AFastXrayTomographyandRadioscopyforAlbaWorkingteam:

FedericoSketEusebioSolrzanoJuanGomezBarreiroJoseAntonioYagFabraBartBijnensVicenteGomezRuizdeArgandonaFranciscoGarcaMoreno

Albaworkingteam:

EvapereiroSalvadorFerrerJosepNicolasXabierMikelTurrillasJordiJuanhuixJosepCampmanyGuillotMiguelA.G.Aranda

Peregrine falcon is one of the FASTEST animals in the planet with capacity of diving at 300km/h We have decided to use this animal as a representative icon for the future FAST TOMOGRAPHY beamline

TABLE OF CONTENTS 1. ABSTRACT........................................................................................................................11

2. INTRODUCTION...............................................................................................................12

2.1. ImportanceofXrayimagingandtomography.......................................................12

2.2. VirtuesofXraytomography...................................................................................13

2.3. DevelopmentofSXCTinthelastdecades...............................................................14

2.3.1. 4Dtomography................................................................................................16

2.3.2. Insitutomography..........................................................................................17

2.4. Scopeofthisproposal.............................................................................................18

3. THESPANISH(ANDEUROPEAN)USERCOMMUNITY......................................................19

3.1. CurrentpanoramaofSXCTinEurope......................................................................19

3.2. PotentialusersinSpain...........................................................................................20

4. RELEVANTSCIENTIFICCASES...........................................................................................23

4.1. MultidisciplinaryFasttomographyandradiography:insitustudies......................23

4.1.1. Bubblenucleationandgrowthcharacterizedbyultrafasttomography.........23

4.1.2. InsitusolidificationofAlalloys.......................................................................26

4.1.3. Understandingexplosivevolcanoes:riskevaluationthroughmorphometricanalysisofbubblesandcrystalsinlava...........................................................................30

4.1.4. Foodscience:tastingthetexture....................................................................33

4.1.5. Ultrafast2DRadioscopyoncellwallrupturestostudymetalfoamstabilitymechanisms.....................................................................................................................35

4.1.6. Insitutomographyofcreepprocessofbrass.................................................38

4.1.7. Insitutomographyofdamagedevelopmentofcarbonfiberreinforcedcomposites......................................................................................................................40

4.2. Materialscience......................................................................................................42

4.2.1. ResinmicroflowbyXraycomputedtomography...........................................42

4.2.2. 3DmultiphasenetworksprovidinghightemperaturestrengthtoAlSipistonalloys 44

4.2.3. Submicrometerholotomographyofmultiphasemetals................................47

4.3. Lifesciencesandbiomedicine.................................................................................50

4.3.1. HighresolutionStructuralImagingofstatictissue:........................................51

4.3.2. HighthroughputVirtualPathology.................................................................52

4.3.3. Highspeeddynamicimagingoffunctionalorgans.........................................53

4.4. Historicalbuilding....................................................................................................54

4.4.1. Insitutomographyofthefluidmovementinsiderocks:applicationtohistoricalbuildingconservation......................................................................................54

4.5. Biology.....................................................................................................................57

4.5.1. Investigatingthecontinuousdentalreplacementofmammalsthroughanewrodentmodel...................................................................................................................57

4.6. Paleontology(foraminiferatomcat).......................................................................60

4.6.1. Morphologicalcharacterizationoffossils.......................................................60

5. BEAMLINECONCEPT,LAYOUTANDREQUIREMENTS.....................................................62

5.1. Technicalrequirements...........................................................................................62

5.2. Source......................................................................................................................63

5.2.1. Sourceproperties............................................................................................63

5.3. MultilayerandSi(111)monochromators................................................................65

5.4. Beamlinelayout.......................................................................................................68

5.5. Experimentalendstationanddetectionsystems...................................................69

5.5.1. Samplepositioningsystem:.............................................................................69

5.5.2. Imagingsystems..............................................................................................72

5.6. Sampleenvironment...............................................................................................75

5.6.1. Tensile,compression,fatiguetestrigs............................................................75

5.6.2. Hightemperaturefurnace...............................................................................77

5.6.3. Cryogeniccell...................................................................................................79

5.6.4. Highpressurecell............................................................................................80

5.7. Computationanddatastorage...............................................................................80

5.8. Estimatedbudget....................................................................................................82

5.9. Futuredevelopment................................................................................................83

6. REFERENCES....................................................................................................................84

ANNEX1.LettersofsupportfromSpanishcompaniesandrelevantinstitutions..................89

TABLE OF FIGURES

Figure1.Tomographicmethodsspanningover9ordersofmagnitude[11]........................................13

Figure2.Scientificproductionconsideringsynchrotrontomographyoverthelast20years(a)Numberof indexed publications (b) Cites per year, total number of cites and hindex for synchrotrontomography. (c)Scientificproduction considering synchrotron tomographyanddiffractionover thelast20years.Thenumberofpapers isnormalized to themaximumnumberofpaperperyear. (d)Relativenumberofpaperfordifferentspecifictomographictechniques(normalizedtothemaximumnumberofpaperperyear).(e)Publicationbysubjectforsynchrotronmicrotomography.Source:WebofScienceandScopus............................................................................................................................15

Figure 3.Map of Europe including the list of European Synchrotronswith available tomographictechniques..............................................................................................................................................19

Figure4.GeographicdistributionofthesupportingclusterintheIberianterritory.............................22

Figure5.Detailof the stirringheadover the kaptonmould containing the isocyanate and polyolblendsbeforethemixingprocess..........................................................................................................24

Figure 6. Volume rendering at different instants for the two examinedmaterials (TOP: pure PU;BOTTOM:PUwith3%wt.nanosilica)at(a)9.8s,(b)21.7s,(c)26.3sand(d)32.6s).............................25

Figure7.Left: Insitucelldensityevolutioncomparedmodels.Right: Insitucelldiametercomparedwiththetheoreticalmodels...................................................................................................................26

Figure8.ReconstructedtomographicslicesobtainedduringinsitusolidificationofAlMg4.7Si8atthetemperaturesatwhichconsecutivesolidificationofthedifferentphasesisobserved,[38]................28

Figure9.a) tod): rendered3D imagesof theAldendriticsolidificationatdifferent temperaturesduringcoolingofanAlMg4.8Si7alloyobtainedinsitubySXCT.e)toh):distributionofthemeanandGauss curvatures of the surface of the Al dendritic structure at the different stages of thesolidificationprocess.[38]......................................................................................................................29

Figure10:Bubblesize,wallthicknessandinterconnectionfrombasalticfoams[53]...........................30

Figure11:Differentpyroclasticmicrotexturesfromsilicicmelts.Bubblesappearsegmented[56].....31

Figure12.(a)3Ddesignand(b)topphotographofthelasersystemmountedonTOMCATbeamlineatSLS.Trangeis4001700C[58,59].........................................................................................................32

Figure 13. ac 3D rendering of acid melt at different temperatures (bubbles); d) bubble sizedistributionsatdifferenttemperatures;e)bubbleanisotropyandfractionversustemperature[59].33

Figure14.Evolutionbubblesinbreadduringproofing:(a)2Dimagesofhorizontalsections(diameter9mm)extractedfromreconstructedvolumes(628x628x256voxels)(b)and(c)Voidvolumefractionandaveragecellwallthicknessforthreedifferentdoughs[68]............................................................34

Figure15.(upperleft)Synchrotronradiationtomography:phasecontrastslicesofthefruitcortexofapple (left) and pear (right); cell walls are indicated by arrows. (lower left)Modeled (a) againstmeasured(b)3Dgeometryofapplecortexcells.(Right)Theoxygenconcentrationprofileinsidecellsusingfiniteelementsimulations.Drivenforcewaspartialpressureacrosstheboundariesofthetissue.Thepartialpressureandconcentrationinsidethetissuewasrelatedbytheuniversalidealgaslaw[65].................................................................................................................................................................35

