundamentals of theory of elasticity. The Standard measuring procedure are described and special experimental differences to the common powder diffractometry are outlined.
XTEM and TFXRD investigations of ohmic Ti/Al/Ti/Au/WSiN contacts on AlGaN/GaN HFET layer systems
(2002)
The microstructural features of the high-temperature-stable ohmic contact system Ti/Al/Ti/Au/WSiN on AlGaN/GaN were investigated using analytical transmission electron microscopy and thin film x-ray diffraction.
For two typical rapid thermal annealing steps at 750 ◦C (non-ohmic behaviour) and 850 ◦C (ohmic behaviour) the intermetallic phases at the metal–semiconductor interface are presented. Increased annealing leads to the transformation of an Al2Au-AlAuTi phase mixture to a mixture of Al2Au-Al3Au8 phases and the formation of Ti-Al-nitride layers at the interfaces. In light of these results the electrical contact properties are discussed.
This Report describes the certification of the reference material antimony implanted in Si/SiO2 intended to be used for calibration of surface and near surface analytical methods. It describes the preparation, homogeneity measurements and the analytical work performed for the certification of both Areal density of antimony Atoms (retained dose) and the isotope amount Ratio as well as giving considerations on the stability of the material.
HIIRM final report
(2002)
Accurate analytical results have become more and more an absolute essential tool for further progresses in technology and science. Precision however, often used in this context as a quality criterion for analytical methods, is not a replacement for accuracy in any way. Therefore, analytical procedures are necessary, which will generate reliable and accurate results and can be used for evaluation of other analytical procedures and certification of reference materials (RM). Especially the certification of reference materials for the amount content of trace elements requires highly accurate results with a small combined uncertainty. The best example for an analytical procedure having this capability is undoubtedly Isotope Dilution Mass Spectrometry, for inorganic as well as for organic applications. Applied on Thermal Ionization Mass Spectrometry (TIMS) isotope dilution provides results of highest quality and proven high accuracy especially in the field of RM certifications for more than 30 years.
The major drawback of this approach often is the necessity for a complex chemical separation step. A major advantage of Inductively Coupled Plasma Mass Spectrometry (ICP-MS) is the potential to cope with a simplified or an on-line-carried-out sample preparation. A key requirement of isotope dilution analysis however is the accurate and precise determination of isotope ratios, because of its limiting factor for the accuracy and the total uncertainty of the result. Very precise isotope ratios can be determined in combination with a detection system that is capable of simultaneous detection of different isotopes, a so-called multi-collector system.
The objective of the presented project is to evaluate the advantages of such a multi-collector ICP-MS for the application of IDMS in the field of trace elemental analysis in reference materials. The focus is on the development of simple and fast procedures for isotope ratio measurements in general and IDMS analysis in particular. Furthermore, it is an objective to develop and evaluate on-line spiking procedures.
One of the first conclusions, which had a severe impact on the HIIRM project, arose during the early days of the project. Currently most certification experiments are accomplished by certification campaign based on a variety of participants’ results. The sample preparation, sending, analyzing and data evaluation however require lot of resources and the process may take a long time. An alternative way is given by using fewer participants with methods of higher metrological quality. For elemental amount contents such a method undoubtedly is isotope dilution analysis and multi-collector ICP-MS offers the necessary precision and matrix robustness and ruggedness as said above. Therefore, a multiple collector ICP-MS was manufactured as part of the project instead of the originally planned high-resolution instrument. Due to the novelty of the multicollector ICP-MS instrument, a lot of additional fundamental research became necessary. Especially interferences needed further attention. Fortunately, the IsoProbe is additionally equipped with a high-resolution option and with a brand new collison cell. The high-resolution option however can only be used to identify interferences but cannot be used to quantify them. On the other hand, the use of the collision cell proved to be a vital tool to overcome interferences. This is especially true because high resolution would have reduced the available sensitivity by a factor of ~100. Applying the collision cell technology the high sensitivity was maintained whilst most interferences were eliminated. However finding the right parameters of operation for the collision cell became a huge part of the method development process. A variety of gases like argon, helium, hydrogen, deuterium, nitrogen, krypton and xenon were tested for their suitability. Especially the tests accomplished for iron determinations revealed that carefully selected parameters have an incredible influence on the quality of the final results. Nonetheless collision cell technology will undoubtedly be widely used for newer ICP-MS instrumentation and contribute to eliminate wrong analytical values caused by interferences.
