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In Situ Quantification of a Wetted Surface Area during Scanning Electrochemical Cell Microscopy Using Retraction Curves

2024· article· en· W4403136443 on OpenAlex
Nishtha Saxena, Emmanuel Mena‐Morcillo, Mia Tripp, Peter Keech, Mehran Behazin, Samantha Michelle Gateman

Why this work is in the frame

A frame that forgets how it found something cannot be audited. These are the routes that admitted this work.

affAt least one author lists a Canadian institution in the pinned OpenAlex snapshot.
fundA Canadian funder is recorded on the work.

Bibliographic record

VenueACS Measurement Science Au · 2024
Typearticle
Languageen
FieldChemistry
TopicElectrochemical Analysis and Applications
Canadian institutionsNuclear Waste Management OrganizationWestern University
FundersNatural Sciences and Engineering Research Council of CanadaNuclear Waste Management Organization
KeywordsIn situMaterials scienceMicroscopyScanning ion-conductance microscopyScanning electrochemical microscopyElectrochemistryBiomedical engineeringAnalytical Chemistry (journal)Scanning electron microscopeChemistryScanning confocal electron microscopyElectrodeComposite materialChromatographyOpticsMedicinePhysics

Abstract

fetched live from OpenAlex

High Resolution Image Download MS PowerPoint Slide This work presents a new methodology to estimate the surface area of the working electrode during scanning electrochemical cell microscopy (SECCM) in situ by utilizing retraction curves. In this approach, the current is measured as a function of pipet displacement in the z -direction. When the current drops to zero, it is indicative of droplet detachment from the surface, allowing for the estimation of the droplet contact diameter based on the pipet displacement. This enables real-time estimations of surface areas of the wetted electrode at each point of measurement, rather than performing time-consuming measurements using ex situ correlative image analysis or estimating an average working electrode size from the pipet aperture. Notably, during SECCM measurements on copper in nitric acid, the working electrode diameter estimated using retraction curves was significantly smaller than the droplet footprint diameter observed post experiment using ex situ correlative image analysis. This discrepancy is attributed to droplet spreading after pipet retraction, as confirmed by goniometer and silanized pipet measurements. Upon cleaning the surface, the true wetted surface areas during SECCM measurements were found to be in good agreement with values estimated using retraction curves yet were larger than the pipet aperture. Additionally, the effects of approach separation, retraction rates, and probe diameter on the droplet contact size were analyzed using retraction curves. These findings were compared to ex situ methods to assess the reliability of the retraction curves for determining the working electrode surface area. This study demonstrates the potential of retraction curves to provide a higher accuracy in the quantitative analysis of local current density values extracted using SECCM.

Fetched live from OpenAlex and de-inverted. Abstracts are not stored in this database: the inverted indexes are 8.6 GB of the frame’s 9.3 GB of text, and the host has 13 GB free.

Direct model labels (unvalidated)

Per-model category and study-design labels from the labeling rounds. They are machine output, unvalidated, and the disagreement between models ships as data. No study design here is MEDLINE-validated yet.

Model armCategoriesStudy designConfidence
gemmano category
Domain: not available · Genre: Empirical
About the Canadian research system: no · About a Canadian topic: no
Bench or experimentalhigh
gptno category
Domain: not available · Genre: Empirical
About the Canadian research system: no · About a Canadian topic: no
Bench or experimentalhigh
models agreeAgreement compares identical category sets and study designs across arms.

Full frame distilled prediction

Teacher imitation

Not calibrated prevalence, not ground truth. Human validation pending. Learned from the 10,348 direct Codex labels and 10,348 direct Gemma labels. Candidate is the union of thresholded teacher heads; consensus is their intersection. These outputs are machine_predicted_unvalidated and are not human labels or direct frontier model labels.

metaresearch head score (Codex)0.001
metaresearch head score (Gemma)0.000
Version: codex-gemma-dda1882f352aValidation status: machine_predicted_unvalidated
Candidate categoriesnone
Consensus categoriesnone
DomainCandidate signal: none · Consensus signal: none
Study designCandidate signal: Bench or experimental · Consensus signal: Bench or experimental
GenreCandidate signal: Empirical · Consensus signal: Empirical
Teacher disagreement score0.003
Threshold uncertainty score0.501

Codex and Gemma teacher scores by category

CategoryCodexGemma
Metaresearch0.0010.000
Meta-epidemiology (narrow)0.0000.000
Meta-epidemiology (broad)0.0000.000
Bibliometrics0.0000.002
Science and technology studies0.0000.000
Scholarly communication0.0000.000
Open science0.0000.000
Research integrity0.0000.000
Insufficient payload (model declined to judge)0.0000.000

Machine scores (provisional)

The two teacher heads of the student model, read on this work. A score orders the frame for review; it never asserts a category, and the validation status ships verbatim with every row.

Baseline scores from an immature model (maturity gate not passed, 7 training rounds). Scores rank; they never assert a category.

Opus teacher head0.039
GPT teacher head0.299
Teacher spread0.260 · how far apart the two teachers sit on this one work
Validation statusscore_only:v0-immature-baseline · verbatim from the scoring run: score_only means the number may rank works, and no category label ships from it