BASTARDO-FERNÁNDEZ I., CHEKRI R., NOIREAUX J., GIVELET L., LAMBENG N., DELVALLÉE A., LOESCHNER K., FISICARO P. and JITARU P., "Characterisation of titanium dioxide (nano)particles in foodstuffs and E171 additives by single particle inductively coupled plasma-tandem mass spectrometry using a highly efficient sample introduction system", Food Additives & Contaminants: Part A, 2024, 41, 8, 867‑884, DOI: 10.1080/19440049.2024.2359532.

CROUZIER L., FELTIN N. and JABLON B., "A new metrology tool: using transmission Kikuchi diffraction (TKD) to identify and separate nanoparticles for regulatory purposes", Measurement Science and Technology, 2025, 36, 1, 015038, DOI: 10.1088/1361-6501/ad93ee.

FELTIN N., DELVALLÉE A. and CROUZIER L., "Strategy for Ensuring the Metrological Traceability of Nanoparticle Size Measurements by SEM", Nanomaterials, 2024, 14, 11, 931, DOI: 10.3390/nano14110931.

ENNIAFA M., KAFTANDJIAN V., OBATON A-F., and BRZUCHACZ S., "Configuration of the surface determination parameters for dimensional measurements with/using helpful metric as visualisation tool", e-Journal of Nondestructive Testing, 2024, 29, 3, DOI: 10.58286/29281.

GUILLORY J., BASELGA S., WALLERAND J-P., TRUONG D., GARCÍA-ASENJO L., LUJÁN R., PESCE D., WEYER B., FUCHS J-F. and MISSIAEN D., "Comparison between a Two-Wavelength Absolute Distance Meter and a GNSS-Based Distance Meter at CERN Geodetic Network", Journal of Surveying Engineering, 2025, 151, 1, 04024014, DOI: 10.1061/JSUED2.SUENG-1523.

GUILLORY J., TRUONG D., WALLERAND J-P. and ALEXANDRE C., "A sub-millimetre two-wavelength EDM that compensates the air refractive index: uncertainty and measurements up to 5 km", Measurement Science and Technology, 2024, 35, 2, 025024, DOI: 10.1088/1361-6501/ad0a22.

OBATON A-F., "About Osseointegration Evaluation Criteria", Orthopedics and Rheumatology Open Access Journal, 2024, 23, 1, DOI: 10.19080/OROAJ.2024.23.556104.

OBATON A-F., FAIN J., MEINEL D., TSAMOS A., LÉONARD F., LÉCUELLE B., DJEMAÏ M. and BRUNO G., "Investigation of a New Ti Alloy for a New Generation of Additively Manufactured Implants with Lattice", Contemporary Perspective on Science, Technology and Research Vol. 7, B P International, 2024. p. 12‑37. ISBN 978-81-971391-8-5.

OBATON A-F., FALLAHI N., TANICH A., LAFON L-F. and WEAVER G., "Statistical Analysis and Automation Through Machine Learning of Resonant Ultrasound Spectroscopy Data from Tests Performed on Complex Additively Manufactured Parts", Journal of Nondestructive Evaluation, 2024, 43, 1, 21, DOI: 10.1007/s10921-023-01035-8.

OBATON A-F., TANICH A., FISCHER N., ANTONA S., MONTAGNER F., GENOT S., BRZUCHACZ S., SOETE PD., DUBOEUF K., BEUVIER T., NANJAREDDY R., COUTANT N., COCHENNEC N. and GAY L., "Accuracy of XCT to Perform Dimensional Measurements on Different Measurands", Science and Technology: Developments and Applications Vol. 1, BP International, 2024. p. 22‑61. ISBN 978-93-48859-70-9.

OMPALA C., RENAULT J-P., TACHÉ O., COURNÈDE É., DEVINEAU S. and CHIVAS-JOLY C., "Stability and dispersibility of microplastics in experimental exposure medium and their dimensional characterization by SMLS, SAXS, Raman microscopy, and SEM", Journal of Hazardous Materials, 2024, 469, 134083, DOI: 10.1016/j.jhazmat.2024.134083.

RIBOTTA L., DELVALLÉE A., CARA E., BELLOTTI R., GIURA A., CARLO ID., FRETTO M., KNULST W., KOOPS R., TORRE B., SAGHI Z. et BOARINO L., "AFM interlaboratory comparison for nanodimensional metrology on silicon nanowires", Measurement Science and Technology, 2024, 35, 10, 105014, DOI: 10.1088/1361-6501/ad5e9f.

SENTIS M.P.L., FELTIN N., LAMBENG N., LEMAHIEU G., BRAMBILLA G., MEUNIER G. and CHIVAS-JOLY C., "Investigation of nanoparticle dispersibility and stability based on TiO2 analysis by SMLS, DLS, and SEM", Journal of Nanoparticle Research, 2024, 26, 3, 55, DOI: 10.1007/s11051-024-05959-8.

XU J., REFINO AD., DELVALLÉE A., SEIBERT S., SCHWALB C., HANSEN PE., FOLDYNA M., SIAUDINYTE L., HAMDANA G., WASISTO HS., KOTTMEIER J., DIETZEL A., WEIMANN T., PRÜSSING JK., BRACHT H. and PEINER E., "Deep-reactive ion etching of silicon nanowire arrays at cryogenic temperatures", Applied Physics Reviews, 2024, 11, 2, 021411, DOI: 10.1063/5.0166284.

OBATON A-F., FERRUCCI M., GIERA B., HARRIS A. and HASLAM J., "Benefit of X-ray imaging to improve additive manufacturing", Electronic imaging 2024, San Francisco (Etats-Unis), 21 January 2024.

ENNIAFA M., KAFTANDJIAN-DOUDET V., OBATON A-F. and BRZUCHACZ S., "XCT parametric study on the influence of acquisition setup and tweaking of surface determination on the dimensional measurement with helpful metric as visualization tool", ICT2024, Wels (Autriche), 6 February 2024.

GUILLORY J., "Multilateration-based coordinate measurement system", NPL workshop “Celebrating Science”, Teddington (Royaume-Uni), 28 February 2024.

CHIBANE L., DELVALLÉE A., FLEURENCE N., MORAN J., FLAHAUT E. and FELTIN N., "Correlative imaging of single graphene oxide flake: sample selection and limitations", E-MRS Spring Meeting 2024 – Symposium L: ALTECH 2024, Graz (Autriche), 27 May 2024.

CHIBANE L., DELVALLÉE A., FLEURENCE N., MORAN J., FLAHAUT E. and FELTIN N., "Correlative imaging of single graphene oxide flake: sample selection and limitations", Summer School ELENAM, Fréjus (France), 3 June 2024.

OBATON A-F., "Image quality and standardization", 9th CIA‐CT Conference, Lyngby (Danemark), 4 June 2024.

