Operando X-ray scattering reveals ordering-mediated solidification in additive manufacturing

preprint OA: closed
Full text JSON View at publisher

Abstract

Abstract Solidification in fusion-based metal additive manufacturing (AM) occurs under non-equilibrium conditions, often producing microstructures that deviate from classical theories, such as refined grains with high twin density arising from abnormal columnar-to-equiaxed transition (CET). While such feature has been linked to liquid atomic orderings, direct mechanistic evidence has been lacking. Here, we perform operando synchrotron X-ray total scattering measurement with rapid pair distribution functon(PDF) analysis to probe atomic structures in AM melt pools. We characterize the evolution of short- and medium-range orderings and connect their selective consumption to distinct solidification pathways in Inconel 718 and other alloys. Our findings show that abnormal CET originates from decomposition of icosahedral clusters into twinned nuclei, offering new opportunities for alloy design and microstructure control in AM.
Full text 12,657 characters · extracted from preprint-html · click to expand
Operando X-ray scattering reveals ordering-mediated solidification in additive manufacturing | Research Square window.SnipcartSettings = { analytics: { enabled: false } }; (function() { var accessVector = localStorage.getItem('access_vector') || ''; window.dataLayer = window.dataLayer || []; if (accessVector) { window.dataLayer.push({ user: { profile: { profileInfo: { snid: accessVector } } } }); } })(); (function(w,d,s,l,i){w[l]=w[l]||[];w[l].push({'gtm.start':new Date().getTime(),event:'gtm.js'});var f=d.getElementsByTagName(s)[0],j=d.createElement(s),dl=l!='dataLayer'?'&l='+l:'';j.async=true;j.src='https://www.googletagmanager.com/gtm.js?id='+i+dl;f.parentNode.insertBefore(j,f);})(window,document,'script','dataLayer','GTM-K279D39R'); Browse Preprints In Review Journals COVID-19 Preprints AJE Video Bytes Research Tools Research Promotion AJE Professional Editing AJE Rubriq About Preprint Platform In Review Editorial Policies Our Team Advisory Board Help Center Sign In Submit a Preprint Cite Share Download PDF Article Operando X-ray scattering reveals ordering-mediated solidification in additive manufacturing Tao Sun, Lin Gao, Kyle Mumm, Zhongshu Ren, Zhou Yu, Xingyang Li, and 1 more This is a preprint; it has not been peer reviewed by a journal. https://doi.org/ 10.21203/rs.3.rs-7890736/v1 This work is licensed under a CC BY 4.0 License Status: Under Review Version 1 posted You are reading this latest preprint version Abstract Solidification in fusion-based metal additive manufacturing (AM) occurs under non-equilibrium conditions, often producing microstructures that deviate from classical theories, such as refined grains with high twin density arising from abnormal columnar-to-equiaxed transition (CET). While such feature has been linked to liquid atomic orderings, direct mechanistic evidence has been lacking. Here, we perform operando synchrotron X-ray total scattering measurement with rapid pair distribution functon(PDF) analysis to probe atomic structures in AM melt pools. We characterize the evolution of short- and medium-range orderings and connect their selective consumption to distinct solidification pathways in Inconel 718 and other alloys. Our findings show that abnormal CET originates from decomposition of icosahedral clusters into twinned nuclei, offering new opportunities for alloy design and microstructure control in AM. Physical sciences/Materials science/Structural materials/Metals and alloys Physical sciences/Engineering/Mechanical