The enhanced sensitivity of the instrument revealed also problems not detectable by other means. The control of contaminations seems to be one of the major analytical challenges in the future. Sector field based ICP-MS will give the user an opportunity to trace sources of contamination back to their origin and eliminate them. Even lower limits of detection will be the result as well as an enhanced reliability for analysts dealing with higher amount contents. The analyst will also benefit in controlling blank levels when the method of isotopically spiked procedure blanks is used as demonstrated in this project.
Another main part of the project was the validation of the developed procedures. The first validation step was successfully accomplished by applying these procedures on the standard solutions provided by NRG. The main part of this validation however consisted of the evaluation of the fundamental parameters of the isotope dilution process and related measurements. This approach turned out to be superior compaired to the first step as a highly reliable uncertainty calculation can be easily performed. The best reputation and acceptance of the methods can however only be accomplished by participating in certification campaigns or in interlaboratory comparisons on highest metrological level. The results of the participations in general were brilliant. Not only the results but also the obtained realistic uncertainties were of superior quality. Direct comparisons at BAM with the results obtained by a multicollector TIMS applying the same calculation schemes showed the benefits of using multicollector ICP-MS. The main benefits of ICP-MS were identified, of which the first one is the enhanced precision of the isotope ratio measurement. For a variety of elements the values obtained by multicollector ICP-MS are even more precise than the ones obtainable by multicollector TIMS. The second important advantage identified was the simplified sample preparation. The laborious and time consuming analyte-matrix-separation step as necessary for TIMS measurements can either be omitted or at least be drastically reduced. Therefore, the advantages regarding time and enhanced sample throughput will result in further spread of ICP-MS in general and multicollector ICP-MS in particular.
The third major part in terms of the method development process was mainly focused on developing an online isotope dilution system. The volumetric instead of the gravimetric IDMS approach proved difficult, if the high demands necessary for RM definition measurements are to be fulfilled. The major obstacle in this case is the missing stability and precision in terms of mass flow. Consequently, the initial development failed as the system made up of two piezoelectric droplet injectors was unable to reach the required stability as well as precision. The thereupon-created system consisting of two HPLC pumps proved to be far more valuable regarding automation and particularly the quantification of transient signals. Nevertheless, such a system will probably be rarely used in certification campaigns, as the gain of time is too small compared to the loss of reliability. However, this system proved most valuable in terms of species-specific elemental analysis as preliminary investigations showed. In this context this system will be suitable for certification measurements, as the major uncertainty contributions derive from sampling, sample treatment and species distribution and as moreover all availabel methods demonstrate far beyond.
During the whole project, one of the main concerns regarding the multicollector ICP-MS instrument were software issues caused by the early development state of the original control programs. A lot of effort was necessary to accomplish the necessary data manipulations externally. The development of a new software suite by Micromass for the HIIRM project has solved this issue almost completely. With the new software suite and the validated parameters of measurement a step forward for institutes dealing with reference material certifications was achieved.
Future certifications campaigns for minor elemental contents in different matrices should be performed by a small number of participants from highly qualified institutes. These institutes should apply very reliable methods of measurement like the ones developed in the HIIRM project. Many resources may be saved that way while the outcome of the certifications may easily be improved. ICP-MC-MS has the potential to be an important method in this context. Stable isotope dilution analysis in combination with a multi-detector ICP-MS, equipped with a hexapole collision cell for the suppression of important spectral interferences and for enhanced sensitivity, proved to be an advanced method of elemental analysis with a high potential for matrix independent measurements. Since ICP mass spectrometers of this type have only recently been introduced, no systematic evaluation of the capabilities of this specific application of the ICP-IDMS method has yet been made.