OBATON A-F., "High-performance non-destructive techniques for quality assurance of complex-geometry additively manufactured parts", AM conference, Berlin (Allemagne), 12 June 2024.

RIBOTTA L. and DELVALLÉE A., "Silicon nanowires: fabrication and quantitative dimensional characterisation by AFM", NanoInnovation Rome, Rome (Italie), 9 September 2024.

ALASONATI E., CHIVAS-JOLY C., FELTIN N., LALÈRE B., ALTMANN K., WIESNER Y. and GIOVANNOZZI AM., "From Qualitative to Quantitative Measurement of Small Microplastics Using Multi-Detector Field Flow Fractionation Coupled Offline to Microscopy and Raman Spectroscopy", Conférence internationale MICRO 2024, Lanzarote (Espagne), 23 septembre 2024.

CHIVAS-JOLY C., OMPALA C., RENAULT J-P., TACHE O., COURNED E. and DEVINEAU S., "Stability and dispersibility of microplastics in experimental exposure medium and detection of nanoplastic fractions by SMLS, SAXS, Raman microscopy, and SEM", Conférence internationale MICRO 2024, Lanzarote (Espagne), 23 septembre 2024.

SARGEANT B., ROBSON S., RICHARDS C., PUERTO P., GARCIA BERDOTE A., LEIZEA I., GUILLORY J., TRUONG D., WALLERAND J-P., GOUTTEFARDE M., HERVÉ P-E., HEISSELMANN D., POLLINGER F., RAFELD E., FRANKE M. and GEVA K., "Photogrammetry in the DynaMITE Project", 3D Metrology Conference, Loughborough (Royaume-Uni), 24 September 2024.

GUILLORY J., TRUONG D., WALLERAND J-P., SARGEANT B., RICHARDS C., ROBSON S., GARCIA BERDOTE A., PUERTO P., HERVÉ P-E. and GOUTTEFARDE M., "Positioning a cable-driven parallel robot at better than 0.25 mm using a multilateration system assisted by photogrammetry", 3D Metrology Conference, Loughborough (Royaume-Uni), 24 September 2024.

DELALANDE Y., DUCOURTIEUX S., DURAND S., GUILLORY J., LESTRADE A., SEBDAOUI M., LELUAN B. and BOURGOIN C., "Modelling and optimisation of SOLEIL II survey and uncertainty assessment of the measurement process using Monte Carlo approach", International Workshop on Accelerator Alignment, Californie (Etats-Unis), 7 October 2024.

GUILLORY J., WALLERAND J-P., TRUONG D., BASELGA S., GARCÍA-ASENJO L., LUJÁN R., WEZKA K., PRÓCHNIEWICZ D., WISNIEWSKI M., WEYER B., FUCHS J-F. and MISSIAEN D., "Sub-millimetric field measurements over kilometres using Arpent two-wavelength ADM", International Workshop on Accelerator Alignment, Californie (Etats-Unis), 7 October 2024.

CHIBANE L., DELVALLÉE A., FLEURENCE N., MORAN J., FLAHAUT E. and FELTIN N., "Métrologie corrélative pour l’étude des propriétés physico-chimiques de l’oxyde de graphène au cours de sa réduction", Journée des doctorants de l’ED Toulouse, Toulouse (France), November 2024.

SILVESTRI Z., "Planned comparisons on the MQB-Pascal project", MQB-Pascal Workshop 2024, Berlin (Allemagne), 27 November 2024.

OBATON A-F., "X-ray computed tomography (XCT) and resonant ultrasound spectroscopy (RUS) techniques for quality inspection of additively manufactured parts", WSE3DPAM, Prague (République Tchèque), 2 December 2024.

GUILLORY J., "Télémétrie laser et applications en robotique et en géodésie", Photonics Excellence Day 2024, Orsay (France), 5 December 2024.

This thesis work deals with the development and characterization of a single-cavity Fabry-Perot refractometer operating at 532 nm, designed to measure the pressure of pure gases between 100 Pa and 100 kPa. The aim of this new instrument is to improve on the best current measurement capabilities obtained in France by conventional methods based on the measurement of a force applied to a surface. First, the fundamental principles of refractometry are reviewed, detailing the relationships between the refractivity of a pure gas, its molar density and its thermodynamic pressure. The values of gas density and refractivity virial coefficients and their uncertainties have been extrapolated to the working wavelength and temperature of the refractometer developed at LNE-Cnam. After a detailed description of the Fabry-Perot cavity, measurements of its intrinsic parameters and their uncertainties (coefficient of thermal expansion, pressure-induced distortion coefficient, long-term drift and free spectral range) are presented. They make it possible to correct pressure measurement errors due to cavity deformations during the measurement procedure. Methods for controlling millikelvin temperature, stabilizing the gas pressure as well as limiting the thermal effects of gas expansion and compression are described. A metrological characterization of the instrument makes it possible to establish a complete uncertainty budget, and to identify the improvements needed to reach the level of uncertainty of the national references around atmospheric pressure and exceed them for lower pressures. Measurement reproducibility is assessed at 2.7 ppm. A comparison with a PG7607 reference pressure balance between 30 kPa and 100 kPa shows a relative deviation of less than 8 ppm, which is lower than the best current uncertainties. Finally, this thesis explores an innovative application of refractometry for measuring acoustic pressure in the infrasound range, enabling continuity between static and acoustic pressure measurements which is still missing nowadays.

refractivity, Fabry-Perot interferometer, Virial coefficient, Pressure metrology, thermodynamics, opto-acoustic sensor

PhD Thesis (FR) : https://theses.hal.science/tel-04352332v1/file/CNAM_REZKI_2023.pdf

The laser powder bed fusion (PBF-LB) use is increasing in the industry, but a lack of understanding remain on some aspects, which limits its development. This is the case for the dimensional and geometric properties of the parts produced by this process, which can display significant deviations from the numerical model. Thus, the aim of this work is to improve the understanding of the mechanisms behind dimensional and geometric deviations. Following a literature review which identified the main causes of these deviations and the most influential process parameters, it was decided to study the dimensional and geometric aspects at different scales. An initial study was carried out on the scale of the melt bead, which enabled us to gain a better understanding of the ranges of parameters that allow for healthy construction. This study also enabled the determination of the variations in bead morphology as a function of the process parameters used. The second study at part scale illustrated the impact of bead geometry and surface roughness on dimensional deviations. The geometric deviations are influenced by the surface roughness, and by the distortions due to residual stresses, which were specifically studied afterwards. The role of the process parameters laser power and scanning speed was also assessed, revealing a less significant influence than expected compared to the influence of the chosen geometry. Finally, attention was paid to lattice structures, the study of which revealed the importance of orientation as well as the difficulty of evaluating the geometry.