Figure16.Evolutionof time resolution for insitu synchrotronXray radioscopyapplied tovisualizemetalfoaming........................................................................................................................................36

Figure17.SeriesofradiographsofanAlSi10+0.5wt.%TiH2foamat640Cextractedfromaninsitufast synchrotron Xray radioscopic analysis. The coalescence of two bubblesmeasuredwith 9.5sframe interval (105kfps) can be observed.Dashed lines indicate the contours of the bubbles andarrowsindicatethecorrespondingrupturedcellwall...........................................................................37

Figure18.Tomographicvolumes revealing thecavitiesatdifferent timesduring thecreep test. (a)initialcondition,(b)middleofthetest,(c)closetofracture.................................................................38

Figure19.Shapeevolutionofthethree largestcavitiesexhibitingcoalescence. Thedifferentstagescorrespondtothelargestporebeforecoalescence...............................................................................39

Figure20.Evolutionofthespatialorientationofcavities......................................................................40

Figure 21. Damage propagation in 45 plies. Different crack colours indicate their connectivity(adaptedfrom[17])................................................................................................................................42

Figure22.Experimentalsetuptostudy insituthe infiltration processattheP05beamlineofDESYSynchrotron............................................................................................................................................43

Figure23.(a)Crosssectionofthescannedfibertowspecimeninthevacuumbag.Wetglassfibersaresurroundedbythelightergreycolor.(a)3Dreconstructionoftheinfiltratedtow...............................44

Figure24.3DstructuresofaluminidesandSiafter4hofsolutiontreatment:a)SiinAlSi12,b)Siandaluminides in AlSi12Ni, c) aluminides in AlSi10Cu5Ni1, d) aluminides in AlSi12Cu5Ni2, e) Si inAlSi10Cu5Ni1andf)SiinAlSi10Cu5Ni2..................................................................................................46

Figure25.Proofstress0.2at300Cfortheinvestigatedalloysasafunctionofthesolutiontreatmenttime........................................................................................................................................................47

Figure26.Top:scanningelectronmicrographsoftheinvestigatedmaterialsBottom:portionsofslicesofholotomographyreconstructionsofthe investigatedmaterials.From lefttoright:AlMg7Si4alloy,Ti1023alloyandTi64/TiB/5w.................................................................................................................49

Figure 27. Rendered volumes of the investigatedmaterials: a) interconnected SiMg2Si structure(green)inAlMg7Si4;b)largerparticlesremainingfrompreforging(blue)andindividualsecondarygrains (semitransparentgreen) inTi1023; c)TiBneedles (green)and irregularly shaped grains inTi64/TiB/5w(othercolours)...................................................................................................................50

Figure28.Phasecontrast imagingofwhole (rodent)hearts.Beside the anatomicaldetail atorganlevel,thedetailedfibrestructureinwhichmyocytesareorganisedcaneasilybeassessed.Additionally,vesselscanbeobservedandextractedusingcomputationaltools[89]................................................51

Figure29.Imageofapretermrabbitpupthorax,focusingontheair/lungtissueinterface[90].........51

Figure 30. Spatial resolution of histology, Xray phase tomography, and MRI microscopydemonstratingthatresolutiondecreasesfromhistologyviaPCmCTtomMRI[91].............................52

Figure31.AfalsepositiveMRIpostmortem,suggestinglungchangeswhilehistologywasnormal....52

Figure 32. Breathing activity and the increase in endexpiratory lung gas volumes from birth in aspontaneouslybreathingnewbornrabbitpup.PhasecontrastXrayimageswereacquiredatthetimesindicatedbythearrowsdemonstratetheincreaseinlungaeration[94]..............................................53

Figure33.a)Uniformdistributionofthemineralsexcept in ironoxides layers(atthebottom).b)(1)voidspaces;(2)finegrainedcarbonates;(3)largegrainedcarbonatesand(4)claysandironminerals.................................................................................................................................................................54

Figure34.a)CTimagesshowingthevariationinwaterpenetration.b)3Dimagesoftheopenporosity.................................................................................................................................................................55

Figure35.CTimagesatdifferenttimesduringtheabsorptiontest.ThepositionsofnineROIsusedtoquantifythewaterpenetrationrateareindicated................................................................................56

Figure36.EvolutionofthemeanCTnumberoftheinternalROIs......................................................57

Figure37.a)Foresideofacaptivesilverymolerat,b)3Dreconstructionandc)Virtualcrosssectionoftheupperdentitionofanadultsilverymolerat....................................................................................58

Figure 38. a) 3D reconstruction in lateral view of a lower tooth row and b) model of dentalreplacementofthesilverymolerat.c)3Dreconstructioninlateralviewofalowertoothrowandd)modelofdentalreplacementofthepygmyrockwallaby(greenarrows:molarprogression;redarrow:toothloss)...............................................................................................................................................59

Figure39.RightchelalfingersofaPseudogarypussynchrotron[103]fossiltrappedinamber............61

Figure40.HorizontalphasespacedistributionoftheWS400source....................................................64

Figure41.Horizontalspatialfluxdistributionofthesourcefor4photonenergies,forlowenergiesaparasiticsidelobeappears.....................................................................................................................64

Figure42.Photonsourcedistributionfor(verticalandhorizontal)forthreephotonenergies............65

Figure43.Fluxemittedwithinahorizontalacceptanceof1mrad,fortheproposedsourcecomparedtoabendingmagnet..............................................................................................................................65

Figure44.Bragganglefora4nmmultilayermonochromator,andforaSi(111)crystalpair...............66

Figure45.Verticalsizeoftheilluminatedarea(DoubleMultilayerMonochromator=DMLM)...........67

Figure46.Sampleilluminationareafortwodifferentvaluesoftheenergy.Thestripesarecausedbytheslopeerrorofthemultilayer(ML)mirrors.......................................................................................67

Figure47.Schematicopticallayoutoftheimagingbeamline................................................................68

Figure48.LayoutoftheImagingbeamlineattheALBAExperimentalHall...........................................69

Figure49.ZoomedphotographyofasystemsimilartotheoneintendedtoinstallatAlba(CourtesyofPIMicosIberia)........................................................................................................................................71

Figure 50. Schematic description of the twomicroscopes considered to bemounted at FaXToRbeamline.................................................................................................................................................72

Figure51.Left:3DrenderingofthewhitebeammicroscopemountingaPCO.Dimaxcameraontop.Right:photographyofaPCO.DimaxHScamera....................................................................................73

Figure52. Left:3D renderingof themonochromaticbeammicroscopemounting aPCO.Edge4.2cameraontop.Right:photographyofaPCO.Edge4.2.........................................................................75

Figure 53. 3D CAD rendering of a tensile/compressive test rig compatiblewithmicrotomographyexperiments............................................................................................................................................77

Figure 54. Cross section of the radiation furnace (right) and 3D rendering of the system (left).Differentpartssuchasrotaryfeedtrough,parabolicreflectorsandportscanbeobserved.................79

Figure55.Conceptualdesignof thehighpressure setup including themain componentsand thesupport...................................................................................................................................................80

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1. ABSTRACTTheFaXToRinitiativehasbeeninitiatedfromtheinterestandsupportofaclusterof

Spanishscientistscoveringawiderangeofdisciplinesfromfundamentaltoapplied

research.Oneofthekey issuesthatmotivatetheseresearchers isaccessingtothe

internal microstructure of their problemsubstances and investigating about the

dynamicprocessesoccurringinthem.SynchrotronXrayimagingis,nowadaysoneof

themostusedtechniquesforthispurpose.Ontheonehand,fastXrayradioscopy

allow understanding dynamic processes taking place in short times (mili and

submilisecond range) combining the fast imaging acquisitionwith the penetrating

powerofXrays,althoughwiththelimitationofa2Dimagesequence.Ontheother

hand, synchrotron tomography provides a way for visualising and analyzing the

threedimensionalinteriorstructureofrealobjectsnondestructivelyandwithahigh

spatialresolution. Inrecentyearsdifferentbeamlines inEuropehavefocusedtheir

developments towards3D+tor4D techniques (combinedwith in situapproaches)

with the objective of achieving a new technique, real time tomography,which

combines3Dspatialresolutionsoffewmicronsandtemporalresolutionsbellowthe

second.