Wirbelstromprüfung an Eisenbahnschienen - Integration der Wirbelstromtechnik in Ultraschallprüfzüge
(2004)
Eisenbahnschienen sind betriebsbedingt hohen mechanischen Belastungen ausgesetzt. Es ist notwendig, Schädigungen möglichst frühzeitig zu detektieren und hinsichtlich ihrer Schädigungstiefe zu bewerten, um sie durch gezielte Schienenbearbeitung (Schleifen, Hobeln, Fräsen) rechtzeitig zu beseitigen. Mit der bisher in Schienenprüfzügen eingesetzten Ultraschalltechnik lassen sich die Oberflächenfehler nur schwer detektieren. Eine Bewertung der Schädigungstiefe ist nicht möglich. Die Wirbelstromtechnik stellt als oberflächennahes Verfahren der zerstörungsfreien Prüfung eine ideale Ergänzung zur volumenhaften Ultraschallprüfung dar. Es wurde ein Wirbelstromprüfsystem entwickelt, das eine Detektion und Tiefenbewertung von Oberflächenfehlern bei einer Prüfgeschwindigkeit von bis zu 100 km/h und einem Messpunktabstand von 1 mm ermöglicht. Das Wirbelstromsystem kann in das vorhandene Ultraschallsystem integriert werden. Dieses beginnt mit der Übernahme der Dateinamen zur Speicherung der Messdaten, dem synchronen Start und Stopp der Messung, Ortssynchronisation über gemeinsamen Wegtakt und externe Kilometrierung bis hin zur gemeinsamen Darstellung der Prüfergebnisse. Die unterschiedlichen Ultraschallsysteme der verschiedenen Prüfzüge erfordern eine flexible Konfigurierbarkeit der Schnittstelle (Digital-IO, LAN). Wegen des enormen Umfanges der Urdaten ist es erforderlich, die Auswertung der Wirbelstromdaten so weit wie möglich zu automatisieren. Als Ergebnis der automatisierten Auswertung erhält der Prüfer Angaben über Lage, Art und Häufigkeit von Fehlern sowie die maximale Schädigungstiefe. Nebenbei ist das Wirbelstromsystem auch in der Lage, Schweißnähte in den Schienen zu detektieren. Da die Schweißnähte auch optisch zu erkennen sind, stellen sie ein wichtiges Merkmal zum Auffinden von Fehlstellen dar.
The orientation relationship (OR) between the bcc and fcc phase in the plessite microstructure of the iron meteorites Watson, Agpalilik and Gibeon has been analysed in a scanning electron microscope using electron back-scattered diffraction (EBSD). A very strong OR exists, independently on the analysed plessite type and the observed spreading of single orientation data. The agreement between the experimental orientation distribution and existing models varies for each meteorite. The black plessite in the Agpalilik corresponds to the Nishiyama-Wassermann model whereas the Duplex plessite of the Gibeon meteorite shows an OR close to the Kurdjumov-Sachs model. The Watson meteorite is strongly deformed so that a general OR is difficult to determine due to the blurred experimental orientation distribution.
An extensive comparison between the conventional Vickers hardness at 500 mN and indentation hardness measured with Vickers indenters at 500 mN is presented for up to 20 different materials and for three different instruments. Additionally, the indentation modulus is compared to Young’s modulus, which was measured with alternative methods or taken from the literature. It is shown that the agreement between the results from depth-sensing indentation and the reference values can be improved by additional corrections, for the calculation of the indentation area. With corrections the mean hardness difference to the Vickers hardness reference as average of all investigated materials can be reduced to about 10 % although disturbing pile-up or sink-in effects can still not be considered. For the modulus, the mean difference was only about 6 %.
The often poor construction and low maintenance level of tailings dams has caused serious accidents. The EC funded Project TAILSAFE is aimed at the non-destructive assessment of tailings facilities for stabilization analyses and the development of better management methods.