metrology, additive manufacturing, dimensional, powder bed fusion, metal, geometry

Full document (FR) : HAL-04271836

AL-MESLEMI Y., FERREIRA K., MEHDI-SOUZANI C., OBATON A-F., NOUIRA H. et ANWER N., "Quality Control for Additive Manufacturing", PEI, E. et al.Éd. Springer Handbook of Additive Manufacturing, Cham: Springer International Publishing, 2023. p. 797‑819. ISBN 978-3-031-20751-8, DOI: 10.1007/978-3-031-20752-5_47>

BU T., GAO H., YAO Y., WANG J., POLLARD AJ., LEGGE EJ., CLIFFORD CA., DELVALLÉE A., DUCOURTIEUX S., LAWN MA., BABIC B., COLEMAN VA., JÄMTING Å., ZOU S., CHEN M., JAKUBEK ZJ., IACOB E., CHANTHAWONG N., MONGKOLSUTTIRAT K., ZENG G., ALMEIDA CM., HE B-C., HYDE L. et REN L., "Thickness measurements of graphene oxide flakes using atomic force microscopy: results of an international interlaboratory comparison", Nanotechnology, 34, 22, 2023, 225702, DOI: 10.1088/1361-6528/acbf58.

CARCREFF E., LAROCHE N. et OBATON A-F., "Review of Ultrasonic Testing for Metallic Additively Manufactured Parts", SEIFI, M. et al.Éd. Additive Manufacturing Design and Applications, [s.l.]: ASM International, 2023. p. 310‑323. ISBN 978-1-62708-439-0

CHAPPLE R., CHIVAS-JOLY C., ROUX J-C., DUMAZERT L., FERRY L., LOPEZ-CUESTA J-M., ERSKINE EL. et KANDOLA BK., "Characterization of aerosolized particles in effluents from carbon fibre composites incorporating nanomaterials during simultaneous fire and impact", NanoImpact, 29, 2023, 100446, DOI: 10.1016/j.impact.2022.100446.

COFREND C., Fabrication additive, description et comparaison des principaux procédés de FA métallique et composite: Tome 2, [s.l.]: Lexitis, 2024. ISBN 978-2-36233-194-7

EVARISTE L., LAMAS B., ELLERO-SIMATOS S., KHOURY L., CARTIER C., GAULTIER E., CHASSAING B., FELTIN N., DEVOILLE L., FAVRE G., AUDEBERT M. et HOUDEAU E., "A 90-day oral exposure to food-grade gold at relevant human doses impacts the gut microbiota and the local immune system in a sex-dependent manner in mice", Particle and Fibre Toxicology, 20, 1, 2023, 27, DOI: 10.1186/s12989-023-00539-5.

FELTIN N., CROUZIER L., DELVALLÉE A., PELLEGRINO F., MAURINO V., BARTCZAK D., GOENAGA-INFANTE H., TACHÉ O., MARGUET S., TESTARD F., ARTOUS S., SAINT-ANTONIN F., SALZMANN C., DEUMER J., GOLLWITZER C., KOOPS R., SEBAÏHI N., FONTANGES R., NEUWIRTH M., BERGMANN D., HÜSER D., KLEIN T. et HODOROABA V-D., "Metrological Protocols for Reaching Reliable and SI-Traceable Size Results for Multi-Modal and Complexly Shaped Reference Nanoparticles", Nanomaterials, 13, 6, 2023, 993, DOI: 10.3390/nano13060993.

FOURNET-FAYARD L., CAYRON C., KOUTIRI I., LAPOUGE P., GUY J., DUPUY C. et OBATON A-F., "Thermal analysis of parts produced by L-PBF and correlation with dimensional accuracy", Welding in the World, 67, 4, 2023, 845‑858, DOI: 10.1007/s40194-022-01452-9.

GUILLORY J., TRUONG D., WALLERAND J-P. et ALEXANDRE C., "A sub-millimetre two-wavelength EDM that compensates the air refractive index: uncertainty and measurements up to 5 km", Measurement Science and Technology, 35, 2, 2024 (published: 16 Nov. 2023), 025024, DOI: 10.1088/1361-6501/ad0a22.

GUILLORY J., TRUONG D., WALLERAND J-P., LÖSLER M., ESCHELBACH C., MÄHLER S. et KLÜGEL T., "Determination of the reference point of a radio telescope using a multilateration-based coordinate measurement prototype", Precision Engineering, 83, 2023, 69‑81, DOI: 10.1016/j.precisioneng.2023.05.007.

GUILLORY J., TRUONG D., WALLERAND J-P., SVANTESSON C-G., HERBERTSSON M. et BERGSTRAND S., "An SI-traceable multilateration coordinate measurement system with half the uncertainty of a laser tracker", Measurement Science and Technology, 34, 6, 2023, 065016, DOI: 10.1088/1361-6501/acc26a.

LÖSLER M., ESCHELBACH C., MÄHLER S., GUILLORY J., TRUONG D. et WALLERAND J-P., "Operator-software impact in local tie networks: Case study at Geodetic Observatory Wettzell", Applied Geomatics, 15, 1, 2023, 77‑95, DOI: 10.1007/s12518-022-00477-5.

MIMOUNE K., GUILLORY J. et PLIMMER M., "Acoustic thermometer operating up to 11 m: uncertainty assessment and new values for Cramer coefficients around 40 kHz", International Journal of Metrology and Quality Engineering, 14, 2023, 13, DOI: 10.1051/ijmqe/2023011.

OBATON A-F., "Resonant Ultrasound Spectroscopy Testing Methods in Additive Manufacturing", SEIFI, M. et al.Éd. Additive Manufacturing Design and Applications, [s.l.]: ASM International, 2023. p. 333‑344. ISBN 978-1-62708-439-0.

OBATON A-F., FAIN J., MEINEL D., TSAMOS A., LÉONARD F., LECUELLE B. et DJEMAÏ M., “In Vivo Bone Progression in and around Lattice Implants Additively Manufactured with a New Titanium Alloy”, Applied Sciences, 13, 2023, 7282, DOI : 10.3390/app13127282.

OBATON A-F., GAILLARD Y.,BOUVET P., NOVITOM, GUIRAUD O., NIKON, GENOT S., et GAY L., "Evaluation of XCT image quality", e-Journal of Nondestructive Testing, 28, 3, 2023, DOI: 10.58286/27712.

OBATON A-F., KOCH D., COLINE J., et FLOTTÉ D., "Tomosynthesis for large additive manufacturing parts", Research and Review Journal of Nondestructive Testing, 1, 1, 2023, DOI: 10.58286/28193.

OBATON A-F., TANICH A., FISCHER N., ANTONA S., MONTAGNER F., GENOT S., BRZUCHACZ S., SOETE PD., DUBOEUF K., BEUVIER T., NANJAREDDY R., COUTANT N., COCHENNEC N. et GAY L., "Dimensional XCT comparison campaign on an aluminium object", Measurement Science and Technology, 34, 9, 2023, 094004, DOI: 10.1088/1361-6501/acd8dd.