This proposal is oriented to the creation of future fast imaging beamline at Alba

synchrotron which may cover the demands, not only of the Spanish scientific

community but also the European ones. The instrument is conceived as amulti

purpose system thatmay allow the realizationofdiverse imaging techniques that

willbeexplainedanddeveloped in thisproposal. In theproposalwealsoconsider

the future development of the instrument aiming at extending the number of

availabletechniquesintheincomingyears.

Webelievethatthecreationofanimagingbeamlinewithpossibilitiesofdeveloping

3D, insitu, and real time studies constitutes a strong opportunity for Alba

synchrotron for offering an alternative to a highlydemanded technique for

europeanusers.

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2. INTRODUCTION

2.1. ImportanceofXrayimagingandtomography

Several fieldshaveexperienced importantprogressover the lastdecadeswith the

development of threedimensional (3D) characterization techniques. The

understanding ofmaterials, animals, fossils, objects, etc. has gradually increased

aided by the development of methods that provide as complete and unbiased

descriptionofmicrostructureaspossible.Fromthe3Dmicrostructure,quantitative

information in three dimensions can be retrieved usingmethodologies based on

image analysis techniques. 3D data provides access to some very important

geometricandtopologicalquantitiessuchussize,shape,orientationdistributionof

individual features and that of their local neighbourhoods, connectivity between

features and network, composition, etc. Some of these quantities cannot be

determinedapriorifromclassicalstereologicalmethodsthatuseonly2Dimagesor

atthebestonlysemiquantitativelyestimationsarereached.Besides,thepossibility

toconductinsitu3Dcharacterizationofdynamicexperimentsisexpandingourview

on fluid flow inporoussystems,metalmicromechanicsor thearchitectureof food

texture,tonameafew.

Experimentalmethods that enable 3D characterization have undergone dramatic

improvementsinthepastdecadedue,inlargepart,toadvancesinbothcomputing

powerand visualizationandanalysis software thathavebeenenabling factors for

both the acquisition and interpretation of these massive data sets. Several 3D

characterization techniquesareavailable forscientists that span from theatom to

the macroscopic engineering or natural components. Some examples are Atom

ProbeTomography(APT)[1],electrontomography[2,3],neutrontomography[4,8],

3DXraydiffraction(3DXRD)[5,8],serialsectioning(OM,FIBSEM,3DEBSD)[6,7],X

ray tomography (XCT) [812],amongothers.Thevarietyof3D imagingmethods is

large, and theydifferby theprobing rays theyuse,by thephysicalquantity they

measure and by themathematical reconstruction technique they are based on.

Figure1showssomeofthecommonlyusedcharacterizationmethodswhichcovera

range of different resolutions and sample sizes (beginning and end of the bar

respectively)overnineordersofmagnitude[11].

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Figure1.Tomographicmethodsspanningover9ordersofmagnitude[11].

2.2. VirtuesofXraytomography

Absorption contrastXray computed tomography (XCT) isprobably themostwell

known 3D xray imagingmethod. In thismode it ispossible todetectdifferences

between xray absorption coefficients of different phases, provided they are

different enough. This technique can be carried out with lower energy beams

available on desktop instruments (for relative low density specimens). Indeed,

commercial XCT instruments with resolution in the order of micrometers, have

proliferated rapidly in recent years. Synchrotron radiation, on the other hand,

provides the largest number of experimental options for tomography based on

imaging (absorption tomography, phasecontrast tomography, holotomography,

laminography, nanotomography, aborption edge tomography) as well as using

diffraction (3D Xray diffraction microscopy 3DXRD, diffraction contrast

tomography DCT), among others. One reason is the extraordinary brilliance of

thirdgeneration synchrotrons, many orders of magnitude higher than that of

conventional Xray tubes. This characteristic allows the possibility of selecting a

narrowenergyband(usingmonochromators)andstillhavingasignificantfluxoruse

pinkorwhitebeamsifhigherfluxesarerequired,dependingontheapplication.Also,

the high coherence of synchrotron Xray beam allows us to exploit the phase

Page14of97

interactionwithobjectsof this radiation.SXCTalsoprovidesa rangeof resolution

(Figure1) thatcanbeused tostudy the3Dmicrostructureand featuresofawide

varietyofmaterialsandhavebeenasubjectofstudyindifferentpublications[9,13

22]. Other virtues are deep penetration, nondestructiveness (which provides

temporal evaluation possibility), simple sample preparation and the possibility to

providechemicalinformation.

2.3. DevelopmentofSXCTinthelastdecades

Synchrotron Xray computed tomography (SXCT) has experienced a rapid

developmentoverthe last15yearsachievingconsiderable improvements inspatial

andtemporalresolution,volumereconstructionspeedand3Dmethodsofanalysis

thatallowsquantitativeanalysisofthetomographicdata.AsaconsequenceXCTand

SXCT areprogressivelybecoming an accepted tool for scientists and industry as a

reliableandprecise3Dcharacterizationtechnique.Thisstatementcanbeconfirmed

if we observe the scientific production directly related to synchrotron

microtomography during the last decades (Figure 2). The consolidation of the

techniqueisbothintermsofindexedpublicationperyearandvisibility(Figure2ab),

contributing directly to high impact scientific results (Figure 2b). In parallel, the

particular interestof thescientificcommunity inusingSXCT fordifferentpurposes

has leadtoabeamtimeoverwhelmingdemand inmostSXCTbeamlinesacrossthe

world reachinganoverload factorofnearly3 (higher inparticularbeamlines) ina

short time. Interestingly the comparisonwith theuseofdiffraction techniques at

synchrotron facilities reveals that relative productivity has become similar, as

scientificinterestontomographyhasgrownwithyears(Figure2c).

Regarding the scientific production of specific techniques, nanotomography (or

zoomtomography) and insitu 4D tomography are probably themost interesting

developmentsand,asaconsequence,twoofthemostusedtomographictechniques

for the scientific community,highly increasing thedemandof these techniquesat

thesynchrotrons(Figure2d).

AnotherimportantstrengthofSXCTistheversatilityofthetechniquedepictedinthe

multidisciplinary origin of the scientific production (Fig. 2e). This feature strongly

Page15of97

contributes to the expansion of instrumental development and experimental

environmentsavailableatSXCTbeamlines.

Figure2.Scientificproductionconsideringsynchrotrontomographyoverthelast20years(a)Number

ofindexedpublications(b)Citesperyear,totalnumberofcitesandhindexforsynchrotron

tomography.(c)Scientificproductionconsideringsynchrotrontomographyanddiffractionoverthe

last20years.Thenumberofpapersisnormalizedtothemaximumnumberofpaperperyear.(d)

Relativenumberofpaperfordifferentspecifictomographictechniques(normalizedtothemaximum

numberofpaperperyear).(e)Publicationbysubjectforsynchrotronmicrotomography.Source:Web

ofScienceandScopus.

