Delft University of Technology Fluidized Nanoparticle Agglomerates Formation, Characterization, and Dynamics Fabre, Andrea DOI 10.4233/uuid:e7340a8e-1815-469c-9e46-ddea1ef17b04 Publication date 2016 Document Version Final published version Citation (APA) Fabre, A. (2016). Fluidized Nanoparticle Agglomerates: Formation, Characterization, and Dynamics. https://doi.org/10.4233/uuid:e7340a8e-1815-469c-9e46-ddea1ef17b04 Important note To cite this publication, please use the final published version (if applicable). Please check the document version above. Copyright Other than for strictly personal use, it is not permitted to download, forward or distribute the text or part of it, without the consent of the author(s) and/or copyright holder(s), unless the work is under an open content license such as Creative Commons. Takedown policy Please contact us and provide details if you believe this document breaches copyrights. We will remove access to the work immediately and investigate your claim. This work is downloaded from Delft University of Technology. For technical reasons the number of authors shown on this cover page is limited to a maximum of 10. Fluidized Nanoparticle Agglomerates Formation, Characterization, and Dynamics Andrea Fabre FLUIDIZED NANOPARTICLE AGGLOMERATES FORMATION, CHARACTERIZATION, AND DYNAMICS Proefschrift terverkrijgingvandegraadvandoctor aandeTechnischeUniversiteitDelft, opgezagvandeRectorMagnificusprof.ir.K.Ch.A.M.Luyben, voorzittervanhetCollegevoorPromoties, inhetopenbaarteverdedigenop woensdag23november2016 om12:30uur door Andrea FABRE ChemicalandBiologicalEngineer MassachusettsInstituteofTechnology,deVerenigdeStatenvanAmerika geborenteAguascalientes,Mexico Thisdissertationhasbeenapprovedbythepromotors: Prof.dr.ir.J.R.vanOmmen Prof.dr.ir.M.T.Kreutzer Compositionofthedoctoralcommittee: RectorMagnificus chairman Prof.dr.ir.MichielT.Kreutzer TechnischeUniversiteitDelft Prof.dr.ir.J.RuudvanOmmen TechnischeUniversiteitDelft Independentmembers: Prof.dr.AndreasSchmidt-Ott TechnischeUniversiteitDelft Prof.dr.ir.NielsG.Deen TechnischeUniversiteitEindhoven Prof.dr.FrankKleineJäger BASFParticleFormulationandHandling Prof.dr.MiguelA.S.Quintanilla UniversityofSevilla Dr.WouterK.denOtter UniversityofTwente Prof.dr.ir.ChrisR.Kleijn TechnischeUniversiteitDelft,reservelid TheresearchpresentedinthisthesisreceivedfundingfromtheEuropeanResearch CouncilundertheEuropeanUnion’sSeventhFrameworkProgramme (FP/2007-2013)/ERCGrant,agreementno.279632,andwasconductedintheProduct andProcessEngineeringsectionoftheChemicalEngineeringdepartmentfromthe facultyofAppliedSciences(TNW)oftheDelftUniversityofTechnology. Copyright©2016byAndreaFabre ISBN978-94-6186-721-6 PrintedinTheNetherlandsbyXXX Allrightsreserved.Partsofthisthesisarepublishedinscientificjournalsandcopyright issubjectedtodifferenttermsandconditions. Tomyfamily C ONTENTS Summary ix Samenvatting xi 1 Introduction 1 1.1 Nanoparticles. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 1.2 Agglomeration . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2 1.3 Fluidization. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 1.4 Modeling . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4 1.5 ThesisObjective . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 1.5.1 Outline. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 6 2 Thefractalscalingoffluidizednanoparticleagglomerates 11 2.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12 2.2 Experimentalsetup. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15 2.2.1 Reactor. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15 2.2.2 Powders . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16 2.2.3 Dataacquisitionsystem . . . . . . . . . . . . . . . . . . . . . . . 16 2.3 Results . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 17 2.3.1 Fractalanalysis. . . . . . . . . . . . . . . . . . . . . . . . . . . . 17 2.4 Conclusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 21 3 Contactmechanicsofhighlyporousoxidenanoparticleagglomerates 27 3.