Local and quantitative measurement of mechanical properties by electrical-nanoindentation in situ SEM: Application to a multi-phase AgCuPd alloy
Nanoindentation has now become the key technique for measuring the mechanical properties of materials at small scales. However, the quantitative and accurate processing of nanoindentation data relies on a physical quantity that is not directly available: the contact area (Ac) between the indenter ti...
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| Veröffentlicht in: | Materials characterization 2024-08, Vol.214, p.114117, Article 114117 |
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| creator | Boujrouf, Chaymaa Rusinowicz, Morgan Iruela, Solène Antoni-Zdziobek, Annie Champion, Yannick Braccini, Muriel Parry, Guillaume Verdier, Marc Volpi, Fabien |
| description | Nanoindentation has now become the key technique for measuring the mechanical properties of materials at small scales. However, the quantitative and accurate processing of nanoindentation data relies on a physical quantity that is not directly available: the contact area (Ac) between the indenter tip and the sample under test. In complex systems, determining Ac is challenging due to the limitations of standard methods: analytical models have restricted validity domains (sample homogeneity and rheology), and post-mortem observations of residual imprints are time-consuming, do not appraise property gradients and cannot be applied to materials with significant elastic recovery.
In this paper, a comprehensive methodology is proposed to continuously measure contact area during indentation. The proposed methodology, referred to as electrical-nanoindentation (ENI), is based on real-time monitoring of the electrical contact resistance (ECR). The protocol only requires mechanical and electrical calibrations of the indenter tip on reference materials, leading to one-to-one relationship between ECR and contact area. An original approach is also proposed to deal with the presence of surface passivating layers that generally disturb ECR measurements. As an illustration, the methodology is applied to the characterization of a multi-phase alloy (MPA) composed of silver, copper and palladium. This alloy raises the same challenges as those usually faced by nanoindentation in advanced metallurgy: heterogenous distribution of individual phases at the micro-scale, composite response of a complex mixture of hard/stiff and ductile/soft phases, … In addition, the ohmicity of contact is disturbed by surface passivating layers. Despite these numerous hindrances, the proposed methodology is successfully applied to this material. The evolution of contact area is compared with standard methods: an impressive accuracy of |
| doi_str_mv | 10.1016/j.matchar.2024.114117 |
| format | Article |
| fullrecord | <record><control><sourceid>hal_cross</sourceid><recordid>TN_cdi_hal_primary_oai_HAL_hal_04639148v1</recordid><sourceformat>XML</sourceformat><sourcesystem>PC</sourcesystem><els_id>S1044580324004984</els_id><sourcerecordid>oai_HAL_hal_04639148v1</sourcerecordid><originalsourceid>FETCH-LOGICAL-c291t-cae008e6379f018e063a5cd2d251a279e531dbb1ce840721c74384acfc194ea03</originalsourceid><addsrcrecordid>eNqFUc1q3DAQNqWFpmkfoaBrDt5obNmWcynLknYDG1poexaz8rirxZZcSV7Yt-gjV86GXHOan-8HZr4s-wx8BRzq2-NqxKgP6FcFL8QKQAA0b7IrkE2ZC5Dt29RzIfJK8vJ99iGEI-e8ltBcZf92TuPA0Hbs74w2mojRnIiNhGH2NJKNzPVpTP7WLNTJu4l8NBTY_sxoIB39AuQWrTO2S4pk4SwzlgUTZ_bz_vGOradpSKwnIDqGbJyHaPLpgIHY-s9m_tExHAZ3_pi963EI9Om5Xme_v97_2mzz3fdvD5v1LtdFCzHXSJxLqsum7TlI4nWJle6KrqgAi6alqoRuvwdNUvCmAN2IUgrUvYZWEPLyOru5-B5wUJM3I_qzcmjUdr1Ty46LumxByBMkbnXhau9C8NS_CICrJQJ1VM8RqCUCdYkg6b5cdJQOORnyKmhDVlNnfHqb6px5xeE_JESUPQ</addsrcrecordid><sourcetype>Open Access Repository</sourcetype><iscdi>true</iscdi><recordtype>article</recordtype></control><display><type>article</type><title>Local and quantitative measurement of mechanical properties by electrical-nanoindentation in situ SEM: Application to a multi-phase AgCuPd alloy</title><source>Elsevier ScienceDirect Journals Complete</source><creator>Boujrouf, Chaymaa ; Rusinowicz, Morgan ; Iruela, Solène ; Antoni-Zdziobek, Annie ; Champion, Yannick ; Braccini, Muriel ; Parry, Guillaume ; Verdier, Marc ; Volpi, Fabien</creator><creatorcontrib>Boujrouf, Chaymaa ; Rusinowicz, Morgan ; Iruela, Solène ; Antoni-Zdziobek, Annie ; Champion, Yannick ; Braccini, Muriel ; Parry, Guillaume ; Verdier, Marc ; Volpi, Fabien</creatorcontrib><description>Nanoindentation has now become the key technique for measuring the mechanical properties of materials at small scales. However, the quantitative and accurate processing of nanoindentation data relies on a physical quantity that is not directly available: the contact area (Ac) between the indenter tip and the sample under test. In complex systems, determining Ac is challenging due to the limitations of standard methods: analytical models have restricted validity domains (sample homogeneity and rheology), and post-mortem observations of residual imprints are time-consuming, do not appraise property gradients and cannot be applied to materials with significant elastic recovery.