(e)

(d)

(c)

(b) (a)

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2.3.1. 4Dtomography

4D tomography refers to the possibility to perform a repeated series of 3D

topographies at sequential time lapses, providing information about the

microstructureevolution.This isoneofthemostattractivefeaturesofSXCT.Asan

exampleinmaterialscienceandexperimentalmechanics,theevolutionofstructure

canbe very importantduringmanufacturing [9], service lifeand inunderstanding

failuremechanisms[17],aswellasinunderstandingtheprocessofbreadmaking[28],

and is proven to be a valuablemethod in other areas, too. One very important

characteristicof4Dtomography isthetemporalresolutionthatcanbeachieved in

the measurement of one tomogram. In many cases, fast acquisition time are

necessary, normally at expenses of spatial resolution;while in others,when the

microstructure is quasistatic, longer measurement times with better spatial

resolutionareaffordable.

4Dtomogramscanbecarriedout inseveralwaysdependingon itsapplication.Ex

situapproachescanbeused for longtermtreatmentappliedtothesamesamples

providedtheydontneedtobecutfortomographicmeasurements.Someexamples

ofthatarecorrosionstudies,exposuretomoistureandcertainheattreatmentsthat

cannotbecarriedout insitu. Insomecaseswhen thesamplesare larger than the

field of view (FOV) of the detector the evolution of features are evaluated on

differentsamplesatdifferentconditions (becausespecimenshavebecut)and the

extracteddataaretreatedinastatisticalwayasfunctionoftime.Anexampleofthat

is longterm creep studies,manufacturingdefectsormicrostructural changes,etc.

Perse,4Dtomographyprovidestheevolutionofaspecificfeatureasafunctionof

time,which insomespecificcasescanbe linkedtoanothervariable (temperature,

pressure,strain,etc.).Thecombinationof4Dtomographywithinsitudevicesopens

upothernewpossibilitiesandfieldsofresearch(seesection2.3.2).

Surfaceobservationcanbeausefulapproach,butinmanycasesstructuralchanges

occur in the bulkmaterial at hidden view. 4D tomography allows following the

structure evolution nondestructively in 3D manner. A significant amount of

informationcanbeobtainedonly fromvisualizationoftheeventsthatoccur in3D

over a time lapse, but in most of these cases quantitative information is also

Page17of97

required. Increasingly,thenewtrend istoobtainquantitative informationfrom3D

and 4D tomography. This allows to understand the heterogeneities of the

microstructurein3Dand4D,andtoevaluatethepredictivecapabilityofanalyticalor

numerical models to describe behaviour and predict the kinetics of a certain

mechanism. To that end, several approaches for quantitative analysis are been

developed, suchasdigital volume correlation (DVC) [9,23,24],3Dparticle tracking

(3DPT)[9,25,26],howevertheirapplication isstillscarce.Itseemsnaturalthatwith

the increase inapplicationsthesemethodsornewoneswillbecomemoreefficient

and with improved accuracy. Recently commercial codes have become available

whichwillsurelyacceleratethedisseminationofthetechniqueeventotheindustry.

2.3.2. Insitutomography

Another approach is to carry out insitu studies in devices that are specially

developedforthatpurpose.Initially,theyweredevelopedbytheusersandbrought

tothebeamlinefortheexperiment,butthisalsocreatescompatibilityproblemsand

leadtoimportanttimelossesduringthebeamtimesonowadaysitiscommontofind

someofthesedevices(miniaturizedfurnaces,heatingorcoolingstages,tensileand

compression rigs, etc.) at the synchrotron beamlines available for the users.We

believe that an important asset for any tomographybeamline is thepossibility to

carryoutinsituexperimentsofdifferentkindusingspecialdevicesthat,atthesame

time, must be flexible in their configuration according to the high variance of

applications. Inouropinion,theproposedbeamlineshouldprovidetheuserssome

ofthesedevicesfor insitutesting,namelytensileandcompressiontestingrigwith

temperatureregulation,ovensand/orheatingstages.Someotherlesscommonbut

emergingdevicesarepressureanvils,hightemperaturedilatometers, infusion rigs,

fatigue testing rigs, corrosion cells, etc. Of course some of them could even be

combinedtoprovideanevenbroaderspectrumoftesting.

TomographictemporalresolutionisanissuestilladdressedbyonlyafewEuropean

synchrotrons,while inotherstheacquisitiontime isstill intheorderofhours.The

increase in temporalresolution isopeningupasetofpossibilities for tomographic

imaging applications that cannot be studied easily by othermeans. Considerable

Page18of97

improvementshavebeenmadeinrecentyearsbycombiningtheveryintensewhite

(or pink) beams at synchrotron sources with a new generation of highspeed

camerasandnewtypesofscintillators.Timescalesforonetomographyisnowadays

intheorderoftensofmilisecons[27],allowingstudiesinmanydifferentfieldssuch

as food (breadmakingorbeer foam) [28,29]or inmaterialscience forcoarsening,

melting,solidificationofsemisolidmetals,aswellasdamageassessment.

2.4. Scopeofthisproposal

Thisproposalmobilizestheexpertisefromspecialistsfromdifferentfields(material

science and engineering from polymers to nickel superalloys, bioscience, food

science,earthscience,palaeontology,volcanology,metrology,etc.) topropose the

design of an Xray imaging beamline that provides a high resolution tomography

instruments that will permit to carry out different modalities (absorption,

absorptionedge, phase contrast and holo tomography) with optimum temporal

resolution with expected times per tomography below 1 second. Except for

absorption mode (without considering the exceptional expected speed at the

beamline) theother3 lastmentioned tomographic techniquesarenotavailable in

conventionallaboratorysources.Ofcourse,itcouldbealsopossibletocarryoutfast

radiography experiments, over 500 images per second, in those caseswhere 3D

resolvingpower isnot required.Thebeamline concept is completedbyproposing

different insitudevices thatwillbeavailable forusers. In this field, it isbecoming

clearthat,allowingtheobservationofthe interiorofasamplewithoutrequiringa

specific (andpossiblybiasing)preparationprocedure,Xraytomography isthebest

way to obtain reliable information on themicrostructure and its evolution, also

underdifferentloadings(e.g.mechanicalorthermal).

Considering the versatility of the instrument, the combination of different

tomographic techniques and the availability of insitu devices make this future

beamlineattractiveforalargenumberofpotentialusersfrommanydifferentfields,

which makes SXCT an essential technique in a synchrotron. Such tomographic

beamlinewillprovideavaluableasset to thescientificcommunity thatwillattract

researchers frommany different areas not only from Spain but from the rest of

Europe.

Page19of97

3. THESPANISH(ANDEUROPEAN)USERCOMMUNITY

3.1. CurrentpanoramaofSXCTinEurope

In Europewe can find 8 different synchrotronswith beamlines oriented to Xray

tomography(softXraymicroscopy,nanotomographyandnonimagingtomography

difraction, fluorencence,etc.havenotbeen included in this selection).Figure3

show their location in Europe (3 in Germany, 2 in France, 1 in UK, Italy and

Switzerland). According to this list, other synchrotrons in Europe have not been

considered (e.g. Alba) since they do not have any beamline dedicated to Xray

tomographyinthetermspreviouslymentioned.

Figure3.MapofEuropeincludingthelistofEuropeanSynchrotronswithavailabletomographic

techniques.

