Analytische Chemie
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Organisationseinheit der BAM
- 1 Analytische Chemie; Referenzmaterialien (1490)
- 8 Zerstörungsfreie Prüfung (1321)
- 6 Materialchemie (1069)
- 6.1 Oberflächen- und Dünnschichtanalyse (369)
- 6.3 Strukturanalytik (338)
- 8.0 Abteilungsleitung und andere (330)
- 8.2 Zerstörungsfreie Prüfmethoden für das Bauwesen (329)
- 1.1 Anorganische Spurenanalytik (294)
- 1.2 Biophotonik (271)
- 8.4 Akustische und elektromagnetische Verfahren (259)
Paper des Monats
- ja (29)
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.