In this paper, a comprehensive methodology is proposed to continuously measure contact area during indentation. The proposed methodology, referred to as electrical-nanoindentation (ENI), is based on real-time monitoring of the electrical contact resistance (ECR). The protocol only requires mechanical and electrical calibrations of the indenter tip on reference materials, leading to one-to-one relationship between ECR and contact area. An original approach is also proposed to deal with the presence of surface passivating layers that generally disturb ECR measurements. As an illustration, the methodology is applied to the characterization of a multi-phase alloy (MPA) composed of silver, copper and palladium. This alloy raises the same challenges as those usually faced by nanoindentation in advanced metallurgy: heterogenous distribution of individual phases at the micro-scale, composite response of a complex mixture of hard/stiff and ductile/soft phases, … In addition, the ohmicity of contact is disturbed by surface passivating layers. Despite these numerous hindrances, the proposed methodology is successfully applied to this material. The evolution of contact area is compared with standard methods: an impressive accuracy of <2% standard-deviation is achieved when compared to post-mortem observations. The elastic moduli and hardnesses of individual phases are then accurately extracted. In addition, in order to gain in spatial definition, the ENI set-up is integrated into a scanning electron microscope (SEM), enabling indent positioning with a precision close to 100 nm.
Two challenges are successfully met with the ENI methodology. On a mechanical point of view, the response of individual phases can be identified despite the complex rheology of heterogeneous materials, proving the approach applies to all mechanical behaviors (sink-in or pile-up rheologies, homogeneous or heterogeneous materials, with or without elastic recovery, …). On an electrical point of view, even if contact ohmicity is the only requirement of the methodology, it is possible to identify and overcome deviations from contact ohmicity induced by surface passivation. In particular, the non-linear resistive contribution of insulating layers fades during indentation thanks to its dependence as the reciprocal of the square of contact radius. The present work provides the keys to monitoring the contact area on any metallic sample, whether oxide-free or oxidized, making this methodology a promising alternative to standard methods.