Complementarily, Table 1 lists the name of these beamlines, together with the

availabletomographictechniquesandtheenergyrange.Fromtheseresultswecan

state that a total of 12 beamlines in Europe are currently dedicated to Xray

tomography and have developed different tomographic techniques.Nevertheless,

theyarenotmany ifwecompare themwithdiffraction,XANES,orXASbeamlines

presentinEuropeinthedifferentsynchrotrons.Actuallytheoverloadfactorofthese

beamlines is,byfar,higherthanotherstypesoftechniquesandtherefore itwould

be interesting to complete the current European offer of SXCT with a new

tomographic beamline at Alba. It is also important to mention that only two

beamlines have oriented their developments to fast tomography. In this sense

Page20of97

TOMCAT (SLS) [27] and ID19 (ESRF) [30] are currently the leaders in this aspect

reachingupto20tomogramspersecond.TheFaXToRproposalaimsatofferinga

new beamline for the realization of Fast Xray Tomography and Radioscopywith

specialemphasisforinsitustudiesand,thus,completingthecurrentofferforSXCT

inEurope.

Table1.XraytomographyimagingbeamlinesavailableinEurope

Beamline Synchrotron Tomographytechniques ENERGY(keV)

IMAGE ANKA

2D:microscopy,radiography,topography,andmicrodiffractionimaging

3D:tomographyandlaminographywithmonochromatic,pinkorwhitebeam(highcontrasttoultrafast)Notavailableforusersyet

765

TOPOTOMO ANKA WhitebeamXraytomography(submicrometer)Phasecontrastimagingwithgratinginterferometer. 640

BAMline BESSYII MonochromaticTomography(Si111andmultilayer),WhitebeamTomography. 590

I12JEEP DIAMOND WhitebeamXrayTomographyPhasecontrastimaging. 50150

DiamondManchesterImagingBranchline DIAMOND PinkTomographyandMonochromaticTomography. 830

SYRMEP ELETTRA MonochromaticTomography(Si111)WhitebeamTomography. 835

ID16ANanoImagingBeamline ESRF NanoTomography 17.033.6

ID19Microtomographybeamline ESRF

MicroTomography,phasecontrast,holotomography(res.:0.330m).Fasttomography(fewsec.).

DiffractionTopography6.0100.0

IBL(PE05) PETRAIIINanoTomographyMicroTomography

(Absorption&PhaseContrastTomography)550

HEMS(P07) PETRAIII XRD,SAXS,3DXRD,Tomography with1mfocus(basedonabsorptionandphasecontrast) 30200

TOMCAT SLS

AbsorptionbasedTomographicMicroscopy;PropagationphaseContrastTomographicMicroscopy

DifferentialPhaseContrast(DPC)Tomographicmicroscopy

AbsorptionandphasecontrastnanotomographyUltrafasttomographicmicroscopy.

845

PSICH SOLEIL MonochromatichighenergyresolutionTomographyMonochromatichighfluxTomography.

15100keVwhitebeam(lowenergyfiltered)

1550keVmonochromatic

3.2. PotentialusersinSpain

InthepreparationofthisproposalwescannedtheinterestoftheSpanishscientific

communityinthistechniquebycarryingoutamailingsurvey.Asaresultofthispoll,

morethan25Spanishresearchgroupswereinterestedinthistechniqueanddecided

to support thisproposal.Table2 lists thegroups, the institutionand the research

interestobtainedfromthementionedsurvey.Oneofthemaincharacteristicsofthis

Page21of97

supportingclusteristheirmultidisciplinarityconsideringthehighvarietyofresearch

interests they represent,which actually provide an addedvalue to this proposal.

Figure4 shows thedistributionwithin the Iberian territoryof the groups listed in

Table2.

Oneof themainconclusionsof the survey is thatwebelieve there isa significant

criticalmass of groups thatwill be demanding this technique at Albawhen the

beamline isready.Additionallyweareprettysurethatmanyotherresearchgroups

andcompanieswillbecomeuserswhentheycouldseetheresultsobtainedbyother

groups/colleagues.Finallywehavetoconsiderthatitisexpectedthatthisbeamline

willbealsorequestedbyEuropeanusersasitwillbeanalyzedinnextsection.

Table2.SpanishresearchgroupssupportingtheFaXToRproposal

Leader Group/Institution Interest

J.GmezBarreiro U.Salamanca HighpressureandtemperatureofgeologicalmaterialsR.CamposEgea CIEMAT GeologicalmaterialsJ.CostaBalanzat U.Girona CompositeMaterials

J.C.Glvez UPolitcnicadeMadrid FractureofSteelsandCementbasedmaterialL.E.Hernndez U.AutnomadeMadrid Vegetalmaterials

J.Snchez (IETccCSIC) Structures,concreteM.Lanzn U.PolytechnicalCartagena Buildingmaterials,stone,patrimonialbuildings

D.A.CendnFranco U.PolytechnicalMadrid MetallicmaterialsF.SanJoseMartinez U.PolytechnicalMadrid Soilstructure

F.A.Lasagni CATEC CompositematerialsandmetalalloysV.GomezRuiz U.Oviedo GeomaterialsG.GarcsPlaza CENIM MultiphasemetallicmaterialsJ.A.Yage U.Zaragoza Metrology,Imagetreatment

L.FrancoFerreira Aimen NDT,dimensionalmetrology,materialcharacterizationA.Mendikute IDEKO Imagetreatment,nondestructivetestingJ.vanDuijn U.CastillaLaMancha SolidOxidesbateriesV.Amig U.PolitcnicadeValencia Titaniumalloyscharacterization

C.Capdevila CENIMCSIC Febasedalloys,steelsL.Galdos U.Mondragon SuperPlasticFormingofAluminiumSheets.P.Bravo U.Burgos HPDCofMgalloys,polymers

J.C.SurezBermejo U.PolytechnicalMadrid Structuralhybridmaterials,adhesivos,damagingM.A.RodriguezPrez U.Valladolid Cellularmaterials,Xraytechniquedevelopment

D.Val GRUPOANTOLINIRAUSA,S.A. MagnesiumandaluminiumalloysR.ArenasMartn U.ComplutensedeMadrid HighpressuremetamorphicrocksF.J.SierroSnchez UniversityofSalamanca Micropaleontology

SrenJensen UniversityofExtremadura PaleontologyGroup

I.Rosales SpanishNationalGeologicalSurvey Geology

G.GarcsPlaza CENIM MultiphasemetallicmaterialsA.lvarezValero UniversityofSalamanca Volcanology

Page22of97

J.R.MartnezCataln UniversityofSalamanca TectonicsygeophysicsA.RodrguezBarbero UniversityofSalamanca Renalandcardiovascularphysiopathology

P.Ayarza UniversityofSalamanca Geophysics:SeismicyMagnetismsJ.MBentezPrez UniversityofSalamanca microstructurecharacterization

E.GonzlezClavijo SpanishInstituteofGeologicyandMines Tectonicsandnaturalresources

M.SurezBrrios UniversityofSalamanca CrystallographyandMineralogyC.Gonzlez IMDEAMaterials Fibrereinforcedpolymers

T.PerezPrado IMDEAMaterials LightmetalalloysJ.Molina IMDEAMaterials MicroandNanomechanicsmetallicF.Sket IMDEAMaterials FRP;lightmetalalloys;steels

Figure4.GeographicdistributionofthesupportingclusterintheIberianterritory.

Page23of97

4. RELEVANTSCIENTIFICCASES

Xrayradiographyandtomographycanbeappliedtoseveralscientificandindustrial

fields, therefore it isnoeasy toorganize the researchareas inwhich tomography

wasor couldbe applied.Wehave subjectively selected some research categories

whichinsomecasesthescientificcaseswilloverlapothercategories.