POLLINGER F., BASELGA S., COURDE C., ESCHELBACH C., GARCÍA-ASENJO L., GARRIGUES P., GUILLORY J., HEDEKVIST PO., HELOJÄRVI T., JOKELA J., KALLIO U., KLÜGEL T., KÖCHERT P., LÖSLER M., LUJÁN R., MEYER T., NEYEZHMAKOV P., PESCE D., PISANI M., POUTANEN M., PRELLINGER G., SAUTHOFF A., SEPPÄ J., TRUONG D., UNDERWOOD R., WEZKA K., WALLERAND J-P. et WIŚNIEWSKI M., "The European GeoMetre project: developing enhanced large-scale dimensional metrology for geodesy", Applied Geomatics, 15, 2, 2023, 371‑381, DOI: 10.1007/s12518-022-00487-3.

PRANIEWICZ M., FOURNET-FAYARD L., FOX JC., CAYRON C., KOUTIRI I. et OBATON A-F., "Bearing area curve based partitioning for the verification of theoretical supplemental geometry on additively manufactured lattice structures", Additive Manufacturing, 68, 2023, 103521, DOI: 10.1016/j.addma.2023.103521.

VIGNARD J., PETTES-DULER A., GAULTIER E., CARTIER C., WEINGARTEN L., BIESEMEIER A., TAUBITZ T., PINTON P., BEBEACUA C., DEVOILLE L., DUPUY J., BOUTET-ROBINET E., FELTIN N., OSWALD IP., PIERRE FH., LAMAS B., MIREY G. et HOUDEAU E., "Food-grade titanium dioxide translocates across the buccal mucosa in pigs and induces genotoxicity in an in vitro model of human oral epithelium", Nanotoxicology, 17, 4, 2023, 289‑309, DOI: 10.1080/17435390.2023.2210664.

OBATON A-F., GAILLARD Y., BOUVET P., GUIRAUD O., GENOT S. et GAY L., "Evaluation of XCT image quality", 12th Conference on Industrial Computed Tomography, Furth, Allemagne, 27 février-2 mars 2023.

ENNIAFA M., KAFTANDJIAN V., OBATON A-F. et BRZUCHACZ S., "Modeling of a measuring chain including a CT system to estimate the dimensional uncertainties of additive manufacturing parts", Congrès International de Métrologie 2023, Lyon, France, 7-10 mars 2023.

FOURNET-FAYARD L., CAYRON C., KOUTIRI I., LAPOUGE P., DUPUY J. et OBATON A-F., "Influence of the thermal gradients on residual stress and distortions for cantilever parts made by L-PBF", Congrès International de Métrologie, Lyon, France, 7-10 mars 2023.

OBATON A-F., "Material and dimensional characterizations of part additively manufactured", Global Industrie 2023, Lyon, France, 7-10 mars 2023.

OBATON A-F., TANICH A., ANTONA S., MONTAGNER F., GENOT S., BRZUCHACZ S., DE SOETE A., BEUVIER T., CHOINET E., RIVET C., SALGADO J., FARGIER E. et GAY L., "Investigation of the dimensional performances of industrial XCT”, International metrology congress", Congrès International de Métrologie, Lyon, France, 7-10 mars 2023.

CHIBANE L., DELVALLÉE A., KAJA K., FLEURENCE N., FLAHAUT E. et FELTIN N., "Correlative imaging of single graphene oxide flake: sample selection and limitations", C’Nano - The Nanoscience Meeting 2023, Poitiers, France, 15-17 mars 2023.

REZKI A., "Status and performance of the Fabry-Perot refractometer developed at LNE-Cnam for pressure measurement", CCM & IMEKO TC16 7th International Conference on Pressure and Vacuum Metrology, Washington, Etats-Unis, 15-19 mai 2023.

OBATON A-F., "Le contrôle non-destructif pour la fabrication additive en normalisation nationale et internationale", École Technologique 2023 – Fabrication Additive, Limoges, France, 12-16 juin 2023.

OBATON A-F., KOCH D., COLINE J. et FLOTTÉ D., "Tomosynthesis for large additive manufacturing parts", European Conference on Non-Destructive Testing, Lisbonne, Portugal, 3-7 juillet 2023.

CAYRON C., OBATON A-F., AMIEL S., LECONTE N., GAY L., VU ANH Q., ZHANG F., TRAORÉ S., RAZAFINTSALAMA F. et BERNIER B., "Contrôle qualité des pièces finies par spectroscopie par résonnance ultrasonore (RUS)", Forum France Additive 2023, Paris Saclay, France, 4-6 juillet 2023.

GUILLORY J., TRUONG D. et WALLERAND J-P., "Multilateration system using glass spheres to determine station positions at better than 50 µm", 3D Metrology Conference, Pays Basque, Espagne, 26-28 septembre 2023.

DELVALLÉE A., XU J., PEINER E. et FELTIN N., "Nanowire dimensional characterization with AFM and SEM: pitch, diameter, height and roundness error measurements", NanoScale 2023, Helsinki, Finlande, 10-12 octobre 2023.

DOURI S., FLEURENCE N., DELVALLÉE A. et GOMES S., "Numerical investigation of the nano-contact heat transfer for SThM probes", NanoScale 2023, Helsinki, Finlande, 10-12 octobre 2023.

DOURI S., FLEURENCE N., DEMEYER S., DELVALLÉE A. et HAY B., "Uncertainty evaluation associated with the measurement of thermal conductivity at the nanoscale", NanoScale 2023, Helsinki, Finlande, 10-12 octobre 2023.

OBATON A-F., FERRUCCI M. et GIERA B., "Quality of additively manufactured parts", ASTM International Conference on AM ICAM 2023, Washington, Etats-Unis, 30 octobre-3 novembre 2023.

CARCREFF E., LAROCHE N. and OBATON A.-F., “Review of ultrasonic testing for metallic additive manufactured parts”, Additive Manufacturing Design and Applications, ASM Handbook, 2022, 24A, ASM International, ISBN: 978-1-62708-437-6, Publisher: ASM International.

CHAPPLE R., KANDOLA B.-K., MYLER P., FERRY L., LOPEZ-CUESTA J.-M. and CHIVAS-JOLY C., “Material Integrity and fate of particulates released from carbon fibre composites containing nanomaterials during simultaneous fire and impact”, Environmental Science: Nano, 2022, 9, 3957-3972, DOI: 10.1039/D2EN00222A.

CHAUVEAU D., BOUVET P., OBATON A.-F., GROSJEAN C., NOËL A., SCANDELLA F. and BOURLET C., « Fabrication additive, état de l'art, normalisation - TOME 1 », Collection Les cahiers techniques Cofrend, 2022, ISBN : 978-2-36233-190-9.