engineering Full Text Additional Declarations There is NO Competing Interest. Supplementary Files SupplementarymaterialsNC.pdf Supplementary materials Cite Share Download PDF Status: Under Review Version 1 posted You are reading this latest preprint version Research Square lets you share your work early, gain feedback from the community, and start making changes to your manuscript prior to peer review in a journal. As a division of Research Square Company, we’re committed to making research communication faster, fairer, and more useful. We do this by developing innovative software and high quality services for the global research community. Our growing team is made up of researchers and industry professionals working together to solve the most critical problems facing scientific publishing. Also discoverable on Platform About Our Team In Review Editorial Policies Advisory Board Help Center Resources Author Services Accessibility API Access RSS feed Manage Cookie Preferences © Research Square 2026 | ISSN 2693-5015 (online) Privacy Policy Terms of Service Do Not Sell My Personal Information {"props":{"pageProps":{"initialData":{"identity":"rs-7890736","acceptedTermsAndConditions":true,"allowDirectSubmit":false,"archivedVersions":[],"articleType":"Article","associatedPublications":[],"authors":[{"id":538318202,"identity":"f354262a-7e1b-4d25-80a1-0c17741ca76c","order_by":0,"name":"Tao Sun","email":"data:image/png;base64,iVBORw0KGgoAAAANSUhEUgAAAZAAAAAyAQMAAABI0h/eAAAABlBMVEX///8AAABVwtN+AAAACXBIWXMAAA7EAAAOxAGVKw4bAAAA6UlEQVRIiWNgGAWjYPACGxDBhiTAhkMhEPBAqDQgZgYrkyBWy2EStNizHz78mXfH+Tx+6fPHHvNU1NXxS589wPCh7DBuW3jS0qR5z9wuluxLZjfmOXNYQrIvL4Fxxjk8WhhyzJh5224nbjjDzCad23ZAwuAMjwFQBI8W/jfGn3nbzkG1/KuTsAdp+YtPi0SOgTRv2wGolgZmCQMeoBZGfFpuPEuTnNuWnDizh9lM+s+xw5IzgLYc7DmXjlMLe3/y4Q9v2+wS+3kYn0nOqKnj5+/hMXzwo8wapxbs4ACJ6kfBKBgFo2AUoAEA3NVLc75ruTIAAAAASUVORK5CYII=","orcid":"https://orcid.org/0000-0002-4881-9774","institution":"Northwestern University","correspondingAuthor":true,"prefix":"","firstName":"Tao","middleName":"","lastName":"Sun","suffix":""},{"id":538318203,"identity":"3b394368-86f7-453e-aada-45f364aefa4d","order_by":1,"name":"Lin Gao","email":"","orcid":"","institution":"The University of Alabama","correspondingAuthor":false,"prefix":"","firstName":"Lin","middleName":"","lastName":"Gao","suffix":""},{"id":538318204,"identity":"0ccead01-46f0-488d-943c-e87b69da397a","order_by":2,"name":"Kyle Mumm","email":"","orcid":"","institution":"Northwestern University","correspondingAuthor":false,"prefix":"","firstName":"Kyle","middleName":"","lastName":"Mumm","suffix":""},{"id":538318205,"identity":"0ed88004-cb8f-453c-9d51-17d4539ce9b3","order_by":3,"name":"Zhongshu Ren","email":"","orcid":"https://orcid.org/0000-0003-4662-2422","institution":"Brookhaven National Laboratory","correspondingAuthor":false,"prefix":"","firstName":"Zhongshu","middleName":"","lastName":"Ren","suffix":""},{"id":538318206,"identity":"cdbbd030-5d92-4c01-9e07-c37e8e7edfb6","order_by":4,"name":"Zhou Yu","email":"","orcid":"","institution":"The University of Alabama","correspondingAuthor":false,"prefix":"","firstName":"Zhou","middleName":"","lastName":"Yu","suffix":""},{"id":538318207,"identity":"7f62384f-9abb-4ad1-83c2-0480d1302d20","order_by":5,"name":"Xingyang Li","email":"","orcid":"","institution":"Northwestern University","correspondingAuthor":false,"prefix":"","firstName":"Xingyang","middleName":"","lastName":"Li","suffix":""},{"id":538318208,"identity":"ddd6dd09-74d6-46d2-b472-3c2e51675495","order_by":6,"name":"Chihpin Chuang","email":"","orcid":"https://orcid.org/0000-0003-0295-381X","institution":"Argonne National