4.1. MultidisciplinaryFasttomographyandradiography:insitustudies

Inmanyresearchareas,evolutionofthestructureisofprimeimportance.Asanon

destructivetechnique,XrayCTcanprovideaverydetailedpictureoftheevolution

of the structure/damage through a certain processes applied to a material.

Furthermore the opportunity to host environmental stages means that

structure/damage canbe followed in situunder a rangeofdemanding conditions

representative of those experienced in reality. Consequently SXCT enables the

quantificationofaverywiderangeofstructuralchangesanddamagemechanisms.

Someexamplesarepresentedbelow.

4.1.1. Bubblenucleationandgrowthcharacterizedbyultrafasttomography

The use of Xray tomography brings the possibility of performing detailed

characterizations of the cellular structure of foam specimens in three dimensions

(3D)although ingeneraltomographiesareacquired instaticconditions. Inevolving

systemsitwouldbeexpectedthatthehighnumberofprojectionsandtherelatively

long exposure time neededmay output blurred tomographies. Thanks to the last

developmentsatsynchrotronbeamlinesnowadays it ispossibletocarryouttime

resolved Xray tomography studies reaching time resolutions unimaginable a few

yearsago[29].

This study uses synchrotron timeresolved Xray tomography to understand the

effectofnanoparticlesonthebubblegenerationnucleationanditslaterevolution

growthofa reactivepolyurethane foam formulation.The time resolutionof the

performed experimentswas 156ms per tomographic scan (near to 10Hzmicro

Page24of97

tomography) and a total number of 90 tomographies during the foaming process

whereacquired.

Acommercialbicomponentpolyurethane(PU)formulationfromBASFwasselected

for this investigation. The turbulentmixing of two liquids (polyol and isocyanate)

promotesasimultaneousblowingandgellingreactionthatresultsintoasolidfoam.

The density of the foam in a free foaming process is 52 kg/m3. The nucleating

nanoparticleselectedforthisinvestigationwashydrophobicfumedsilicaandtothis

end3%wt.ofsilicananoparticleswereinitiallydispersedfor120sintheisocyanate

compound.

Aspecificsetup(Figure5)wasdevelopedtomixtheisocyanate(neatformulationor

the blend containing the particles)with the polyol in the same rotating table in

whichthesequencesoftomographiesweretaken.Thisallowsobtaininginformation

fromthe initialstagesoftheprocess.Thepolyoland isocyanatecomponentswere

placed inadedicatedminiaturecylindricalmold (h=40mm,=12mm, thickness=75

mKaptonwalls),attachedtothetomographyrotatingtable.Amotorizedminiature

stirreratthetopwasautomatically immersed inthe liquidsandstirredthemixture

for15 seconds at1500 rpmpromoting theblowing andpolymerization reactions.

Thetomographyscansstarted10secondsaftertheendofthemixingprocess.

Figure5.Detailofthestirringheadoverthekaptonmouldcontainingtheisocyanateandpolyol

blendsbeforethemixingprocess.

Xray tomographic experimentswere performed at the TOMCAT beamline of the

SwissLightSourceatthePaulScherrerInstitute(Villigen,Switzerland).Theultrafast

endstation incorporates a PCO.Dimax camera,which acquires and transfers data

ordersofmagnitudefasterthanCCDcameras.TheopticswerecoupledtoaLuAG:Ce

Foaming mould

Stirrer to mix the components

Rotary stage for the tomographic

experiments

Page25of97

100mthickscintillatorscreen.Magnificationofx4intheopticalmicroscopelenses

wasselectedforthisexperiment.Thiscorrespondstoapixelsizeof3.23.2m2and

a field of view of 6.446.44mm2.Monochromatic Xrays (20KeV, no filter)were

used; generating300projections capturedover180of rotationwith a total scan

timeof156ms.Spantimeof2.5swasusedinbetweenscans.Reconstructionswere

performedbyusingtheGRIDRECalgorithm[31,32]coupledwithParzenfilteringof

thesinograms.

Reconstruction of the tomographic scans allows visualizing, in 3D, the cells

nucleation and growth processes from the early stages in both studiedmaterials.

Figure 6 shows the corresponding 3D renderings for four selected instants (9.8s,

21.7s,26.3sand32.6s.)duringthefoamingprocess. It ispossibletoappreciatethe

highercellsizeintheneatPUformulationandthesmallersizetogetherwithamuch

higherdensityofcellsinthefoamednanocompositecontaininghydrophobicsilica.

Figure6.Volumerenderingatdifferentinstantsforthetwoexaminedmaterials

(TOP:purePU;BOTTOM:PUwith3%wt.nanosilica)at(a)9.8s,(b)21.7s,(c)26.3sand(d)32.6s).

Theanalysisofthetomographicsequencesallowsdeterminingthenumberofcells

percubiccentimetreandtheaveragecellsizeevolution.Figure7,left,showsthecell

density evolution during the foaming process. The results show that the cell

density increases linearly during the first 1015 seconds and subsequently slows

downwithtime. It isalsoclearlyobservedthatthenucleationdensity ishigherfor

thecompositionwith3%wt.ofsilicananoparticlessincethesefillerscouldfacilitate

bubbles formationat solid/liquid interfacesdue toa freeenergybarrier reduction

[33].Ontheotherhand,theexperimentalresultsforthecellsizeevolutionwithtime

(a) (b) (c) (d)

Page26of97

by several authors for the initial bubble radius evolution [34,35]. Bubble growth

stabilizationisnotobservedandthemodellingdoneisthenvalidinourstudysince

the resultspresented here only focus on the first 50s of the expansion. It is also

possible to observe that average cell diameter keeps constant in the very early

instants (t

Page27of97

allowing acquisition times of a complete tomogram in less than one secondwith

voxelsizesdownto~1m[42].

c) The applicability of phase contrast tomography to determine the internal

architectureoflightalloysformedbyphaseswithverysimilarattenuationsuchas

Tialloys,AlSiandAlMgSialloys[4345].

d) The exploitation of Kedge subtraction technique to identify concentration

variationsofdifferentaluminidesinAlcastalloysduringthermaltreatments[46,47].

e) The achievability of subm resolution to reconstruct the architecture of

multiphaseAlandTialloys[44,47,48].

Cast AlMgSi alloys are potential candidates to be used in the automotive and

aerospace industries [49]. The investigation of the kinetics of solidification is

necessary to understand how casting parameters, such as cooling rate and

temperature gradient in the melt, affect the development of the internal

architecture of alloys and consequently determine their resulting mechanical

properties.TheformationandtheevolutionofthemicrostructureofanAlMg4.7Si8

alloy were investigated by in situ synchrotron tomography (SXCT) during

solidification[38].TheexperimentwascarriedoutattheID15AbeamlineoftheESRF

usingapinkbeamandatotalscanningtimeofabout15sforeachtomogram.SXCT

wasperformedeveryminute,whileamoltensamplewassolidifyingatacoolingrate

of5K/min.

Figure 8 shows reconstructed tomographic slices extracted from the in situ

solidification experiment of the AlMg4.7Si8 alloy. The experiment allowed

determiningthesequenceandtemperatureofformationofthedifferentphases,as

wellastheirlocationanddistributionduringsolidification.

Page28of97

Figure8.ReconstructedtomographicslicesobtainedduringinsitusolidificationofAlMg4.7Si8atthe

temperaturesatwhichconsecutivesolidificationofthedifferentphasesisobserved,[38].