[Display omitted]
•A methodology is proposed to continuously measure contact area during indentation.•The methodology processes ECR after simple electrical and mechanical calibrations.•The effect of surface passivating layer on electrical contact ohmicity is discussed.•Applied to a multi-phase alloy, an impressive accuracy is obtained (2% std-dev.).•Hardness and modulus can then be extracted accurately at a micrometer-scale.</description><identifier>ISSN: 1044-5803</identifier><identifier>EISSN: 1873-4189</identifier><identifier>DOI: 10.1016/j.matchar.2024.114117</identifier><language>eng</language><publisher>Elsevier Inc</publisher><subject>Chemical Sciences ; Contact area monitoring ; ECR ; In situ SEM ; Material chemistry ; Mechanical properties of multi-phase alloys ; Mechanics ; Mechanics of materials ; Nanoindentation ; Physics</subject><ispartof>Materials characterization, 2024-08, Vol.214, p.114117, Article 114117</ispartof><rights>2024 Elsevier Inc.</rights><rights>Distributed under a Creative Commons Attribution 4.0 International License</rights><lds50>peer_reviewed</lds50><oa>free_for_read</oa><woscitedreferencessubscribed>false</woscitedreferencessubscribed><cites>FETCH-LOGICAL-c291t-cae008e6379f018e063a5cd2d251a279e531dbb1ce840721c74384acfc194ea03</cites><orcidid>0000-0003-0563-2675 ; 0000-0002-1372-9058</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://www.sciencedirect.com/science/article/pii/S1044580324004984$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>230,314,776,780,881,3537,27901,27902,65306</link.rule.ids><backlink>$$Uhttps://hal.science/hal-04639148$$DView record in HAL$$Hfree_for_read</backlink></links><search><creatorcontrib>Boujrouf, Chaymaa</creatorcontrib><creatorcontrib>Rusinowicz, Morgan</creatorcontrib><creatorcontrib>Iruela, Solène</creatorcontrib><creatorcontrib>Antoni-Zdziobek, Annie</creatorcontrib><creatorcontrib>Champion, Yannick</creatorcontrib><creatorcontrib>Braccini, Muriel</creatorcontrib><creatorcontrib>Parry, Guillaume</creatorcontrib><creatorcontrib>Verdier, Marc</creatorcontrib><creatorcontrib>Volpi, Fabien</creatorcontrib><title>Local and quantitative measurement of mechanical properties by electrical-nanoindentation in situ SEM: Application to a multi-phase AgCuPd alloy</title><title>Materials characterization</title><description>Nanoindentation has now become the key technique for measuring the mechanical properties of materials at small scales. However, the quantitative and accurate processing of nanoindentation data relies on a physical quantity that is not directly available: the contact area (Ac) between the indenter tip and the sample under test. In complex systems, determining Ac is challenging due to the limitations of standard methods: analytical models have restricted validity domains (sample homogeneity and rheology), and post-mortem observations of residual imprints are time-consuming, do not appraise property gradients and cannot be applied to materials with significant elastic recovery.
In this paper, a comprehensive methodology is proposed to continuously measure contact area during indentation. The proposed methodology, referred to as electrical-nanoindentation (ENI), is based on real-time monitoring of the electrical contact resistance (ECR). The protocol only requires mechanical and electrical calibrations of the indenter tip on reference materials, leading to one-to-one relationship between ECR and contact area. An original approach is also proposed to deal with the presence of surface passivating layers that generally disturb ECR measurements. As an illustration, the methodology is applied to the characterization of a multi-phase alloy (MPA) composed of silver, copper and palladium. This alloy raises the same challenges as those usually faced by nanoindentation in advanced metallurgy: heterogenous distribution of individual phases at the micro-scale, composite response of a complex mixture of hard/stiff and ductile/soft phases, … In addition, the ohmicity of contact is disturbed by surface passivating layers. Despite these numerous hindrances, the proposed methodology is successfully applied to this material. The evolution of contact area is compared with standard methods: an impressive accuracy of <2% standard-deviation is achieved when compared to post-mortem observations. The elastic moduli and hardnesses of individual phases are then accurately extracted. In addition, in order to gain in spatial definition, the ENI set-up is integrated into a scanning electron microscope (SEM), enabling indent positioning with a precision close to 100 nm.
Two challenges are successfully met with the ENI methodology. On a mechanical point of view, the response of individual phases can be identified despite the complex rheology of heterogeneous materials, proving the approach applies to all mechanical behaviors (sink-in or pile-up rheologies, homogeneous or heterogeneous materials, with or without elastic recovery, …). On an electrical point of view, even if contact ohmicity is the only requirement of the methodology, it is possible to identify and overcome deviations from contact ohmicity induced by surface passivation. In particular, the non-linear resistive contribution of insulating layers fades during indentation thanks to its dependence as the reciprocal of the square of contact radius. The present work provides the keys to monitoring the contact area on any metallic sample, whether oxide-free or oxidized, making this methodology a promising alternative to standard methods.