The focus of geophysical field studies was on the discrimination of different layering and construction steps as well as the determination of the spatial (relative) water content in the dams. SIP measurements at three tailings facilities different in their geological backgrounds, composition and age have been conducted.
Electron backscatter diffraction and energy-dispersive X-ray spectrometry were used to investigate the intermixed interface produced during laser cladding of a Co-Cr-Mo alloy on a steel substrate. A multi-component system and rapid solidification conditions together lead to a complex microstructure at the interface. The solidification of the cladding starts with the formation of an interface layer, which is about 75µm in thickness and consists of randomly oriented equiaxed grains of Co-Cr-Fe solid solution and martensite. Orientation analysis of the grains in the interface layer revealed that some grains have a special orientation relationship with the former austenite grains in the heat affected zone but the cladding is not formed by epitaxial growth on the substrate. Intermixing of the materials at the interface is providing a strong bond between the substrate and the cladding. For a grain from the interface layer to emerge as columnar grain in the cladding, it was determined that its <001> crystallographic direction is not supposed to deviate more than 25° from the sample normal direction.
A Co-Cr-Mo laser cladding applied on railway wheels is characterised by a combination of EBSD and EDX. A complete pass of the cladding is investigated to achieve a better understanding of the microstructure evolution during laser cladding. A microstructure with columnar grains extending over the whole thickness of the cladding is observed. The grains have a <001>-fibre texture with the fibre axis parallel to the normal of the substrate surface, and a substructure consisting of cells/dendrites. During the cladding process, two different kinds of precipitates form in the cell walls, which can be identified as M6C and a non-equilibrium phase. Furthermore, stacking faults are observed to occur in the cladding grains and are discussed with respect to the laser cladding process.
The hydrogen influence on the microstructure of the austenitic-ferritic Cr22-Ni5-Mo3 stainless steel was investigated. Cathodic hydrogen charging was performed electrochemically from aqueous solution of 0.1M H2SO4 with hydrogen entry promoter addition. The aim of this study was to reveal microstructural changes appearing during the hydrogen charging and particularly to clarify the occurrence of phase transformations induced by hydrogen. The specific changes in both phases of steel were observed. In the ferritic phase, strong increase of dislocation density was noticed. Longer time of hydrogen charging leaded also to the strips and twin plates formation in ferrite phase. In the austenitic phase, the generation of stacking faults, followed by the formation of α' martensite was remarked.
During focused ion beam microscopy (FIB) of crystalline materials imaging contrast and milling result are effected by orientation of the crystals with respect to the incident ion beam. This is due to the possibility of ion channeling along preferred crystal directions which effects the depth at which interaction between ions and specimen atoms takes place. As a result of channeling emission of ion induced secondary electrons (iiSE) and secondary ions (SI) as well as the sputter rate decreases.
Theoretical channeling orientations and critical angles can be calculated.
These effects have been studied quantitatively for polycrystalline recrystallized Cu as a typical model case.
The competitive growth of columnar grains in a single-grain selector, which is used for directional solidification of single-crystal blades from nickel-based superalloys, has been investigated by electron backscattered diffraction and local X-ray diffraction analysis. It has been found that the competitive grain growth in a starter block is determined by the crystallographic factor: rapidly growing grains with the axial orientation close to the [001] direction dominate in this part of the casting. For the competitive grain growth in a helicoidal separator, the geometric factor (the position of a grain at the input of the separator) is also important. The results obtained suggest that an appropriate geometry of the single-grain selector was chosen. In addition, the distribution of the orientations of columnar grains obtained by electron backscattered diffraction, can be used for approximate estimation of the yield of suitable (i.e., with the deviation of the axial orientation from the [001] direction within a specified tolerance) single-crystal blades.