Laboratory","correspondingAuthor":false,"prefix":"","firstName":"Chihpin","middleName":"","lastName":"Chuang","suffix":""}],"badges":[],"createdAt":"2025-10-18 04:15:28","currentVersionCode":1,"declarations":"","doi":"10.21203/rs.3.rs-7890736/v1","doiUrl":"https://doi.org/10.21203/rs.3.rs-7890736/v1","draftVersion":[],"editorialEvents":[],"editorialNote":"","failedWorkflow":false,"files":[{"id":95162138,"identity":"551da7e8-708a-488a-9836-530ceb3056fa","added_by":"auto","created_at":"2025-11-05 03:48:56","extension":"pdf","order_by":0,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":7814556,"visible":true,"origin":"","legend":"","description":"","filename":"ManuscriptNC.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7890736/v1/29ca90e8a12384cc76525fed.pdf"},{"id":95162137,"identity":"07b58ceb-4be5-47d0-bb44-60d4181ed1f7","added_by":"auto","created_at":"2025-11-05 03:48:56","extension":"json","order_by":1,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":7483,"visible":true,"origin":"","legend":"","description":"","filename":"NCOMMS2585327T.json","url":"https://assets-eu.researchsquare.com/files/rs-7890736/v1/2cf34205c6af338f0b0d63bd.json"},{"id":95162139,"identity":"9efce49d-96c5-42f7-818d-6687aca08629","added_by":"auto","created_at":"2025-11-05 03:48:56","extension":"pdf","order_by":2,"title":"","display":"","copyAsset":false,"role":"acdc-reference","size":19401457,"visible":true,"origin":"","legend":"","description":"","filename":"SupplementarymaterialsNC.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7890736/v1/db866c027c1b1dbac2b91146.pdf"},{"id":95226941,"identity":"af374c55-0e76-43f3-98fd-c9d47b69c98c","added_by":"auto","created_at":"2025-11-05 16:31:55","extension":"pdf","order_by":1,"title":"","display":"","copyAsset":false,"role":"manuscript-pdf","size":6533851,"visible":true,"origin":"","legend":"Article File","description":"","filename":"ManuscriptNC.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7890736/v1_covered_1edbec78-8fe0-4798-a464-e68bebb0b82c.pdf"},{"id":95162140,"identity":"792cb12c-04e3-4b28-8314-1d13aedf74a1","added_by":"auto","created_at":"2025-11-05 03:48:56","extension":"pdf","order_by":1,"title":"","display":"","copyAsset":false,"role":"supplement","size":19401457,"visible":true,"origin":"","legend":"Supplementary materials","description":"","filename":"SupplementarymaterialsNC.pdf","url":"https://assets-eu.researchsquare.com/files/rs-7890736/v1/278204e60611f27290ac72d2.pdf"}],"financialInterests":"There is \u003cb\u003eNO\u003c/b\u003e Competing Interest.","formattedTitle":"Operando X-ray scattering reveals ordering-mediated solidification in additive manufacturing","fulltext":[],"fulltextSource":"","fullText":"","funders":[],"hasAdminPriorityOnWorkflow":false,"hasManuscriptDocX":false,"hasOptedInToPreprint":true,"hasPassedJournalQc":"","hasAnyPriority":true,"hideJournal":false,"highlight":"","institution":"","isAcceptedByJournal":false,"isAuthorSuppliedPdf":true,"isDeskRejected":"","isHiddenFromSearch":false,"isInQc":false,"isInWorkflow":false,"isPdf":true,"isPdfUpToDate":true,"isWithdrawnOrRetracted":false,"journal":{"display":true,"email":"[email protected]","identity":"nature-portfolio","isNatureJournal":true,"hasQc":false,"allowDirectSubmit":false,"externalIdentity":"","sideBox":"","snPcode":"","submissionUrl":"","title":"Nature Portfolio","twitterHandle":"","acdcEnabled":false,"dfaEnabled":false,"editorialSystem":"ejp","reportingPortfolio":"","inReviewEnabled":true,"inReviewRevisionsEnabled":false},"keywords":"","lastPublishedDoi":"10.21203/rs.3.rs-7890736/v1","lastPublishedDoiUrl":"https://doi.org/10.21203/rs.3.rs-7890736/v1","license":{"name":"CC BY 