CHIVAS-JOLY C., LONGUET C., POURCHEZ J., LECLERC L., SARRY G. and LOPEZ-CUESTA J-M, “Physicochemical characterization and toxicity of nanowaste after incineration process of PA-6/PP/ZnO or TiO2 nanocomposites”, Environmental Science: Nano, 2022, 9, 12, 4570-4584, DOI: 10.1039/D2EN00630H.

DELVALLÉE A. and DUCOURTIEUX S., « Comparaison de mesures des dimensions caractéristiques de réseaux pour l’étalonnage des AFM et MEB », Techniques de l’ingénieur, 2022, DOI: 10.51257/a-v1-r6741.

EL GHAZOUALI S., VISSIERE A., LAFON L.-F., BOUAZIZI M-L. and NOUIRA H., “Optimised calibration of machine vision system for close range photogrammetry based on machine learning”, Journal of King Saud University - Computer and Information Sciences, 2022, 34, DOI: 10.1016/j.jksuci.2022.06.011.

GUILLORY J., TRUONG D. and WALLERAND J.-P., “Multilateration with Self-Calibration : Uncertainty Assessment, Experimental Measurements and Monte-Carlo Simulations”, MDPI Metrology, 2022, 2, 2, 241-262, DOI: 10.3390/metrology2020015.

OBATON A.-F., « FA : contrôles », Techniques de l’ingénieur, 2022, DOI: 10.51257/a-v2-bm7950.

OBATON A.-F., “Resonant Ultrasound Spectroscopy Testing Methods in Additive Manufacturing”, Additive Manufacturing Design and Applications, ASM Handbook, 2022, 24A, ISBN: 978-1-62708-437-6.

OBATON A.-F., VAN DEN BOSSCHE A., BURNET O., BUTSCH B., ZOUGGARH I., SOULARD F. and JOHNSON W., “Novel or Improved NDE Inspection Capabilities for Additively Manufactured Parts”, Progress in additive manufacturing 2020, 2022, 251-264, 10.1520/STP163720200096.

OBATON AF., WEAVER G., FAYARD L.F., MONTAGNER F., BURNET O. and VAN DEN BOSSCHE A., “Classification of metal PBF-LB parts manufactured with different process parameters using resonant ultrasound spectroscopy”, Welding in the World, 2022, 67, 1091–1103, DOI: 10.1007/s40194-022-01419-w.

POLLINGER F., COURDE C., ESCHELBACH C., GARCÍA-ASENJO L., GUILLORY J., OLOF HEDEKVIST P., KAL-LIO U., KLÜGEL T., NEYEZHMAKOV P., PESCE D., PISANI M., SEPPÄ J., UNDERWOOD R., WEZKA K. and WISNIEWSKI M., “Large-scale dimensional metrology for geodesy - first results from the European GeoMetre Project”, International Association of Geodesy Symposia, Springer, Berlin, Heidelberg, 2022, DOI : 10.1007/1345_2022_168.

OBATON A.-F., QUAGLIOTTI D., YARDIN C., LILTORP K. and DE CHIFFRE L., “Comparison campaign of XCT systems using machined standards representative of additively manufactured parts”, 11th Conference on Industrial Computed Tomography, https://www.ndt.net/article/ctc2022/papers/ICT2022_paper_id207.pdf, Wels, Austria, Vol. id207, 8-11 February 2022.

FLEURENCE N., DELVALLEE A., DOURI S., HAMEURY J. and FELTIN N., “Traceability of thermal conductivity measurements by SThM technique to characterize nanowires”, Forum des microscopistes, Saint-Valery-Sur-Somme, France, 7-13 March 2022.

GUILLORY J., TRUONG D. and WALLERAND J.-P., “Optical distance measurements at two wavelengths with air refractive index compensation”, 5^th Joint International Symposium on Deformation Monitoring (JISDM), DOI: 10.4995/JISDM2022.2022.13786, Valencia, Spain, 6-8 April 2022.

CHAUVEAU D., BOUVET P., OBATON A.-F., GROSJEAN C., NOËL A., SCANDELLA F. and BOURLET C., “Review of additive manufacturing standards and proposal to speed up the development of NDT ISO/ASTM standards”, ICWAM (Remote conference), 8-9 June 2022.

FLOTTE D., CHAUVEAU D., OBATON A.-F., BURNET O., MONTAGNER F., CARRÉ O., ZHANG F., COLIN N., HUILLERY R., MORETTI CARTAILLAC A., HAOUA J., MEYNARD P. and MAHAUT S., “Presentation of the NDT round robin performed by the working group on additive manufacturing at Cofrend”, ICWAM, (Remote conference), 8-9 June 2022.

FOURNET-FAYARD L., CAYRON C., KOUTIRI I., LAPOUGE P., DUPUY C. and OBATON AF., “Thermal analysis of parts produced by L-PBF and correlation with dimensional accuracy”, ICWAM, (Remote conference), 8-9 June 2022.

OBATON A-F., GAILLARD Y., MONTAGNER F., FLOTTÉ D., GENOT S., LAMBERT X., REMACHA C., TERZI S. and GAY L., “XCT qualitative inter-comparison on an additively manufactured part with planned flaws”, ICWAM, (Remote conference), 8-9 June 2022.

OBATON A.-F., TANICH A., ANTONA S., MONTAGNER F., GENOT S., BRZUCHACZ S., DE SOETE P., BEUVIER T., CHOINET E., RIVET C., SALGADO J., FARGIER E. and GAY L., “Dimensional XCT comparison campaign on an aluminium object”, 6^th Dimensional X-ray Computed Tomography conference, Manchester, United-Kingdom 13-16 June 2022.

DELVALLÉE A., CHIBANE L., FLEURENCE N., FLAHAUT E. and FELTIN N., “Correlative imaging of single graphene oxide flake including Raman microscopy technique: sample selection and limitations”, Raman Fest, Paris, France, 15-16 September 2022.

FORSSÉN C., SILANDER I., ZAKRISSON J., AMER E., SZABO D., BOCK T., KUSSICKE A., RUBIN T., MARI D., PASQUALIN S., SILVESTRI Z., BENTOUATI D., AXNER O. and ZELAN M., “Circular comparison of conventional pressure standards using a transportable optical refractometer”, Joint IMEKO TC3, T5, TC16 and TC22 International Conference, DOI: 10.21014/tc16-2022.137, Cavtat-Dubrovnik, Croatia, 11-13 October 2022.