Fatigue crack propagation investigations have been performed in austenitic-ferritic duplex stainless steel H22N5M3 in air and during hydrogen charging, using various frequencies of loading. Strong differences of crack propagation velocity depending on the test conditions were noticed. Lower frequency with applied hydrogen charging led to the huge increase of crack propagation velocity compared to the tests performed in air. To understand such a behaviour in each case and characterize crack mode, the samples were observed using electron back-scattered diffraction (EBSD). It was shown that in air, the fatigue crack propagation involved plastic deformation and the resulting cracks had ductile character. The presence of hydrogen led to more brittle mode of cracking. This effect was also connected with frequency of loading: lower frequency, which assured longer time for hydrogen-crack tip interaction, resulted in the highest crack propagation velocity and the brittle cracking mode with lower amount of plastic deformation. The performed observations indicated that the path of the crack went mostly transgranularly through both austenite and ferrite phases. Phase and grain boundaries were not the preferred paths for crack propagation.
Interphase boundary characterization in duplex steel and iron meteorites using EBSD technique
(2006)
The properties of materials are mainly described by the orientation distribution of the crystalline phases in a material. Beside the so considered anisotropy also the grain as well as phase boundaries are of extreme importance for a whole string of properties, e.g. the strength of a material. On the example of the interface between fcc and bcc iron the discovered and derived models are discussed. Although the common models are based on the crystal lattice description, the atomic configuration on the interface is analysed. Since experimentally a wide spread of orientations data appears the consideration of the frequency distribution is proposed to find at least the main orientation relationship between fcc and bcc. High-indexed pole figures as well as the Euler subspace are introduced in order to increase the accuracy and to compare different measurements. For the sake of simplicity EBSD measurements on iron meteorites are used since they commonly consist of large fcc single crystals which transformed to a low and very specific number of bcc grains. In special cases the described procedure could also be used for steels.
Die Erarbeitung der Grundlagen für effiziente und bedarfsgerechte Instandsetzungsmaßnahmen an Schottergleisbetten ist das Ziel des Projektes „SafeRail“. Das Impulsradarverfahren wird als zerstörungsfreie Methode für die Zustandsbestimmung des Schotters verwendet, um entsprechend den hohen Anforderungen der Netzbetreiber Unterbrechungen des Schienenverkehrs weitgehend zu vermeiden. Für eine automatisierte Bewertung der Vermischung des Schotters mit dem Untergrund sowie des Abnutzungszustandes des Schotters wird ein Antennenarray entwickelt, das bezüglich seiner Messgeometrie optimiert wird.
In this paper, a new method for the investigation of the degradation of ballast railway track beds is proposed. An array of antennas is used for simultaneous acquisition of reflected radar impulses, which have been transmitted from different sending positions. This array setup allows an automated CMP-measurement, which enables a direct calibration of the ballast thickness. These multiple offset measurements using the array setup are well suited for fast railway inspections. The method offers the possibility to visualize the state of degradation of the ballast in a velocity spectrum.
Dyke breaks - caused by e.g. Overflows or Slop breaks during long lasting high water gauge - Play a great role in a failure potential of extreme flood Events.
Using conventional dyke condition Monitoring dyke messengers can undertake only a visual surface inspection. Thus defective Areas can oftentimes be discovered too late.
A critical area in which failures due to soil displacement and moisture Penetration become more significant is located at a landside dyke foot. Geotextiles are integrated here as a Drainage in case of modern three-zone type of dyke.
Aflatoxins, a group of structurally related mycotoxins, are well known for their
toxic and carcinogenic effects in humans and animals. Aflatoxin derivatives and protein
conjugates are needed for diverse analytical applications. This work describes a reliable
and fast synthesis of novel aflatoxin derivatives, purification by preparative HPLC and
characterisation by ESI-MS and one- and two-dimensional NMR. Novel aflatoxin bovine
serum albumin conjugates were prepared and characterised by UV absorption and
MALDI-MS. These aflatoxin protein conjugates are potentially interesting as immunogens
for the generation of aflatoxin selective antibodies with novel specificities.
