Innovative Measurement and Analysis for Structural Materials

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1 SIP Structural Materials for Innovation (SM 4 I) D-2 : Materials Integration Innovative Measurement and Analysis for Structural Materials M. Ohkubo AIST nanometronics lab for structural materials, Department of electronics and manufacturing H. Kitazawa E. Kita M. Kimura KEK Request to innovative measurement and analysis Conventional mechanical test and measurement Fatigue fracture Fatigue test for HAZ (empirical data) Gap between macro and nano Innovative nanomeasurement Vacancy-type defects (scientific data) Request for nanoscale observation The empirical-to-scientific change in materials integration requires the acquisition of hidden structural information at nanoscale and bridging the gap.

2 Keen measurement needs (manifest but unrevealed) Four domains A. Polymers and CFRP Solution Measurement needs Matrix polymer Subnano-space in polymer chains CFRP rupture process B. Heat Resistant Alloys Ti 6-4 Strain in lamella structure C. Ceramic Coating D. Materials Integration EBC Nano-structure of ceramic coating 9-Cr Steel Critical role of trace light elements in creep lifetime Our focus and an example of mechanical (fatigue) test Pre-deterioration Crack growth Propagation l 0 Our focus l 0 μ μ

3 Approach and implementation for solution Approach 1 Acquisition of manifest but unrevealed information by using Approach 2 Integrated analysis (Finding of latent information) Positron Probe Microanalyzer (PPMA), X-ray Absorption Fine Structure with superconductivity (SC-XAFS), 3D atom probe with laser (3D AP), KEK One of the inventors of AP Unique e + microbeam KEK AIST and LLNL only Nano-scale Moiré interferometry, and Unique nano-scale Conventional analytical instruments. International hub SR-based X-CT with XAFS (XAFS-CT), Unique combination KEK Tsukuba Uni and PIXE for light elements with superconductivity, and Jyväskylä Uni only Ultrasonics with new laser (nano-ftir). Unique laser Approach 1 Acquisition of manifest but unrevealed information that cannot be obtain by daily analysis

4 Stage: Pre-deterioration (free volume) Free volume (< 1 nm) and mechanical property of plastics for CFRP The validity of the MD calculation has been confirmed by innovative measurement, which is the first step for changing empirical approach into scientific one.

5 Future plan for tensile and fatigue tests T. Oka et al., Appl. Phys. Lett. 101, (2012) Stage: Crack initiation (deformation imaging) DIC limit: 1 µm Moiré with nanotechnology may go to 100 nm spatial resolution.

6 Stress imaging of lamella texture Ti-6Al-4V (Challenge for stress imaging at 100 nm resolution around initial cracks) Stage: Crack growth

7 SR-based X-CT in situ imaging (< 1 μm) Stage: Trace light element and nanotexture (pre-deterioration)

8 Role of B and N in creep lifetime of 9Cr-Steel Time to rupture ( h ) 9Cr-3W-3Co-0.2V-0.05Nb-0.08C-0.014B o C, 120 MPa Nitrogen ( ppm ) Is there a way to go beyond? Minimum creep rate ( 1 / h ) Atomic scale : 3D AP image of PAGB of heat resistant steel

9 Role of institutes and approach for solution Approach 2 Integrated analysis (Finding of latent information) KEK Positron microprobe Superconducting spectrometer Moiré interferometry Approach 1 Acquisition of manifest but unrevealed information 1. Stress & Cracks 2. Trace Light Elements 3. Heterogeneous Boundaries 4. Vacancies & free volume 5. Delamination Synchrotron Radiation Positron generation 3D Atom Probe & Nanocharacterization Moiré interferometry Ion Beam Analysis Positron (doppler broadening) Approach 2 Integrated analysis (Finding of latent information)

10 Goal and international collaboration Interim goal: revealing hidden information that cannot be obtained before 1 st Symposium on Innovative Measurement and Analysis for Structural Materials 2015 KEK Guest speech Keynote 1 Keynote 2 Eizo Matsumoto (Deputy Director General, Cabinet Office) Teruo Kishi (Program Director, Cabinet Office) Yutaka Kagawa (Deputy PD, University of Tokyo) Invited speakers "XRD Analysis of Structure Material at APS "Ion Beam Analysis for Materials Science J. D. Almer (ANL) M. Ionescu (ANSTO) Asia-pacific region to world-wide expansion is expected. Final goal is to be a world-wide hub of innovative measurement and analysis. Current level may be TRL 6.