Fluidized Nanoparticle Agglomerates Andrea Fabre

132 Pages·2016·12.28 MB·English

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
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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