[Display omitted]
•A methodology is proposed to continuously measure contact area during indentation.•The methodology processes ECR after simple electrical and mechanical calibrations.•The effect of surface passivating layer on electrical contact ohmicity is discussed.•Applied to a multi-phase alloy, an impressive accuracy is obtained (2% std-dev.).•Hardness and modulus can then be extracted accurately at a micrometer-scale.</description><subject>Chemical Sciences</subject><subject>Contact area monitoring</subject><subject>ECR</subject><subject>In situ SEM</subject><subject>Material chemistry</subject><subject>Mechanical properties of multi-phase alloys</subject><subject>Mechanics</subject><subject>Mechanics of materials</subject><subject>Nanoindentation</subject><subject>Physics</subject><issn>1044-5803</issn><issn>1873-4189</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2024</creationdate><recordtype>article</recordtype><recordid>eNqFUc1q3DAQNqWFpmkfoaBrDt5obNmWcynLknYDG1poexaz8rirxZZcSV7Yt-gjV86GXHOan-8HZr4s-wx8BRzq2-NqxKgP6FcFL8QKQAA0b7IrkE2ZC5Dt29RzIfJK8vJ99iGEI-e8ltBcZf92TuPA0Hbs74w2mojRnIiNhGH2NJKNzPVpTP7WLNTJu4l8NBTY_sxoIB39AuQWrTO2S4pk4SwzlgUTZ_bz_vGOradpSKwnIDqGbJyHaPLpgIHY-s9m_tExHAZ3_pi963EI9Om5Xme_v97_2mzz3fdvD5v1LtdFCzHXSJxLqsum7TlI4nWJle6KrqgAi6alqoRuvwdNUvCmAN2IUgrUvYZWEPLyOru5-B5wUJM3I_qzcmjUdr1Ty46LumxByBMkbnXhau9C8NS_CICrJQJ1VM8RqCUCdYkg6b5cdJQOORnyKmhDVlNnfHqb6px5xeE_JESUPQ</recordid><startdate>20240801</startdate><enddate>20240801</enddate><creator>Boujrouf, Chaymaa</creator><creator>Rusinowicz, Morgan</creator><creator>Iruela, Solène</creator><creator>Antoni-Zdziobek, Annie</creator><creator>Champion, Yannick</creator><creator>Braccini, Muriel</creator><creator>Parry, Guillaume</creator><creator>Verdier, Marc</creator><creator>Volpi, Fabien</creator><general>Elsevier Inc</general><general>Elsevier</general><scope>AAYXX</scope><scope>CITATION</scope><scope>1XC</scope><scope>VOOES</scope><orcidid>https://orcid.org/0000-0003-0563-2675</orcidid><orcidid>https://orcid.org/0000-0002-1372-9058</orcidid></search><sort><creationdate>20240801</creationdate><title>Local and quantitative measurement of mechanical properties by electrical-nanoindentation in situ SEM: Application to a multi-phase AgCuPd alloy</title><author>Boujrouf, Chaymaa ; Rusinowicz, Morgan ; Iruela, Solène ; Antoni-Zdziobek, Annie ; Champion, Yannick ; Braccini, Muriel ; Parry, Guillaume ; Verdier, Marc ; Volpi, Fabien</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c291t-cae008e6379f018e063a5cd2d251a279e531dbb1ce840721c74384acfc194ea03</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2024</creationdate><topic>Chemical Sciences</topic><topic>Contact area monitoring</topic><topic>ECR</topic><topic>In situ SEM</topic><topic>Material chemistry</topic><topic>Mechanical properties of multi-phase alloys</topic><topic>Mechanics</topic><topic>Mechanics of materials</topic><topic>Nanoindentation</topic><topic>Physics</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Boujrouf, Chaymaa</creatorcontrib><creatorcontrib>Rusinowicz, Morgan</creatorcontrib><creatorcontrib>Iruela, Solène</creatorcontrib><creatorcontrib>Antoni-Zdziobek, Annie</creatorcontrib><creatorcontrib>Champion, Yannick</creatorcontrib><creatorcontrib>Braccini, Muriel</creatorcontrib><creatorcontrib>Parry, Guillaume</creatorcontrib><creatorcontrib>Verdier, Marc</creatorcontrib><creatorcontrib>Volpi, Fabien</creatorcontrib><collection>CrossRef</collection><collection>Hyper Article en Ligne (HAL)</collection><collection>Hyper Article en Ligne (HAL) (Open Access)</collection><jtitle>Materials characterization</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Boujrouf, Chaymaa</au><au>Rusinowicz, Morgan</au><au>Iruela, Solène</au><au>Antoni-Zdziobek, Annie</au><au>Champion, Yannick</au><au>Braccini, Muriel</au><au>Parry, Guillaume</au><au>Verdier, Marc</au><au>Volpi, Fabien</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Local and quantitative measurement of mechanical properties by electrical-nanoindentation in situ SEM: Application to a multi-phase AgCuPd alloy</atitle><jtitle>Materials characterization</jtitle><date>2024-08-01</date><risdate>2024</risdate><volume>214</volume><spage>114117</spage><pages>114117-</pages><artnum>114117</artnum><issn>1044-5803</issn><eissn>1873-4189</eissn><abstract>Nanoindentation has now become the key technique for measuring the mechanical properties of materials at small scales. However, the quantitative and accurate processing of nanoindentation data relies on a physical quantity that is not directly available: the contact area (Ac) between the indenter tip and the sample under test. In complex systems, determining Ac is challenging due to the limitations of standard methods: analytical models have restricted validity domains (sample homogeneity and rheology), and post-mortem observations of residual imprints are time-consuming, do not appraise property gradients and cannot be applied to materials with significant elastic recovery.
