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In this study, a novel quartz crystal microbalance (QCM)\u2010based method is developed for in situ monitoring of the grafting kinetics of poly(N\u2010isopropylacrylamide) (PNIPAM) onto gold nanoparticles (AuNPs). Experimental results show that during the initial grafting stage (t = 360 s), a grafting rate constant (\n                    <jats:italic>k<\/jats:italic>\n                    <jats:sub>1<\/jats:sub>\n                    ) of 1.06 \u00d7 10\n                    <jats:sup>\u22122<\/jats:sup>\n                    chains nm\n                    <jats:sup>\u2212<\/jats:sup>\n                    <jats:sup>2<\/jats:sup>\n                    s\n                    <jats:sup>\u22121<\/jats:sup>\n                    and a diffusion\u2010controlled mechanism can be observed. As grafting proceeds, the polymer chains adopt an extended conformation, resulting in a slower grafting rate. Isothermal titration calorimetry (ITC) measurements further validated the reliability of the QCM approach. Further investigations revealed the significant influence of polymer chain length, interparticle spacing, and temperature on grafting behavior. In situ small\u2010angle X\u2010ray scattering (SAXS) studies demonstrated that grafting density plays a decisive role in determining the assembly structures: long\u2010chain PNIPAM grafted at low density forms random close\u2010packed (RCP) structure, while high grafting density promotes face\u2010centered cubic (FCC) ordering. This work not only establishes an in situ method for monitoring grafting on AuNPs, but also clarifies polymer density\u2010structure relationships for nanomaterial design.\n                  <\/jats:p>","DOI":"10.1002\/smll.202512449","type":"journal-article","created":{"date-parts":[[2025,12,17]],"date-time":"2025-12-17T20:16:29Z","timestamp":1766002589000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":1,"title":["Real\u2010Time Investigation of PNIPAM Grafting Dynamics and Grafting Density\u2010Dependent Assembly of Gold Nanoparticles"],"prefix":"10.1002","volume":"22","author":[{"given":"Rui","family":"Ren","sequence":"first","affiliation":[{"name":"Key Laboratory of Materials Chemistry for Energy Conversion and Storage (HUST) of Ministry of Education School of Chemistry and Chemical Engineering Huazhong University of Science and Technology (HUST)  Wuhan 430074 China"},{"name":"Hubei Optical Fundamental Research Center  Wuhan \u00a0 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-5815-8674","authenticated-orcid":false,"given":"Bijin","family":"Xiong","sequence":"additional","affiliation":[{"name":"Key Laboratory of Materials Chemistry for Energy Conversion and Storage (HUST) of Ministry of Education School of Chemistry and Chemical Engineering Huazhong University of Science and Technology (HUST)  Wuhan 430074 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jintao","family":"Zhu","sequence":"additional","affiliation":[{"name":"Key Laboratory of Materials Chemistry for Energy Conversion and Storage (HUST) of Ministry of Education School of Chemistry and Chemical Engineering Huazhong University of Science and Technology (HUST)  Wuhan 430074 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