Rendered3DimagesoftheAldendritessolidifiedatdifferenttemperaturesduring

cooling are shown in Figure 9a) to d). The colours represent theGauss curvature

between0.005m2and0.005m2,whilethegreypartsareoutofthisrange.Figure

9e)toh)showthedistributionofthemeanandGausscurvaturesofthesurfaceof

the Al dendritic structure at the different stages (temperatures) of the

solidification process. The characteristicmorphologies for the axes and for each

quadrant are indicated schematically Figure 6e). It can be seen that twomaxima

emergeduringsolidification:oneclosertotheoriginrepresentingslightlysaddlelike

shapes,whichare related to thebasesand sidesof the secondarydendriticarms,

and another in the positivepositive quadrant representing spheroidlike regions

owing to the secondary dendrite tips. This indicates that themorphology of the

dendrites during cooling is characterised by coarsening,which is a simultaneous

processofgrowthandcoalescenceofthesecondarydendritearms,similarlytothe

Page29of97

caseofisothermalcoarsening[50].Asthesolidificationadvances,thegrowthofthe

secondarydendriticarmsbecomesasymmetric,thetipsgrowwithahigherratethan

thebases,resultinginadropletlikeshape,wherethetipsofneighbouringarmscan

coalesce[50,51].

Figure9.a)tod):rendered3DimagesoftheAldendriticsolidificationatdifferenttemperatures

duringcoolingofanAlMg4.8Si7alloyobtainedinsitubySXCT.e)toh):distributionofthemeanand

GausscurvaturesofthesurfaceoftheAldendriticstructureatthedifferentstagesofthe

solidificationprocess.[38]

Page30of97

4.1.3. Understanding explosive volcanoes: risk evaluation through

morphometricanalysisofbubblesandcrystalsinlava

About500millionpeopleare livingnearactivevolcanoesand thereforea reliable

evaluationofthenaturalriskinthoseareasisofprimaryimportance.Thepotential

ofexplosiveeruptionhastobedeterminedonthebasisofquantitativeevaluationof

thephysicalprocessesoccurringatcertaindepth in thevolcanicsystem.Access to

those levels is restricted to erupted fragments and indirect measurement from

outside.Inthisline,quantitativemicrotextureanalysisofbotheruptedclastsandin

situmeltingexperimentshasrecentlybecomingthe focusofattentionofgeologist

andgeophysicist sinceexplosivepotentialofavolcanic systemappears tobevery

related to the degassing path ofmelt all through the ascending conduit [53,54].

Throughthedetailedanalysisofbubbleshapesandinterconnection,parameterslike

bubblecoalescenceandtexturalrelaxationareconnectedwiththephysicalresponse

ofmelts [55]. The socalled vesiculationprocesses inmagmasdeterminewhether

theeruptionbecomeeffusiveofexplosive,soboth insituexperimentsandanalysis

of selected natural samples are needed to advance in our knowledge on vesicle

nucleation, growth and coalescence, and their connection with permeability

evolutionofmelts[54].Adependenceofthemicrotexturewithmagmacomposition

has been known atmacroscopic level, but not completely understanding at the

microscopic detail. While basaltic composition seems to evolve towards non

explosiveeruptionasporosityincreases(Figure10,[53]),siliciccounterpartsareless

known,andhencemoreunpredictable[56].

Figure10:Bubblesize,wallthicknessandinterconnectionfrombasalticfoams[53]

Page31of97

Particularlystrikingisthecaseofsiliciceruptionswhichseemstoalternatebetween

violenteruptionsandgentleones. Ithasbeendemonstratedthattheway inwhich

volatiles escape from the shallow part of the volcano conduit, determine such a

behavior[54].Onecriticalissueistounderstandhowbubblesnucleateandgrowin

response to decreasing pressure asmagma rises toward the surface. Synchrotron

microtomography analysis on Kilaueas pyroclast has showed the complexity of

bubblegenerationatdifferentpressuresduring2008eruption[56].Pyroclastswere

imagingatALSsynchrotronfacilityat20keV,200msexposuretimeand1400rotation

steps between angles of 0 and 180. Threemain pyroclastic typeswere found,

which depicted large bubbles (mm) surrounded bymicrometricthick haloes that

containsanelevatednumberofsmallisolatedroundbubbles(radius=2.5m35m,

Figure11A)D)[56]).

Figure11:Differentpyroclasticmicrotexturesfromsilicicmelts.Bubblesappearsegmented[56].

Themicrotexture found in thosepyroclastsrevealsahighdensityofsmallbubbles

withinthehaloes,pointingtonucleationratesrelativelyhigh,butwithlittletimefor

coalescence. This important fact support the ideas thatwater concentrations are

onlyhighenoughinthecloserangeoflargevaporbubblespriortoeruption[56,57].

The existence of a thin region around bubbleswheremeltwith dissolvedwater

occurs. It is an intimate result of preeruption and it is interpreted as a water

Page32of97

reabsorptionback intomagmapriortoeruption.Thosetexturescouldalsobeused

totrackconvectivebehavioratamacroscalewithinthevolcano.

Recent developments include in situ investigation ofmagma vesiculation at high

temperature. Heating systems combined with ultrafast acquisition, like those

implemented inTOMCATbeamline(Figure12ab;[27,58])areofthemost interest

formelt foams research [59]but also in similarmaterialsone.g.managementof

nuclearwaste[60].

Figure12.(a)3Ddesignand(b)topphotographofthelasersystemmountedonTOMCATbeamlineat

SLS.Trangeis4001700C[58,59]

The application of this experimental system to the investigation of vesicles

development inacidmeltsatdifferent temperatures is showed inFigure13, [59].

Interestingly, shape and volume analysis reveals a connection of rigid and soft

behavior of bubbleswithmagma rheology [61], providing crucial parameters for

understanding how the viscosity ofmelts and gas overpressure during degassing

processes controlmagma ascent along volcanic conduits. This is crucial topredict

explosiveeruptionsinthosesystems[59].

Page33of97

Figure13.ac3Drenderingofacidmeltatdifferenttemperatures(bubbles);d)bubblesize

distributionsatdifferenttemperatures;e)bubbleanisotropyandfractionversustemperature[59].

4.1.4. Foodscience:tastingthetexture

Thephysiochemical,functionaland insomecasesnutritionalpropertiesoffoodare

intimately controlled by its microstructure. The quantitative analysis of food

microstructure has become critical in order to understand the physical and

rheologicalbehavioraswellassensoryattributesoffoods.Foodprocessingarenow

changing toward to the microstructure level design and testing, and xray

microtomography is the technique of choice for visualizing those systems.

Microstructural elements such as air bubbles or cells, starch granules, protein

assemblies and food biopolymermatrices contribute greatly to the identity and

qualityoffoods[62,63].

Themicrostructureoffoodhasastronginfluenceovertheattributesofaproductas

evaluated by consumers. Many of those macroscopic properties are poorly

understoodbecauseoftheircomplexnature,derivingfrommultiple interactionsof

processesandfoodmicrocomponents[63].

Page34of97

Example of that interconnection between microstructure and complex

physicochemical processes, and the profound impact of texture on the taste and

flavorquality isfoundmanyproducts likefruit[64,65],bread[28,66,67]andcoffee

[68] to name a fewwith a very high social and economic impact. Both fruit and

bakedproductsshare thestrongdependenceon theircellularstructure thatcould

beoptimized through appropriateddesignduring growth andproduction andwill

determine transport/distribution strategies and midlong term durability of the

product.Inthecaseofbread,3Dimagingthroughxraymicrotomographycombined

withfastacquisitionhasproventobeveryefficientwaytounderstandcellstructure

evolution during proofing time (Figure 14, [67,68]). These results can be used to

improvethedesignandproductionofnotonlybreadbutotherbiopolymericfoams.