Reinigung wird in der Lebensmittel- und Pharmaindustrie aufgrund des stetig steigenden Kosten- und Zeitdrucks sowie der hohen Verbrauchererwartungen hinsichtlich Produktsicherheit und -haltbarkeit ein immer zentraleres Thema. Eine verbesserte Reinigbarkeit bedeutet für die produzierende Industrie eine Steigerung der Effizienz der Produktionsanlage. Besonders in der heutigen medienintensiven Zeit kommt ein "Lebensmittelskandal" durch ein unsicheres Produkt einem finanziellen Desaster und immensem Imageverlust gleich. Aus diesem Grund ist die Reinigbarkeit der produktberührenden Oberflächen stets ein wichtiges Kriterium für die Werkstoffauswahl.
Basierend auf den Theorien zu Schmutzhaftung und -entfernung wurde im Rahmen dieser Arbeit überprüft, ob und wie die theoretisch relevanten Parameter auch in den Experimenten den Reinigungserfolg beeinflussen. Der Schwerpunkt wurde auf die Einflussgrößen des Werkstoffes gelegt, um herauszufinden, wie stark eine Oberfläche selbst zu ihrer Reinigbarkeit beitragen kann (self-cleaning).
In den durchgeführten Versuchen hat sich gezeigt, dass die Oberflächenrauheit lediglich bei der Reinigung von kohäsiven Schmutzfilmen eine entscheidende Rolle gespielt hat. Hingegen ist ihr Einfluss auf das Reinigungsergebnis von sich auflösenden Schmutzfilmen und Partikeln nur begrenzt bis gar nicht zur Geltung gekommen. Das Oberflächenmaterial hatte keinen starken, aber dennoch signifikanten Einfluss auf die Reinigbarkeit der untersuchten Oberflächen. Dass die Reinigbarkeit einer Oberfläche keine Materialkonstante sein kann, wurde unter Verwendung spezieller Oberflächen mit definiert geätzten Rauheitsstrukturen nachgewiesen. Der Reinigungserfolg hängt immer auch von der Verunreinigungsart ab, was sich auch in vergleichbaren Versuchen der Einzelpartikelablösung mittels AFM in dem Einfluss der Elastizität bzw. Plastizität der Partikeln geäußert hat.
Praxistaugliche Empfehlungen gehören mit zu den wichtigsten Zielen dieser Arbeit gewesen. Mit Fokus auf die Oberflächenparameter und auf Basis der durchgeführten Untersuchungen wurde zur Optimierung der Reinigung produktberührender Oberflächen für bekannte Kontaminationen eine Checkliste als Orientierungshilfe erarbeitet. Ist die Verunreinigungsart dennoch unbekannt, so sollte der "Grenzwert" von Ra = 1 µm unterschritten werden, um bei Vorhandensein filmartiger Verschmutzungen keine negativen Auswirkungen auf die Reinigbarkeit zu haben. Die Notwendigkeit nach hochpolierten Oberflächen (Ra < 0,3 µm) aus Reinigbarkeitsgründen kann aufgrund der Untersuchungen nicht nachvollzogen werden.
Das Ziel des Vorhabens wurde erreicht.
Carrying out dimensional measurements by CT means assessing coordinates in space. CT must therefore be treated as a coordinate measuring technique similar to optical or tactile Coordinate Measuring Machines (CMMs). The well-established standards and guidelines for the acceptance- and verificationtesting of CMMs require the use of calibrated reference standards to achieve measurement machine characteristics.
Hence, transferring these concepts from coordinate metrology to CT, a dedicated CT-specific reference standard was designed, manufactured and calibrated using a tactile CMM. For comparison purposes, a CAD model was created by reverse engineering using the calibration data. The calibrated model was fed into a virtual CT and the measurement process was simulated. The reference standard was measured by micro-CT.
By comparing the characteristics of the measurement output of CT and the output gained from simulation, the influences of measurement artefacts can be judged, for the first time, in analogy to existing Guidelines of coordinate metrology.