RUBIN T., SILANDER I., FORSSÉN C., ZAKRISSON J., AMER E., SZABO D., BOCK T., KUSSICKE A., GÜNZ C., MARI D., GAVIOSO R.-M., PISANI M., MADONNA RIPA D., SILVESTRI Z., GAMBETTE P., BENTOUATI D., GARBEROGLIO G., LESIUK M., PRZYBYTEK M., JEZIORSKI B., SETINA J., ZELAN M. and AXNER O., “Quantum-based realizations of the pascal’ status and progress of the EMPIR-project: Quantumpascal”, Joint IMEKO TC3, T5, TC16 and TC22 International Conference, DOI: 10.21014/tc16-2022.103, Cavtat-Dubrovnik, Croatia, 11-13 October 2022.

OBATON A-F., FALLAHI N., TANICH A., LAFON L-F. and WEAVER G., “Statistical analysis and automation through machine learning of resonant ultrasound spectroscopy data from tests performed on complex additively manufactured parts”, International  Conference on NDE 4.0, Berlin, Germany, 24-27 October 2022.

FOURNET-FAYARD L., CAYRON C., KOUTIRI I., LAPOUGE P., DUPUY C. and OBATON AF., “Influence of the L-PBF bead dimensions on part dimensional accuracy”, International Conference on Additive Manufacturing, Orlando, USA, 31 Oct. - 4 Nov. 2022.

OBATON (INVITÉE) A-F., WEAVER G., FOURNET FAYARD L., CAYRON C., MONTAGNER F., BURNET O. and VAN DEN BOSSCHE A., “Inconel 625 L-PBF part categorization by process parameters using resonant ultrasound spectroscopy”, International Conference on Additive Manufacturing, Orlando, USA, 31 Oct. - 4 Nov. 2022.

LAFON L.-F., VISSIERE A., MEHDI-SOUZANI C., BOUAZIZI M-L., ANWER N. and NOUIRA H., “Novel boundary rejection step for point cloud registration”, Mathmet 2022 conference, Paris, France, 2-4 November 2022.

LAFON L.-F., VISSIERE A., MEHDI-SOUZANI C., BOUAZIZI M-L., ANWER N. and NOUIRA H., “Optimization Strategy of Camera Calibration for Close Range Photogrammetry”, Proceedings of the 9th International Conference of Asian Society for Precision Engineering and Nanotechnology (ASPEN2022), Singapore, 15-18 November 2022.

TOGUEM TAGNE S-C., VISSIÈRE A., DAMAK M., MEHDI-SOUZANI C., ANWER N. and NOUIRA H., “A Cylindricity Measurement with Nanometric Uncertainty”, Proceedings of the 9th International Conference of Asian Society for Precision Engineering and Nanotechnology (ASPEN2022), Singapore, 15-18 November 2022.

Cylindricity is a geometric specification that describes the three-dimensional shape of a cylindrical element. Its control using commercial machines raises a number of practical issues that limit current measurement capabilities. Indeed, there is currently no measuring instrument capable of generating a three-dimensional mapping of the cylindricity deviation with a nanometric uncertainty. The Laboratoire Commun de Métrologie LNE-CNAM has recently developed a ultra-high accuracy cylindricity measuring machine named NanoCyl. As a primary standard, the NanoCyl aims to improve the current calibration and cylindricity measurement capabilities. In this thesis, a general description of the NanoCyl is provided. Its design is then completed by the development of a new sensor carriage structure including a linear positioning axis with nanometer resolution for docking the target surface. A mathematical and geometrical analysis of the sources of uncertainty leads to the proposal of adjustment strategies to minimize measurement errors. An error separation method based on the Fourier transform is developed in the specific case of commercial machines. The method is then adapted to the NanoCyl architecture and validated experimentally. An optimal cylindricity measurement protocol for measurements with nanometre uncertainty is then described. It allows the identification of all the components of the cylindricity deviation. Experimental studies are conducted on a cylindrical artefact in order to validate the introduced protocol. The results obtained show an achievable measurement uncertainty of the order of 30 nm.

Precision engineering, Dimensional metrology, Error separation methods, Cylindricity

 This thesis describes the development of an acoustic thermometry apparatus to estimate the mean temperature along an optical measurement path and thereby better determine the air refractive index. The measurement principle uses the time-of-flight (TOF) of an ultrasonic wave at 40 kHz. The temperature is extracted from the speed of sound using the Cramer equation which gives acoustic velocity as a function of atmospheric parameters (temperature, pression, humidity and CO2 concentration). Different methods for estimating the TOF were studied for six types of signal (single-frequency or modulated, top-hat, Gaussian and Blackman envelopes), notably intercorrelation, and a calibration procedure with respect to reference thermometers placed at intervals along the path developed. The temperature uncertainty achieved for a 10 m distance is 90 mK.

Thermometry, Acoustics, Metrology, Cross-correlation, Ultrasonics, Refractive index

PhD thesis (French) : https://theses.hal.science/tel-03997959v1/document

This thesis is focused on the investigation and development of a 3D vision system coupled with a robot for contactless 3D scanning on mechanical parts in the aeronautic domain. Unlike probe contact-based coordinate measurement machines, 3D vision systems lead to scan parts in a short time. All these scanning operations, initially performed on simple parts, have recently been extended to complex surfaces while catching the new industrial needs in terms of in-line measurement automation, as specified in the industry of the future (or Industry 4.0). Therefore, the quality assurance of multi-camera scanning systems and their traceability to the SI meter definition represents a challenging objective. The full measurement system combining a camera-projector system and one industrial robot is dedicated to in-line 3D scanning on mechanical large volume parts with complex shapes. The system is designed, developed and assembled in-house in order to ensure a complete traceability chain of the measurement process.One 3D vision system based on the principle of structured light has been developed and calibrated in-house. The calibration of 3D vision systems is a crucial step prior to any 3D scanning operations. It allows to identify the requested internal, external and distortion parameters used later to collect a dense and accurate point-cloud of the mechanical part. In this context, calibration techniques of 3D vision systems have been studied and one novel optimisation method is proposed to improve the calibration accuracy. A synthetic and experimental evaluation was conducted to prove the efficiency of the optimization method where the convergence has been proven to be faster. The calibration of the developed 3D vision system is carried out with a traceable ceramic checkboard that has been measured by an optical CMM internally using MicroVu excel optical CMM machine.Finally, a large volume part quite similar to that of aeronautics with complex shapes is developed, measured by a traceable Zeiss UPMC carat CMM machine, and used for the evaluation of the developed 3D vision system. A local scanning strategy is adopted to cover the entire surface of the large volume part. It consists of independently scanning several areas of the part and then aligning the measurement in a single reference frame using validated registration techniques. To obtain a reliable and accurate measurement result, 3D data processing and fusion algorithms are studied. The result of large volume part measurement has shown a maximum fitting error of about 150 µm.

photogrammetry, 3D measurement, programming, image processing, C++ / Matlab, metrology

Full document (FR) : HAL-03994528

ALASONATI E., CAEBERGS T., PÉTRY J., SEBAÏHI N., FISICARO P. and FELTIN N., “Size measurement of silica nanoparticles by asymmetric flow field-flow fractionation coupled to multi-angle light scattering: A comparison exercise between two metrological institutes,” J. Chromatogr. A, 2021, 1638, 461859, DOI: 10.1016/j.chroma.2020.461859.

