Preparation of Stainless Steel Surfaces for Scanning Probe Microscopy

Warren, Alexander; Martinez-Ubeda, Ana I.; Payton, Oliver D; Picco, Loren; Scott, Tom

doi:10.1017/s1551929516000341

Cited by 18 publications

(26 citation statements)

References 7 publications

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“…Following the specimen preparation described by Warren et al [15], the surface was imaged under a droplet of demineralised water. The mosaic shown in Figure 7 was captured in 10 seconds, and represents an imaging resolution comparable to transmission electron microscopy (TEM).…”

Section: Resultsmentioning

confidence: 99%

“…Offcuts of un-irradiated fuel cladding, made of 20Cr-25Ni-Nb stabilised stainless steel, were cut as C-rings from a tube with a diameter of approximately 1.5 cm. A schematic in Figure shows the processes involved in making the c-rings, following the ASTM standard [15]. Cring specimens were first annealed for 30 minutes at 1150 °C (followed by quenching in water) and then aged for 50 hours at 600 °C, both steps in flowing argon.…”

Section: Cr-25ni-nb Stabilised Stainless Steelmentioning

confidence: 99%

“…Some of the C-rings were mounted in a non-conductive resin and an electrical connection was established on the curved side of the C-ring, with a bolted connection to a PTFE insulated wire. The cross sections (perpendicular to the extrusion direction) were prepared according to Warren et al [15]. The quality of the surface finish is crucial in obtaining high resolution HS-AFM scans and particular care was given to the removal of polishing debris from the scratch-free surface.…”

Section: Cr-25ni-nb Stabilised Stainless Steelmentioning

confidence: 99%

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In situ imaging of corrosion processes in nuclear fuel cladding

Laferrere

Burrows

Glover

et al. 2017

Corrosion Engineering, Science and Technology

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In-Situ Imaging of Corrosion Processes in Nuclear Fuel Cladding Spent nuclear fuel in the UK is stored within ponds dosed with NaOH in order to inhibit corrosion and, to ensure the efficiency of storage regimes, there is a need to define and quantify the corrosion processes involved during immersion of fuel cladding. In this project, state-of-the-art characterisation techniques were employed to image the corroding surfaces of two nuclear fuel cladding materials: stainless steel and Magnox. Advanced gas-cooled reactor (AGR) fuel cladding consists of 20Cr-25Ni-Nb stabilised stainless steel and during irradiation the microstructure of the cladding undergoes significant changes, including grain boundary element depletion and segregation. Highspeed atomic force microscopy (HS-AFM) with nanoscale resolution, enabled precipitates and pit initiation in stainless steel to be imaged. Magnox is a magnesiumaluminium alloy and during irradiation in a reactor the outer metal surface oxidises, forming an adherent passive layer which subsequently hydrates when exposed to water. Corrosion processes encompass breakdown of passivity and filiform-like corrosion, both of which were imaged in-situ using the scanning vibrating electrode technique (SVET).

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Section: Resultsmentioning

confidence: 99%

Section: Cr-25ni-nb Stabilised Stainless Steelmentioning

confidence: 99%

Section: Cr-25ni-nb Stabilised Stainless Steelmentioning

confidence: 99%

See 1 more Smart Citation

In situ imaging of corrosion processes in nuclear fuel cladding

Laferrere

Burrows

Glover

et al. 2017

Corrosion Engineering, Science and Technology

Self Cite

View full text Add to dashboard Cite

show abstract

“…The samples were annealed at 1050 o C for thirty minutes and cooled in air (giving a resultant proof stress of approximately 290 MPa). Preparation of the sample surface is critical for quantitative measurement from the HS-AFM and a suitable surface finish was achieved on the tensile face of the beam following the method outlined by Warren et al [16].…”

Section: Materials and Sample Preparationmentioning

confidence: 99%

Development of Fatigue Testing System for in-situ Observation by AFM & SEM

et al. 2019

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A three-point bend fatigue miniature stage for in-situ observation of fatigue microcrack initiation and growth behaviour by scanning electron microscopy (SEM) and atomic force microscopy (AFM) has been manufactured. Details of the stage design with finite element analysis of the stress profiles on loading are provided. The proposed stage facilitates study of the micro mechanisms of fatigue when used during SEM and AFM scanning of the sample surface. To demonstrate the applicability of the system, fatigue tests have been performed on annealed AISI Type 316 stainless steel. Surface topography images obtained by SEM and HS-AFM (High Speed AFM) are presented for comparison. The data can be used to validate crystal plasticity models which should then directly predict multiaxial behaviour without recourse to deformation rules such as equivalent stress or strain.

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“…28 The sample surface was initially polished using progressively ner grades of silicon carbide (SiC) grit paper, from P600 up to P4000, using water as lubricant. The sample was then polished using 3 mm to 0.25 mm diamond paste (Kemet International Ltd., KD Diamond Pastes), using a Struers™ DP-Lubricant (Brown).…”

Section: Materials and Sample Preparationmentioning

confidence: 99%

A study of dynamic nanoscale corrosion initiation events using HS-AFM

et al. 2018

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Atomic force microscopes (AFMs) are capable of high-resolution mapping of structures and the measurement of mechanical properties on nanometre scales within gaseous, liquid and vacuum environments. The contact mode high-speed AFM (HS-AFM) developed at Bristol Nano Dynamics Ltd. operates at speeds that are orders of magnitude faster than conventional AFMs, and is capable of capturing multiple frames per second. This allows for direct observation of dynamic events in real-time, with nanometre lateral resolution and subatomic height resolution. HS-AFM is a valuable tool for the imaging of nanoscale corrosion initiation events, such as metastable pitting, grain boundary (GB) dissolution and short crack formation during stress corrosion cracking (SCC). Within this study HS-AFM was combined with SEM and FIB milling to produce a multifaceted picture of localised corrosion events occurring on thermally sensitised AISI 304 stainless steel in an aqueous solution of 1% sodium chloride (NaCl).HS-AFM measurements were performed in situ by imaging within a custom built liquid cell with parallel electrochemical control. The high resolution of the HS-AFM allowed for measurements to be performed at individual reaction sites, i.e. at specific GB carbide surfaces. Topographic maps of the sample surface allowed for accurate measurements of the dimensions of pits formed. Using these measurements it was possible to calculate, and subsequently model, the volumes of metal reacting with respect to time, and so the current densities and ionic fluxes at work. In this manner, the local electrochemistry at nanoscale reaction sites may be reconstructed.

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Preparation of Stainless Steel Surfaces for Scanning Probe Microscopy

Cited by 18 publications

References 7 publications

In situ imaging of corrosion processes in nuclear fuel cladding

In situ imaging of corrosion processes in nuclear fuel cladding

Development of Fatigue Testing System for in-situ Observation by AFM & SEM

A study of dynamic nanoscale corrosion initiation events using HS-AFM

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