4.0","url":"https://creativecommons.org/licenses/by/4.0/"},"manuscriptAbstract":"Solidification in fusion-based metal additive manufacturing (AM) occurs under non-equilibrium conditions, often producing microstructures that deviate from classical theories, such as refined grains with high twin density arising from abnormal columnar-to-equiaxed transition (CET). While such feature has been linked to liquid atomic orderings, direct mechanistic evidence has been lacking. Here, we perform operando synchrotron X-ray total scattering measurement with rapid pair distribution functon(PDF) analysis to probe atomic structures in AM melt pools. We characterize the evolution of short- and medium-range orderings and connect their selective consumption to distinct solidification pathways in Inconel 718 and other alloys. Our findings show that abnormal CET originates from decomposition of icosahedral clusters into twinned nuclei, offering new opportunities for alloy design and microstructure control in AM.","manuscriptTitle":"Operando X-ray scattering reveals ordering-mediated solidification in additive manufacturing","msid":"","msnumber":"","nonDraftVersions":[{"code":1,"date":"2025-11-05 03:48:51","doi":"10.21203/rs.3.rs-7890736/v1","editorialEvents":[],"status":"published","journal":{"display":true,"email":"[email protected]","identity":"nature-communications","isNatureJournal":true,"hasQc":false,"allowDirectSubmit":false,"externalIdentity":"NCOMMS","sideBox":"Learn more about [Nature Communications](http://www.nature.com/ncomms/)","snPcode":"","submissionUrl":"https://mts-ncomms.nature.com/","title":"Nature Communications","twitterHandle":"","acdcEnabled":true,"dfaEnabled":true,"editorialSystem":"ejp","reportingPortfolio":"Nature Communications","inReviewEnabled":true,"inReviewRevisionsEnabled":false}}],"origin":"","ownerIdentity":"aea3686e-8eff-497f-b38c-8dc944b47dd6","owner":[],"postedDate":"November 5th, 2025","published":true,"recentEditorialEvents":[],"rejectedJournal":[],"revision":"","amendment":"","status":"under-review","subjectAreas":[{"id":57256623,"name":"Physical sciences/Materials science/Structural materials/Metals and alloys"},{"id":57256624,"name":"Physical sciences/Engineering/Mechanical engineering"}],"tags":[],"updatedAt":"2026-04-13T13:07:12+00:00","versionOfRecord":[],"versionCreatedAt":"2025-11-05 03:48:51","video":"","vorDoi":"","vorDoiUrl":"","workflowStages":[]},"version":"v1","identity":"rs-7890736","journalConfig":"researchsquare"},"__N_SSP":true},"page":"/article/[identity]/[[...version]]","query":{"redirect":"/article/rs-7890736","identity":"rs-7890736","version":["v1"]},"buildId":"8U1c8b4HqxoKbykW_rLl7","isFallback":false,"isExperimentalCompile":false,"dynamicIds":[84888],"gssp":true,"scriptLoader":[]}

Text is read by the "Ask this paper" AI Q&A widget below. Extraction quality varies by source — PMC NXML preserves structure cleanly, OA-HTML may include some navigation residue, and OA-PDF can have broken hyphenation. The publisher copy (via DOI) is the canonical version.

My notes (saved in your browser only)

Ask this paper AI returns verbatim quotes from the full text · source: preprint-html

Answers must be backed by verbatim quotes from this paper's full text. Hallucinated quotes are dropped automatically; if no verbatim passage answers the question, we say so. How this works

Citation neighborhood (no data yet)

We don't have any in-corpus citations linked to this paper yet. This is a recent paper (2025) — citers typically take a year or two to land, and the OpenAlex reference graph may still be filling in.

Source provenance

europepmc
last seen: 2026-05-20T01:45:00.602351+00:00