Mapping Crystal and Material Phases with Neutron Imaging

Mapping crystal and material phases with neutron imaging

Daniel S. Hussey J.M. LAMANNA, D.L. JACOBSON National Institute of Standards and Technology, Gaithersburg, MD

H-Bearing Minerals Type I/II Chondrules Iron-Nickel and Opaque and Metallic Veins Assemblages 2nd Congreso Argentino Técnicas Neutrónicas National Institute of Standards and Technology (NIST)

• Main Campus Located in Gaithersburg, MD USA • Satellites in Boulder, CO and Charleston, SC • ~15 miles north of Washington D.C. • Established 1901, First U.S. National Lab • ~650 acres, ~3000 people, 4 Nobel Laureates

NCNR

2nd Congreso Argentino Técnicas Neutrónicas NIST Center for Neutron Research (NCNR) • Operating since 1967, re-licensed to run till 2029 • 20 MW Research Reactor • Largest neutron scattering user program in the U.S.

2nd Congreso Argentino Técnicas Neutrónicas NCNR Scattering and Imaging Instruments 2018: 28 operational instruments • 7 thermal • 21 cold – 2 new under development – 2 Neutron Imaging Instruments – Access via call for proposals 2x per year (no fee for beamtime) • Proposals from any country accepted – Proprietary experiments at full cost recovery ~$6k / day

2nd Congreso Argentino Técnicas Neutrónicas NIST Imaging Program Usage (2006-2018)

Instrument & USAGE BY RESEARCH TOPIC • Total Number of Beam Battery & Alternate Energy Detector Irradiation 6% Days: 1931 Development 1% Biology Cyrogenic 11% 3% Liquids • 416 Unique Experiments 2% Industrial Engineering / • 2% 40 Patents (Fuel Cells only) Materials • 200 papers Hydrogen 5% Storage & • 66 PhD Students Production 4% Heat Pipe Usage by Institute Type 4%

Indsutry

34% 28% Academic Concrete, Geology, Fuel Cells National Lab Porous Media 49% 38% / Agency 13% Continue to grow with NeXT

2nd Congreso Argentino Técnicas Neutrónicas Seeing the world with neutron vision

Did Superman have the wrong vision?

2nd Congreso Argentino Técnicas Neutrónicas Seeing the world with neutron vision

2nd Congreso Argentino Técnicas Neutrónicas 7 The NIST Simultaneous Neutron and X-ray Tomography System Neutron X-ray

Full Volumes

Segmented Composite Volume

J.M. LaManna et al, Rev. Sci. Inst., 88, 113702 (2017). ➢ Neutrons: organics ➢ X-rays: minerals nd 2 Congreso Argentino Técnicas Neutrónicas W.S. Chiang et al, PETROPHYSICS, 2018 NeXT Phase Segmentation

Neutron attenuation (mm-1)

X-ray attenuation (mm-1)

Neutron (a) and X-ray (b) tomograms of an Alkaline AA battery

2nd Congreso Argentino Técnicas Neutrónicas One NeXT segmented slice Identifying structure formed by ASR

Highly reactive Na/K volcanic glass as gel ‘point source’ Characteristic structures formed by ASR imaged destructively with SEM

X N X N

This is the first time ASR has been identified nondestructively in a large volume, i.e. 10 mm dia, 15 mm height vs single slices in SEM 2nd Congreso Argentino Técnicas Neutrónicas Dissolution of Limestone Under Acidic Conditions 3.8 cm diameter cores, 60 micrometer resolution • Aim: understand pore network evolution during acid flow in limestone for purpose

of CO2 sequestration • Neutron radiography to capture dynamic pore formation • Simultaneous CT to obtain 3D pore network • XCT used to segment and extract pore network ❖Algorithm to remove the vertical stripe image artifact is now developed, but not applied to this data set

2nd Congreso Argentino Técnicas Neutrónicas L.M. Anovitz et al, Abstract #H13F-1442, AGU fall meeting 2016. 4D NeXT of Water Retention in Soils 1 Hour 4 Hour 7 Hour 10 Hour

• Measure the preferential pathways for water removal from sand column • NeXT provides simple segmentation of water, sand, and void (analysis in process)

2nd Congreso Argentino Técnicas Neutrónicas Yan Jin et al, in prep Bragg Edge Imaging

• 푛 휆 = 2 푑 sin(휃) • θ=90° represents the maximum λ that this crystal plane can scatter • This causes a sharp drop in scattering called a Bragg edge • Use to measure strain or distribution of crystal phases

2nd Congreso Argentino Técnicas Neutrónicas R. Woracek et al, Advanced Materials (2014). TRIPP Steel

• With applied strain, TRIPP steels undergo phase transformations from Martensite to Austenite • Surface EBSD maps can be used to calculate the “volume” fraction of ferrite (α), martensite (α′), and austenite (γ) each phase as a function of strain

2nd Congreso Argentino Técnicas Neutrónicas Wanchuck Woo et al, Scripta Materialia 158 (2019) 105–109 TRIPP Steel Volume Fractions vs. Strain ferrite (α), martensite (α′), and austenite (γ)

Neutron Bragg Edge Imaging and Diffraction volume fractions used to correct surface sensitive EBSD Bragg Edge Imaging and neutron diffraction (not measurements shown) provide contrary results for the volume fraction compared to EBSD ➢ Bulk probes are important!! 2nd Congreso Argentino Técnicas Neutrónicas Wanchuck Woo et al, Scripta Materialia 158 (2019) 105–109 Hydrogen Embrittlement with Bragg Edge Imaging

H2 environment Air environment

+2500 µε -2500 µε

Strain field (εzz) maps over the specimen face for the same load (P=5150 N) in hydrogen (left) and in air (right). NIST in situ hydrogen charging/fatigue rig 2nd Congreso Argentino Técnicas Neutrónicas M. Connolloy et al, in prep Dark Field Imaging : Spatially Resolved SANS

Mesh

Dark field (loss of amplitude) measures the correlation function:

Autocorrelation Length: ξ = Z λ / Pd = Z λ D / Pg L γ( ξ ) = 1 - 흁흃 / 흁∞ Open 흁흃t = -ln(AS(ξ) / AEmpty)

Build

Mesh Microspheres Raw images as ξ varied in water by changing D Pushin et al, PRA (2017) & Sarenac et al, PRL (2018) Dark field of microspheres; solid line is 2nd Congreso Argentino Técnicas Neutrónicas expected from SANS data



1.07 μm 1.07 0.96 μm 0.96 Additively Manufacture Tensile Test at 50% Lifetime



1.07 μm 1.07

0.84 μm 0.84

0.96 μm 0.96 0.72 μm 0.72

➢ Stress changes pore structure,

build up of porosity at 840 nm in μm 0.84 the middle indicates failure point ➢ From the series of ξ-points, we extract the pore size and volume

fraction changes with applied μm 0.72 fatigue across the sample

2nd Congreso Argentino Técnicas Neutrónicas Brooks et al, Materials and Design 140 (2018) Conclusions

• Neutron imaging provides a unique view into materials and systems • Neutron and X-ray Tomography is a powerful tool to understand the composition of a complex sample • Bragg edge imaging has the promised to measure strains and crystalline phase distributions, maybe even in 3D • Dark-field imaging is an emerging technique that might be a valuable tool for additive manufacturing and geological studies

2nd Congreso Argentino Técnicas Neutrónicas The NIST Neutron Imaging Team (some old photos … )

Muhammad Arif David Jacobson Elias Baltic Daniel Hussey Elias Baltic

Jacob LaManna

Thanks for your attention. Questions??

2nd Congreso Argentino Técnicas Neutrónicas