2nd Science Link Conference Chamber of Commerce and Industry , St. Petersburg

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The Concept Factory 2012. Science Link 2013

2nd Science Link Conference Chamber of Commerce and Industry 10.06.2013, St. Petersburg The Concept Factory 2012.

Neutrons and Synchrotron Radiation in Construction and Engineering Dr. Marc Thiry, Industrial Liaison Officer Helmholtz-Zentrum Geesthacht (HZG) 10.06.2013, St. Petersburg The Concept Factory 2012.

Content: The German Engineering Materials Science Center Neutrons and Synchrotron Radiation in Construction and Engineering Methods and Examples Summary

The German Engineering Materials Science Center GEMS is a central user access platform for complementary research with photons and neutrons in engineering materials science. HEMS (High Energy Materials Science Beamline) IBL (Imaging Beamline) BioSAXS Beamline Neutron Source FRM II (SANS-1, REFSANS, STRESS-SPEC, contribution to ANTARES) Instruments using synchrotron radiation are operated at DESY in Hamburg, instruments using neutrons are located at the outstation at the FRM II in Garching near Munich.

The German Engineering Materials Science Center High Energy Materials Science Beamline (HEMS) Texture determination Residual stress analysis Characterisation of nanostructures with high energy small-angle X-ray scattering (HE-SAXS) experiments Phase transformation analysis In-situ sample environments

The German Engineering Materials Science Center IBL: Tomography of engineering materials BioSAXS: Structural research on soft matter samples (biomolecules, polymers, vesicles, micelles )

In situ sample environments Furnaces Cooling devices Tensile strain measurements Dilatometer Laser and stir welding environments

GEMS Neutron Experiments FRM II: small angle neutron scattering (SANS1) reflectometer and evanescent wave small angle neutron spectrometer (REFSANS) residual stress analysis, texture determination (STRESS-SPEC) neutron computerised tomography (NCT) (contribution to instrument ANTARES)

Additional GEMS services Custom in-situ sample environments (stir and laser welding, dilatometer) Sample Preparation (including FIB) Expertise of the Institute of Materials Research at HZG Integrated beamtime proposals for photons and neutrons Laboratory infrastructure: lab X-ray diffractometer (RöDi), Tomography (Nanotom), SAXS (Nanostar) Industry specific user support (data analysis, secrecy agreements)

X-Ray tomography: 3-dimensional analysis of engineering materials X-ray Imaging has been used in medical diagnostics for over 100 years Development of the first anodes for clinical use in Hamburg around the end of the 19th century Many advancements have been made since in the use of X-rays in medicine as well as in materials science

X-ray tomography: 3-dimensional analysis of engineering materials Rotation of the sample in the X-ray beam 3-dimensional image is created by computer software

X-ray tomography: 3-dimensional analysis of engineering materials Corrosion morphology of in vivo corroded magnesium alloy Regular pattern of pitting corrosion Reduced, more uniform corrosion with singular deep pits F. Witte, J. Fischer, J. Nellesen, C. Vogt, J. Vogt, T. Donath, F. Beckmann Acta Biomaterialia 6 (2010), 1792-1799

X-ray tomography: 3-dimensional analysis of engineering materials Study of intergranular corrosion in aircraft aluminium alloys using X-ray tomography S.P. Knight et al. / Corrosion Science 53 (2011) 727 734

X-ray tomography: 3-dimensional analysis of engineering materials 6 mm Pores in Al laser beam welds very high density resolution achieved, different Al alloys can be distinguished J. Herzen et al., Proc. of SPIE 7078, 70781V (2008)

The Concept Factory 2012.

Neutron radiography Pyrotechnology in Space: Ca. 800 devices on board of ARIANE 5 for separation of components e.g. cable cutters for steel ropes of up to 10 mm tickness. Devices include modern explosives (e.g. Hexogen) Quality assurance: Every single device has to be tested before launch for Sufficient density Homogeniety of the explosive => Neutron Radiography Large penetration Good contrast for light elements, esp. hydrogen rich materials Significant portion of the production for Ariane 5 checked at GeNF since 2004 J. Vollbrandt, H.-W. Schmitz, GKSS; Fa. Dassault Aviation, Argenteuil, France

Neutron radiography Initiators Cable cutter Advantage of Neutrons: Large penetration depth Sensitivity for light elements

Microtomography of iron ore pellets (LKAB) The use of additive mixes in pellets production leads to increases in steelwork s productivity while energy use, wear and slag are reduced. Knowledge about porosity and grain sizes in the pellets will help in further development and optimization of the product 1mm HZG/DESY

X-Ray and Neutron Diffraction Interplanar distances are of same length as X-ray wavelength

X-Ray and Neutron Diffraction Interference of light at a double slit

X-Ray and Neutron Diffraction Interference:

X-Ray and Neutron Diffraction

INDUSTRIAL APPLICATIONS CI S

Phase analysis and residual stresses in welded steel plates Ykkösmetalli The influence of welding of on residual stresses in steel plates used for tunnel drillng machines in mines was investigated by XRD at P07 (HEMS by HZG/DESY) XRD Intensity (arb. units) diffraction angle (2θ) /