AREZKI Y., SU R., HEIKKINEN V., LEPRETE F., POSTA P., BITOU Y., SCHOBER C., MEHDI-SOUZANI C., ALZAHRANI B.A.M., ZHANG X., KONDO Y., PRUSS C., LEDL V., ANWER N., BOUAZIZI M.L., LEACH R. and NOUIRA H., “Traceable reference full metrology chain for innovative aspheric and freeform optical surfaces accurate at the nanometer level”, Sensors, 2021, 21, 4, 1103, DOI: 10.3390/s21041103.

CHAMI K., FELTIN N., GAFFET E., LACOUR S., LASSUS M., LE BIHAN O., NIAUDET A., RICAUD M. and NESSALNY F., « Les nanomatériaux manufacturés dans l’environnement professionnel: un aperçu de l’état de l’art | Engineered nanomaterials at workplace: An overview of the state of the art », Arch. des Mal. Prof. l’Environnement, 2021, 82, 1, 51-68, DOI: 10.1016/j.admp.2020.07.003.

CHAPPLE R., KANDOLA B. K. MYLER P., FERRY L., LOPEZ-CUESTA J.-M., CHIVAS-JOLY C. and ERSKINE E. L., “The effect of simultaneous heat/fire and impact on carbon fibril and particle release from carbon fiber-reinforced composites”, Polymer Composites, 2021, 42, 11, DOI: 10.1002/pc.26290.

CHAUVEAU D., BOUVET P., OBATON A-F., GROSJEAN C., NOËL A., SCANDELLA F. and BOURLET C., “Review of additive manufacturing standards and proposal to speed up the development of NDT ISO/ASTM standards-part 1”, Soudage et Techniques Connexes, mai-juin 2021.

CHAUVEAU D., BOUVET P., OBATON A-F., GROSJEAN C., NOËL A., SCANDELLA F. and BOURLET C., “Review of additive manufacturing standards and proposal to speed up the development of NDT ISO/ASTM standards-part 2”, Soudage et Techniques Connexes, juillet-août 2021.

CHIBOUB A., AREZKI Y., VISSIERE A., MEHDI-SOUZANI C., ANWER N., ALZAHRANI B., BOUAZIZI M.L. and NOUIRA H., “Generation of reference softgauges for minimum zone fitting algorithms: case of aspherical and freeform surfaces”, Nanomaterials, 2021, 11, 12, 3386, DOI: 10.3390/nano11123386.

CROUZIER L., DELVALLÉE A., DEVOILLE L., ARTOUS S., SAINT-ANTONIN F. and FELTIN N., “Influence of electron landing energy on the measurement of the dimensional properties of nanoparticle populations imaged by SEM,” Ultramicroscopy, 2021, 226, DOI: 10.1016/j.ultramic.2021.113300.

CROUZIER L., FELTIN N., DELVALLÉE A., PELLEGRINO F., MAURINO V., CIOS G., TOKARSKI T., SALZMANN C., DEUMER J., GOLLWITZER C. and HODOROABA V.D., “Correlative analysis of the dimensional properties of bipyramidal Titania nanoparticles by complementing electron microscopy with other methods”, Nanomaterials (Basel), 2021, 11, 12, 3359, DOI: 10.3390/nano11123359.

CROUZIER L., PAILLOUX F., DELVALLÉE A., DEVOILLE L., FELTIN N. and TROMAS C., “A novel approach for 3D morphological characterization of silica nanoparticle population through HAADF-STEM,” Meas. J. Int. Meas. Confed., 2021, 180, DOI: 10.1016/j.measurement.2021.109521.

DELVALLEE A., OULALITE M., CROUZIER L., DUCOURTIEUX S., LAMBENG N., AMOR W., BOUZAKHER GHOMRASNI N., FELTIN, N., VIOT A. and JAMET C., “Correlation of AFM/SEM/EDS images to discriminate several nanoparticle populations mixed in cosmetics”, Microscopy Today, 2021, 29, 3, 46-51, DOI: 10.1017/S1551929521000638.

ESCHELBACH C., LÖSLER M., GUILLORY J., TRUONG D., WALLERAND J.-P., RÖSE A., KÖCHERT P., PRELLINGER G., MEYER T. and POLLINGER F., “Vom Kleinen zum Großen, Ein Zwischenbericht zum EMPIR-Projekt GeoMetre”, VDV magazin, 5/21.

GHOMRASNI N. B., TACHÉ O., LEROY J., FELTIN N., TESTARD F. and CHIVAS-JOLY C., “Dimensional measurement of TiO₂ (Nano) particles by SAXS and SEM in powder form”, Talanta, 2021, 234, 122619, ISSN: 0039-9140, DOI: 10.1016/j.talanta.2021.122619.

KIM F., PINTAR A., FOX J., TARR J., DONMEZ A. and OBATON A.-F., “Merging experiments and computer simulations in X-Ray computed tomography probability of detection analysis of additive manufacturing flaws”, NDT&E International, 2021, 119, 102416, DOI: 10.1016/j.ndteint.2021.102416.

LOPEZ-CUESTA J.-M., LONGUET C. and CHIVAS-JOLY C., “chap. 14. Thermal degradation, flammability, and potential toxicity of polymer nanocomposites”, In Woodhead Publishing Series in Composites Science and Engineering, Health and Environmental Safety of Nanomaterials (Second Edition), Editors: James Njuguna, Krzysztof Pielichowski, Huijun Zhu, Woodhead Publishing, 2021, 343-373, ISBN: 9780128205051, DOI: 10.1016/B978-0-12-820505-1.00024-9.

MCGUIGAN S., ARGUELLES A., OBATON A-F., DONMEZ A., RIVIÈRE J. and PARISA S., “Resonant ultrasound spectroscopy for quality control of geometrically complex additively manufactured components”, Additive Manufacturing, 2021, 39, 101808, DOI: 10.1016/j.addma.2020.101808.

MONCHOT P., COQUELIN L., GERROUDJ K., FELTIN N., DELVALLÉE A., CROUZIER C. and FISCHER N., “Deep learning based instance segmentation of titanium dioxide particles in the form of agglomerates in scanning electron microscopy”, Nanomaterials, 11, 4, 2021, DOI, : 10.3390/nano11040968.

