Advantages of combined μ-XRF and μ-XRD for phase characterization of Ti–B–C ceramics compared with conventional X-ray diffraction

Jaroszewicz, Jakub; De Nolf, Wout; Janssens, Koen; Michalski, Andrzej; Falkenberg, Gerald
June 2008
Analytical & Bioanalytical Chemistry;Jun2008, Vol. 391 Issue 4, p1129
Academic Journal
Design and processing of new materials with improved high-temperature properties is one of the most challenging tasks of modern engineering. Among such materials, nonoxidic ceramics hold an important place. When optimizing the synthesis conditions of these new materials in an largely empirical manner, the use of analytical methods that can fully document the resulting phase compositions is of great importance. In this paper, we demonstrate the advantages of using combined microbeam X-ray diffraction and X-ray fluorescence over conventional X-ray diffraction as the characterization method in the specific case of Ti–B–C ceramics. Ceramic samples were synthesized by the pulse plasma method starting from high-purity powders of titanium, boron, graphite, and nickel. Different mixtures were heated in a pulsed fashion and sintered by combustion synthesis at various temperatures and time durations, as is the case during empirical optimization of a synthesis procedure. Conventional X-ray diffraction showed the presence of two phases at the end of the sintering process, TiB2 and TiC, irrespective of the conditions employed. Scanning μ-XRF/μ-XRD on the other hand allowed one to detect and visualize the distribution of additional phases present in the sintering products, during which a dependence on sintering conditions was apparent. The μ-XRD results showed that three phases (TiB2, TiC, and TiB) instead of two were present in samples sintered during a short time interval. The addition of metallic Ni to the initial mixture as a sintering facilitator resulted in the formation of a Ni3B phase. All phases proved to have strongly heterogeneous distributions above the 15-μm level with the presence of TiB2 anticorrelated to that of TiC and TiB, emphasizing the necessity of the use of laterally resolved methods of characterization.


Related Articles

  • Quadrupole lamp furnace for high temperature (up to 2050 K) synchrotron powder x-ray diffraction studies in air in reflection geometry. Sarin, P.; Yoon, W.; Jurkschat, K.; Zschack, P.; Kriven, W. M. // Review of Scientific Instruments;Sep2006, Vol. 77 Issue 9, p093906 

    A four-lamp thermal image furnace has been developed to conduct high temperature x-ray diffraction in reflection geometry on oxide ceramic powder samples in air at temperatures <=2050 K using synchrotron radiation. A refractory crucible made of Pt20%Rh alloy was used as a specimen holder. A...

  • Synchrotron radiation micro-XRD in the study of glaze technology. Pradell, T.; Molera, J.; Salvadó, N.; Labrador, A. // Applied Physics A: Materials Science & Processing;May2010, Vol. 99 Issue 2, p407 

    The production of glass represented an important technological achievement, and it was the starting point for the invention of a large variety of materials, produced by processes involving melting, partial or total, and precipitation of new crystalline compounds during cooling. In particular,...

  • Study of the gilding technique used in polychromed stones and ceramics by dedicated laboratory-made micro X-ray diffraction and complementary techniques. Duran, A.; Perez-Rodriguez, J. L.; De Haro, M. C. Jimenez // Analytical & Bioanalytical Chemistry;Jul2009, Vol. 394 Issue 6, p1671 

    This work describes the use of a new dedicated laboratory-made micro X-ray diffraction system for detecting the phases present in cross-sections of artworks. As an example, the phases present in samples from gilding ceramics and stone sculptures from the heritage of Seville (Spain) were...

  • Phase transition in Ba2In2O5 studied by in situ high temperature X-ray diffraction using synchrotron radiation. Rey, J. F. Q.; Ferreira, F. F.; Muccillo, E. N. S. // AIP Conference Proceedings;1/29/2009, Vol. 1092 Issue 1, p150 

    The order-disorder phase transition in Ba2In2O5 high-temperature ionic conductor was systematically studied by in situ high-temperature X-ray diffraction using synchrotron radiation and electrical conductivity. Pure barium indate was prepared by solid state reactions at 1300 °C. The...

  • Synchrotron X-ray diffraction study of the structure of oral stratum corneum model lipid membranes. Ryabova, N.; Gruzinov, A.; Zabelin, A. // Crystallography Reports;Jan2014, Vol. 59 Issue 1, p117 

    Membranes modeling the lipid fraction of the mucous membrane of the human oral cavity have been studied by X-ray synchrotron diffraction. Ternary systems, composed of a mixture of sphingomyelin, dipalmitoylphosphatidylcholine, and dipalmitoylphosphatidylethanolamine with component weight ratios...

  • High-temperature hydroxyapatite-titanium interaction. Egorov, A. A.; Smirnov, V. V.; Shvorneva, L. I.; Kutsev, S. V.; Barinov, S. M. // Inorganic Materials;Feb2010, Vol. 46 Issue 2, p168 

    Hydroxyapatite-titanium interaction has been studied in the temperature range 700 to 1200°C with a view to designing biocompatible dispersion-hardened hydroxyapatite-matrix materials for bone implants. The sequence of phase transformations in hydroxyapatite-titanium powder mixtures during...

  • Chemical disorder effect on orthorhombic-rhombohedral structural transition in La0.7Ca0.3MnO3. Rozenberg, E.; Mogilyansky, D.; Mukovskii, Ya. M.; Jung, G.; Gorodetsky, G. // Journal of Applied Physics;Jun2013, Vol. 113 Issue 23, p233511 

    High temperature X-ray powder diffraction technique was employed to study the orthorhombic to rhombohedral (O-R) structural transition (ST) in single crystal and ceramics of La0.7Ca0.3MnO3. The data obtained evidence that such ST in both samples occurs in the vicinity of temperature T ∼ 700...

  • In Situ Synchrotron Radiation Study of TiH-6Al-4V and Ti-6Al-4V: Accelerated Alloying and Phase Transformation, and Formation of an Oxygen-Enriched TiFeO Phase in TiH-6Al-4V. Yan, Ming; Dargusch, M.; Kong, C.; Kimpton, J.; Kohara, S.; Brandt, M.; Qian, M. // Metallurgical & Materials Transactions. Part A;Jan2015, Vol. 46 Issue 1, p41 

    In situ heating, synchrotron radiation X-ray diffraction has been used to study the alloying and phase transformation behavior of TiH-6Al-4V and Ti-6Al-4V alloys. Accelerated alloying and phase transformation were observed in the powder compact of the TiH-6Al-4V alloy subjected to a high heating...

  • XRD Study of NiTi Endodontic Files Using Synchrotron Radiation. Braz Fernandes, Francisco; Oliveira, J.; Machado, A.; Schell, Norbert // Journal of Materials Engineering & Performance;Jul2014, Vol. 23 Issue 7, p2477 

    Two types of endodontic files (ProFile and Mtwo) were studied in order to analyze the effect of geometry on the stress-induced martensitic (SIM) transformation during bending. The use of a fine beam spot of synchrotron radiation allowed a detailed structural characterization with a fine spatial...


Read the Article


Sorry, but this item is not currently available from your library.

Try another library?
Sign out of this library

Other Topics