Dilatometer for in situ studies of phase and microstructure transformations commercial dilatometer (Bähr 850 A/D) induction heating: max. heating rate 4000 K/s max. cooling rate 2500 K/s (hollow samples) DSC unit deformation units (25 kn)

Dilatometer for in situ studies of phase and microstructure transformations temperature [ C] time [min] Ti-43Al (at.%), cast material, synchrotron experiment elongation [µm] A. Stark, M. Oehring, F. Pyczak, A. Schreyer, Adv. Eng. Mater. 13 (2011) 700 704

Stress and strain analysis Hydrogen embrittlement Service failure originating in a weld. Source: Journal of Wheel/Rail Interaction Residual stresses are almost always present in technical parts. They superpose the load stresses occurring under service conditions. Residual stresses can be adjusted in the manufacturing process residual stressengineering.

X-ray diffraction on laser spot welds Problem: Depth resolution required for residual stress analysis with high-energy X- rays in overlap joints to distinguish between the two sheets conventional stress map MPa Solution: Conical Slits With X-ray beam diameter <50 µm depth resolution <1 mm possible

Depth resolution with conical slits depth resolution conical slits detector image X-ray E = 63 kev 100 mm depth resolutions between a few mm and a few 100 µm possible T. Fischer, P. Staron, A. King, N. Schell

Residual stress properties for high strength lightweight components Volkswagen develops new light weight components for engines Some aluminium alloys require a heat-treatment step for the hardening process Following heat-treatment, a high level of residual stress is produced which can decrease the lifetime of the component Simulations have been made to predict the stresses and increase the reliability in the durability prediction

Aluminium alloy sample mounted at HZG beamline HEMS at PETRA III (DESY): cylinder head Depth resolved residual stress measurements were performed using the conical slit technique. conical slit cell

Depth resolved stress pattern: s M (max) 0 Experimental results of the project in Science Link validated the simulations made by Volkswagen

Residual stresses in forged aircraft turbine compressor discs Simulated and measured stress distribution Simulated stress pattern Stress measured by neutron diffraction

Residual stress in TiN coating on WC-Co 50 µm (h) x 50 nm (v) waveguide beam variation of microstructure and strain with depth, important for: performance of high-performance coated tool stability / adhesion of hard coating C. Krywka, H. Neubauer, M. Priebe, T. Salditt, J. Keckes, S. V. Roth, M. Müller J. Appl. Cryst. 45, 85-92 (2012)

Texture analysis Crystal arrangement ND RD TD Grains Many technical important materials, such as metals, ceramics and some plastics, are polycrystalline. Texture assessment describes the orientation distribution of the crystallites. All properties* influenced by the anisotropy of the constitutive crystals depend on the texture. *i.e. elastic, plastic, electrical, magnetic, thermal

First grain mapping experiment with in situ tensile testing 0.7 mm accuracy: grain position 30 µm, orientation 0.15, grain volume 35 % Jette Oddershede, Søren Schmidt, Ulrik Lund Olsen, Bettina Camin, Torben Fischer, Norbert Schell (2011)

Nanostructure of the wood cell wall S. Storm, M. Ogurreck, C. Krywka, M. Müller (2012)

Investigation of the setting of cements by time resolved XRD Cement represents a complex colloidal suspension consisting of reacting crystalline and amorphous phases. XRD enables the study of cement hydration on the millisecond timescale. M. Schlegel, A. Sarfraz, U. Müller, U. Panne, F. Emmerling, Angew. Chem. Int. Ed. 2012, 51, 4993 4996

Small angle scattering Available with neutrons and X-rays Useful for structure analysis of hard and soft matter in the nanometer scale

Investigation of agglomeration of nanoparticles in polymer resins By Small angle neutron scattering (SANS), the amount and size of aggregations of nanoparticles in solution as well as in polymer matrices can be examined 1. W. Reimers (editor), A. R. Pyzalla (editor), A. K. Schreyer (editor), H. Clemens (editor,) Neutrons and Synchrotron Radiation in Engineering Materials Science, Viley VCH, 2008, p. 245.

Examination of passivation of iron surfaces by XAS Chemical surface passivation of iron artefacts by carboxylates. Absorption energies match reference substance. F. Mirambet, S. Reguer, E. Rocca, S. Hollner, D. Testemale Applied Physics A, 2010, 99 (2), 341-349.

Possibilities of X-ray absorption spectroscopy in engineering and materials science: Corrosion studies of various materials Corrosion protection Other chemical surface treatments

Summary: Synchrotron- and neutron sources offer a broad field of solutions for scientific problems in construction and engineering: X-Ray and Neutron diffraction texture, phase analysis, residual stress Tomography 3D imaging X-ray absorption spectroscopy chemical surface treatments, corrosion What can Science Link do for your company?

Thank you Contact: Marc.Thiry@hzg.de www.science-link.eu The Concept Factory 2012.