NOIREAUX J., LOPEZ-SANZ S., VIDMAR J., DEVOILLE L., FISICARO P. and LOESCHNER K., “Titanium dioxide nanoparticles in food: comparison of detection by triple-quadrupole and high-resolution ICP-MS in single-particle mode,” J. Nanoparticle Res., 2021, 23, 4, DOI: 10.1007/s11051-021-05198-1.

OBATON A-F., WANG Y., BUTSCH B. and HUANG Q. A., “Non-destructive resonant acoustic testing and defect classification of additively manufactured lattice structures”, Welding in the World, 2021, 65, 361-371, DOI: 10.1007/s40194-020-01034-7.

PIQUEMAL F., MORÁN‐MEZA J., DELVALLÉE A., RICHERT D. and KAJA K., “Progress in traceable nanoscale capacitance measurements using scanning microwave microscopy,” Nanomaterials, 2021, 11, 3, DOI: 10.3390/nano11030820.

RICHERT D., KAJA K., DELVALLÉE A., ALLAL D., GAUTIER B. and PIQUEMAL F., “Traceable nanoscale measurements of high dielectric constant by scanning microwave microscopy”, Nanomaterials, 2021, 11, 1, DOI: 10.3390/nano11113104.

TOGUEM TAGNE S.-C., VISSIERE A., DAMAK M., MEHDI-SOUZANI C., ANWER N., ALZAHRANI B.A.M., BOUAZIZI M.L. and NOUIRA H., “An advanced Fourier-based separation method for spindle error motion identification”, Precision Engineering, 2022, online: 27 Dec. 2021, 74, 334-346, DOI: 10.1016/j.precisioneng.2021.11.016.

CAYRON C., DE SOETE A., GAILLARD Y., YARDIN C., COUTANT N., BOUVET P. and OBATON A.-F., “Comparison of dimensional measurements from images acquired by synchrotron tomography with VGSTUDIO MAX and ImageJ”, Euspen 2021, Online conference, 7-10 juin 2021.

FOURNET-FAYARD L., CAYRON C., OBATON A.F., KOUTIRI I., GUNENTHIRAM V. and SANCHEZ P., “Influence of the processing parameters on the dimensional accuracy of In625 lattice structures made by Laser Powder Bed Fusion”, Euspen 2021, Online conference, 7-10 juin 2021.

POLLINGER F., COURDE C., ESCHELBACH C., GARCIA-ASENJO L., GUILLORY J., OLOF HEDEKVIST P., KALLIO U., KLÜGEL T., NEYEZHMAKOV P., PESCE D., PISANI M., SEPPÄ J., UNDERWOOD R., WEZKA K. and WIŚNIEWSKI M.,”Large-scale dimensional metrology for geodesy - first results from the European GeoMetre Project”, Scientific Assembly of International Association of Geodesy 2021, Beijing, Chine, 28 juin-2 juillet 2021.

OBATON A.-F., “LNE activities on additive manufacturing (AM) and NDT methods”, Assemblée générale de Academia NDT International, Brescia, Italie, 23 octobre 2021.

OBATON A.-F., “Complex AM part quality evaluation though machine learning enhanced resonant ultrasound spectroscopy method”, ICWAM 2021, 21-22 octobre 2021.

GUILLORY J., “Robot characterization based on a multilateration system with retroreflecting glass spheres n=2 as targets”, 3D Metrology Conference, Online conference, 9-11 novembre 2021.

DORIDOT F. and CHIVAS-JOLY C., “NanoFabNet international Hub for sustainable, industrial-scale nanofabrication - An introduction”, C’NANO 2021, Toulouse, France, 23-25 novembre 2021.

SENTIS M., CHIVAS-JOLY C., FELTIN N., LAMBENG N., LEMAHIEU G., BRAMBILLA G. and MEUNIER G., “Comprehensive study of the dispersibility and stability of TiO₂ nanoparticles dispersions with SMLS and SEM”, C’NANO 2021, Toulouse, France, 23-25 novembre 2021.

CHIVAS-JOLY C., “Study on the product lifecycles, waste recycling and the circular economy for nanomaterials”, European Union Observation for Nanomaterials, novembre 2021.

OBATON A.-F., « Tomographie à rayons X et spectroscopie par résonnance ultrasonore pour l’inspection en fabrication additive », JT technique régionale Est de la Cofrend - Les END appliqués à la fabrication additive, Nancy, France, 9 décembre 2021.

In Europe, regulatory requirements for labelling obligation for food, cosmetics or biocides impose to the additives users to know if the substances should be considered as a nanomaterial (NM) or not. A reliable metrology is therefore necessary for the nano-objects identification and characterization. This metrological characterization remains a challenge due to the numerous parameters to be considered in order to fully describe these nano-objects (size, size distribution, agglomeration/aggregation state, shape, specific surface area, chemical composition, surface chemistry and surface charge), which are listed in the ISO/TC 229 (PDTR 13014) standard. The thesis general context is the NMs characterization and more specifically dimensional characterization at the nanometric scale. The study focus on the Titanium dioxide (TiO₂) (nano) particles which are ranked among the 5 most produced nanoparticulate substances (based on tonnage) in the world and used in many applications. The objective is to evaluate and compare measurands of several dimensional characterization techniques for nanoparticles and thus determine their constituent particle size. In this way, ensemble and integral techniques such as SAXS (small angle X-ray scattering), DLS (dynamic light scattering) and BET (Brunauer-Emmett-Teller) have been compared to the direct measurement technique, SEM (scanning electron microscopy). Emphasis is placed on the influence evaluation of several factors, namely, the size, the shape as well as the particles crystallinity and the complex matrix (set of elements in coexistence with the particles of interest), on the realized measurements. The selection of a large materials variety (reference, synthetic, raw material or finished products) enables the NMs characterization difficulties identification according to their sources. After a literature review to place the thesis in its context, a first part is devoted to the elaboration of a sample preparation protocol for SEM in order to improve the image processing step to comply with the regulations and to determine isolated particles size and/or constituents particles from agglomerates. Following the size of particles/agglomerates by DLS, the sonication step impact on the dispersion and dissociation of agglomerated (nano)-objects present in suspension was highlighted. In a second part, a multi-technique approach is implemented to compare two measurands from different instruments (an equivalent diameter to a projected surface area for SEM and a specific surface area for SAXS and BET), in order to access the dimensions of the studied (nano)-objects. The influence of different parameters such as the size distribution (or polydispersity), the purity of the samples (and thus the NMs extraction step from their matrix), the interaction between the particles and the particles anisotropy, are discussed. Interaction between particles and shape anisotropy are the most influential factors on specific surface area measurements, or SAXS/BET equivalent diameters. The achieved results illustrate the (nano)-objects characterization difficulties but they confirm the complementarity of the techniques used in this study (SEM, SAXS and BET).

Nanoparticle, Complex medium, Characterization method, Metrology

PhD thesis: https://tel.archives-ouvertes.fr/tel-03447274/document