We have studied the anisotropic milling of Cu with respect to the milling rate and the milling topography, as well. The background is twofold: i) anisotropic milling has to be taken into account during the preparation of TEM specimens and in the manufacturing of micro parts from crystalline materials, and ii) the orientation depending milling behaviour can be used to generate topographies with specific properties with respect to, for example, adsorption, wear, and corrosion.
A multi-offset radar system will be presented that features the possibility to get quantitative information about the wave propagation velocity as a measure of the ballast quality. This goes beyond the regular application of conventional radar systems offering only qualitative structural information. The new approach provides a fast NDT method for the classification of ballast fouling. A main advantage of the multi-offset radar is that regular ballast digging for velocity evaluation can be avoided and travel time can be directly transformed into an equivalent depth by using the automatically evaluated velocity. The maintenance cost and interruption time can be significantly decreased by this method. The application of velocity evaluation method is common in geophysical applications but it is used for ballast inspection for the first time.
Three petrol reference materials were certified for their total sulfur content in support of Directive 2003/17/EC of the European Parliament and of the European Council, which stipulates that petrol with a maximum S content of 10 mg/kg must be available in all member states by 2009. Commercially available petrol was obtained and filled into borosilicate ampoules without further treatment. Homogeneity of the materials was tested and no heterogeneity was detected for two of the materials, whereas minor heterogeneity was observed for the third material. Stability of the materials was tested for 8-12 months at 60 °C and no degradation was observed. Characterisation was based on isotope-dilution mass spectrometry (IDMS) applied as primary method of measurement by three European metrology institutes and certified values were assigned using all results. The certified uncertainties include contributions of (potential) heterogeneity, potential degradation as well as characterisation. The final assigned values are:
ERM-EF211: 48.8 ± 1.7 mg/kg
ERM-EF212: 20.2 ± 1.1 mg/kg
ERM-EF213: 9.1 ± 0.8 mg/kg
The materials are available from IRMM (ERM-EF211), LGC (ERM-EF212) and BAM (ERMEF213)
Irrational orientation relationship derived from rational orientation relationships using EBSD data
(2008)
The determination of the orientation relationship (OR) between α-Fe matrix (bcc) and γ-Fe precipitates (fcc) is discussed using orientation data collected by electron backscatter diffraction (EBSD). The comparatively low accuracy of EBSD is compensated by the high number of measurements what allows a general statement regarding to the mean OR existing in a sample. The representation and discussion is realized on a part of the Bain zone in a {001} pole figure. A discussion of some selected rational OR which are commonly used for the phase boundary characterization between α and γ shows that the pole figures describing a transformation from γ → α are different to those for α → γ. A technique is proposed based on at least three misorientation angles between the experimental OR to the rational OR's as reference. For the misorientation angle distribution a refinement is applied to extract the mean values. They are used to detect the mean OR, what is also possible for only a few or even a single precipitate if the number of measurements describing the phase boundary is sufficiently high.
The tetragonal crystal- structure type of chalcopyrites (chemical formula AIBIIICVI2) is a superstructure of sphalerite type. The c/a ratio differs generally from the ideal value 2, i.e., the crystal structure is pseudocubically distorted. For CuInSe2 and CuGaSe2 thin films, simulations demonstrate that it is theoretically possible to reveal the tetragonality in electron backscatter-diffraction (EBSD) patterns for CuGaSe2, whereas it may not be possible for CuInSe2. EBSD experiments on CuGaSe2 thin films using the ”Advanced Fit” band-detection method show that it is possible to extract accurate misorientation-angle distributions from the CuGaSe2 thin film. Pole figures revealing the texture of the CuGaSe2 thin film are shown, which agree well with X-ray texture measurements from the same layer.
Following to a brief introduction of BAM the procedures are explained how to prepare reference materials in analytical chemistry. Examples are given for collecting and presenting data in welding, thermomechanical properties and tribology. The use of data for modelling safety in technology and chemistry is demonstrated. Finally there is in outlook on the World Materials Research Institut Forum (WMRIF) and recommendations for action.