In this paper, a comprehensive methodology is proposed to continuously measure contact area during indentation. The proposed methodology, referred to as electrical-nanoindentation (ENI), is based on real-time monitoring of the electrical contact resistance (ECR). The protocol only requires mechanical and electrical calibrations of the indenter tip on reference materials, leading to one-to-one relationship between ECR and contact area. An original approach is also proposed to deal with the presence of surface passivating layers that generally disturb ECR measurements. As an illustration, the methodology is applied to the characterization of a multi-phase alloy (MPA) composed of silver, copper and palladium. This alloy raises the same challenges as those usually faced by nanoindentation in advanced metallurgy: heterogenous distribution of individual phases at the micro-scale, composite response of a complex mixture of hard/stiff and ductile/soft phases, … In addition, the ohmicity of contact is disturbed by surface passivating layers. Despite these numerous hindrances, the proposed methodology is successfully applied to this material. The evolution of contact area is compared with standard methods: an impressive accuracy of <2% standard-deviation is achieved when compared to post-mortem observations. The elastic moduli and hardnesses of individual phases are then accurately extracted. In addition, in order to gain in spatial definition, the ENI set-up is integrated into a scanning electron microscope (SEM), enabling indent positioning with a precision close to 100 nm.
Two challenges are successfully met with the ENI methodology. On a mechanical point of view, the response of individual phases can be identified despite the complex rheology of heterogeneous materials, proving the approach applies to all mechanical behaviors (sink-in or pile-up rheologies, homogeneous or heterogeneous materials, with or without elastic recovery, …). On an electrical point of view, even if contact ohmicity is the only requirement of the methodology, it is possible to identify and overcome deviations from contact ohmicity induced by surface passivation. In particular, the non-linear resistive contribution of insulating layers fades during indentation thanks to its dependence as the reciprocal of the square of contact radius. The present work provides the keys to monitoring the contact area on any metallic sample, whether oxide-free or oxidized, making this methodology a promising alternative to standard methods.
[Display omitted]
•A methodology is proposed to continuously measure contact area during indentation.•The methodology processes ECR after simple electrical and mechanical calibrations.•The effect of surface passivating layer on electrical contact ohmicity is discussed.•Applied to a multi-phase alloy, an impressive accuracy is obtained (2% std-dev.).•Hardness and modulus can then be extracted accurately at a micrometer-scale.</abstract><pub>Elsevier Inc</pub><doi>10.1016/j.matchar.2024.114117</doi><orcidid>https://orcid.org/0000-0003-0563-2675</orcidid><orcidid>https://orcid.org/0000-0002-1372-9058</orcidid><oa>free_for_read</oa></addata></record> |
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| subjects | Chemical Sciences Contact area monitoring ECR In situ SEM Material chemistry Mechanical properties of multi-phase alloys Mechanics Mechanics of materials Nanoindentation Physics |
| title | Local and quantitative measurement of mechanical properties by electrical-nanoindentation in situ SEM: Application to a multi-phase AgCuPd alloy |
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