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 28 3.2 ExperimentalSection. . . . . . . . . . . . . . . . . . . . . . . . . . . . 30 3.2.1 Powdercharacterization. . . . . . . . . . . . . . . . . . . . . . . 30 3.2.2 SamplePreparation . . . . . . . . . . . . . . . . . . . . . . . . . 30 3.2.3 Elasticitymeasurements. . . . . . . . . . . . . . . . . . . . . . . 31 3.3 Results&Discussion . . . . . . . . . . . . . . . . . . . . . . . . . . . . 32 3.3.1 Samplecharacterization. . . . . . . . . . . . . . . . . . . . . . . 32 3.3.2 ForceCurveAnalysis. . . . . . . . . . . . . . . . . . . . . . . . . 33 3.3.3 ElasticityofDifferentMaterials . . . . . . . . . . . . . . . . . . . 35 3.3.4 TheoreticalElasticity. . . . . . . . . . . . . . . . . . . . . . . . . 37 3.4 Conclusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39 v vi CONTENTS 4 EntrainmentofnanosizedClustersfromananopowderfluidizedbed 51 4.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 52 4.2 ExperimentalSection. . . . . . . . . . . . . . . . . . . . . . . . . . . . 53 4.2.1 Powdercharacterization. . . . . . . . . . . . . . . . . . . . . . . 53 4.2.2 Experimentalsetup . . . . . . . . . . . . . . . . . . . . . . . . . 53 4.2.3 Microscopyanalysis . . . . . . . . . . . . . . . . . . . . . . . . . 55 4.3 Resultsanddiscussion . . . . . . . . . . . . . . . . . . . . . . . . . . . 55 4.3.1 Powdercharacterization. . . . . . . . . . . . . . . . . . . . . . . 55 4.4 Conclusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 61 5 Characterizationofthestratifiedmorphologyofnanoparticleagglomerates 67 5.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 68 5.2 Methods . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69 5.2.1 Materials. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 69 5.2.2 SESANS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 70 5.2.3 SettlingTube. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71 5.3 DataAnalysis . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 71 5.4 ResultsandDiscussion . . . . . . . . . . . . . . . . . . . . . . . . . . . 74 5.4.1 SESANS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 74 5.4.2 SettlingTube. . . . . . . . . . . . . . . . . . . . . . . . . . . . . 75 5.4.3 Combiningallthreescales. . . . . . . . . . . . . . . . . . . . . . 77 5.5 Conclusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 79 6 Modelingthesizedistributioninafluidizedbedofnanopowder 85 6.1 Introduction . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 86 6.2 MaterialandMethods. . . . . . . . . . . . . . . . . . . . . . . . . . . . 87 6.3 Theory . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 88 6.3.1 VanderWaalsforce . . . . . . . . . . . . . . . . . . . . . . . . . 90 6.3.2 Collisionforce . . . . . . . . . . . . . . . . . . . . . . . . . . . . 91 6.3.3 SizeDistributionPrediction . . . . . . . . . . . . . . . . . . . . . 92 6.4 ResultsandDiscussion . . . . . . . . . . . . . . . . . . . . . . . . . . . 93 6.4.1 SizeDistribution. . . . . . . . . . . . . . . . . . . . . . . . . . . 93 6.4.2 ModelPredictions . . . . . . . . . . . . . . . . . . . . . . . . . . 94 6.5 Conclusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 95 References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 96 7 ConclusionsandOutlook 103 7.1 Conclusions. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 103 7.2 Opportunitiesforfutureresearch. . . . . . . . . . . . . . . . . . . . . . 104 7.2.1 Agglomerateplasticity . . . . . . . . . . . . . . . . . . . . . . . . 104 7.2.2 Adjustedforcebalancemodel . . . . . . . . . . . . . . . . . . . . 105 7.2.3 Collisiondynamics. . . . . . . . . . . . . . . . . . . . . . . . . . 106 7.2.4 Numberofcontactsbetweenagglomerates . . . . . . . . . . . . . 107 7.2.5 Differentproductionmethods. . . . . . . . . . . . . . . . . . . . 107 7.2.6 Processednanoparticles. . . . . . . . . . . . . . . . . . . . . . . 108 CONTENTS vii References . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 108 Acknowledgements 111 ListofPublications 113 CurriculumVitae 115