Figure14.Evolutionbubblesinbreadduringproofing:(a)2Dimagesofhorizontalsections(diameter

9mm)extractedfromreconstructedvolumes(628x628x256voxels)(b)and(c)Voidvolumefraction

andaveragecellwallthicknessforthreedifferentdoughs[68].

Page35of97

In the case of fruits, the microstructure determines mechanical and transport

properties of tissues. Therefore, a quantitative description of fruit tissue

components in 3D are critical, both to understand the properties and to develop

structure reliablenumericalmodelson them.Figure15 showsananalysisofSXCT

dataonfruittissuefromwhereimportantparameterswereobtained:cellwall,pore

network and cell size. These componentswere then used to design a numerical

model to run multiscale mechanics and mass transfer, thus providing a solid

frameworkforvirtualtissuegeneration,includingcellgrowthmodeling.Thisstrategy

provideaunique tool formoving fromgeometricdescription tophysicalmodelof

fruittissue[65].

Figure15.(upperleft)Synchrotronradiationtomography:phasecontrastslicesofthefruitcortexof

apple(left)andpear(right);cellwallsareindicatedbyarrows.(lowerleft)Modeled(a)against

measured(b)3Dgeometryofapplecortexcells.(Right)Theoxygenconcentrationprofileinsidecells

usingfiniteelementsimulations.Drivenforcewaspartialpressureacrosstheboundariesofthetissue.

Thepartialpressureandconcentrationinsidethetissuewasrelatedbytheuniversalidealgaslaw[65].

4.1.5. Ultrafast2DRadioscopyon cellwall ruptures to studymetal foam

stabilitymechanisms

ThirdgenerationsynchrotronlightsourcesdeliverapolychromaticXrayphotonflux

densityhighenoughtoperformradiographywithmicroresolutioninbothspaceand

time[6972].Therapiddevelopmentof imaginghardware,especially inthefieldof

CMOS sensors, and their continuously improving sensitivity now allows for

extraordinarily high recording speeds, with exposition times down to 1s for a

Page36of97

considerable(atleast1020mm2)fieldofview.TheoptimizeduseofsocalledXray

inline phase contrast (due to the coherence properties of an Xray synchrotron

beam) allows for thebestpossible contrast forour cellularmaterial.Additionally,

radiation hard but highly sensitive and efficient single crystal scintillators such as

LuAG:Ce or YAG:Ce crystals are employed. This permits us to follow the overall

processand resolve insitunotonly slowprocesses (>1msexposure time) suchas

pore nucleation and growth, foam expansion or drainage, or simply observe the

overallfoamingprocess,butalsoveryfastones(1msexpositiontime)suchascell

wall rupture, bubble coalescence, rapid bubblemotions or oscillations. Figure 16

shows the improvement of time resolution for Xray synchrotron radioscopy on

metallicfoamsachievedinthepastyearsasreportedintheliterature[7176].

2000 2002 2004 2006 2008 2010 2012

100

101

102

103

104

105

1

0.1

0.01

1E-3

1E-4

1E-5

0.5 s

Stanzick, Foams & Emulsions, [16] Banhart, AEM, [17] Stanzick, AEM, [18] Garcia-Moreno, APL, [14] Rack, JSR, [15] Garcia-Moreno, ESRF MA 1134

Acq

uisi

tion

rate

[fra

mes

/s]

Year

1 ms

Cell wall rupture,Bubbles coalescence

Foaming behaviour,Process control

9.5 s

Fram

e in

terv

al [

s]

Figure16.EvolutionoftimeresolutionforinsitusynchrotronXrayradioscopyappliedtovisualize

metalfoaming.

Thestabilizationofmetalfilmsorcellwallsinliquidfoamsisakeyissueinmetal

foam science but still not fully understood. To investigate the nature of rupture,

experimentshavebeenperformed inwhich therewasasimultaneousdemand for

both high spatial and high time resolution. It was possible to observe the

coalescenceof twoadjacentbubbleswitha recording speedof105,000fpswitha

frame intervalof9.5s andeffectivepixel sizeof20m.Although the contrastof

Page37of97

suchimagesislowduetotheshortexposuretimeandconsequentlimiteddynamics

oftheimages,itisclearlyvisibleinFigure17thatthecoalescenceoftwobubblesis

completed in~475sandthattheruptureofafilm lastsfor~380s, ifweconsider

theendoftheruptureasthepointwherethecontourofthenewbubblebecomes

straightbeforeitendsasconvex.

Figure17.SeriesofradiographsofanAlSi10+0.5wt.%TiH2foamat640Cextractedfromaninsitu

fastsynchrotronXrayradioscopicanalysis.Thecoalescenceoftwobubblesmeasuredwith9.5s

frameinterval(105kfps)canbeobserved.Dashedlinesindicatethecontoursofthebubblesand

arrowsindicatethecorrespondingrupturedcellwall.

Inthisexperimentsitwaspossibletodemonstratethattherupturetimeofafilmis

dominatedbytheinertiaofthefluidandnotbyitsviscosityasruptureoccurredso

fast [71]. Therefore, it could be demonstrated that stabilization by an effective

viscosityonly,whichwouldbeashighas=0.4Pas (ascalculatedbyGergelyetal.

[77])doesnotapplytometalfoamsofthetypeinvestigatedhere.Otherfactorssuch

as bubble size and alloy compositionmay influence the rupture time andwill be

studiedinfuture.

Page38of97

4.1.6. Insitutomographyofcreepprocessofbrass

The efficiency of electricitygenerating plants in general and gas turbines in

particular increases with increasing service temperature, therefore requiring

components with sufficient hightemperature strength. The lifetime of such

components is usually restricted by creepinduced cavity growth leading to

unacceptablestrainsandfinallytofracture[52].

Synchrotron radiation microtomography provides new possibilities for a non

destructive determination of creep damage evolution in the bulk of samples,

comprising statistical analysis of cavity volume, shape, and orientation evolution

during insitu creep experiments. The results of the experiments enable a

quantitative description of the time dependence of cavity morphology and size

distributions.

FasttomographymeasurementsduringcreepwereperformedatID15Abeamlineof

theESRFusingahighenergybeam (~80keV)witha largebandwidth (~50%).The

acquisition time of a complete tomographic scanwas 3min [78]. The absorption

radiographswererecordedwithafastchargecoupleddevice(CCD)withaneffective

pixel sizeof1.6m. The tensile creep testwasperformed in aminiaturized creep

machineatconstantloaddevelopedforinsitutesting[78].

The cavities developed during the creep testwere quantified in 3D by fitting an

equivalentellipsoid toeach cavity. Figure18 shows the3D reconstructionsof the

sectionedvolumerevealingcreepdamageevolutioninthesample.

Figure18.Tomographicvolumesrevealingthecavitiesatdifferenttimesduringthecreeptest.

(a)initialcondition,(b)middleofthetest,(c)closetofracture.

Page39of97

Figure 19 shows the shape evolution of the three largest cavities between the

reference state and the final state shortly before fracture. The evolutions are

representativeforthelargestvoids,whichusuallycontrolthefinalspecimenfracture.

Void evolutions indicate that creep cavities are relatively small and have nearly

ellipsoidalshape inearlierstagesofcreep.Asthematerialdeformstheygrowand

interactions among neighbors lead to coalescence. These interactionswere quite

significant for the studied brass alloy. A void can experience several coalescence

eventsduringthecreeptest.Thefirstcoalescencewassurprisinglydetectedalready

inthesecondarysteadystateregime.Notonlypairwisecoalescencesweredetected,

butalsothejunctionsoftripletsandquadruplets.

Figure19.Shapeevolutionofthethreelargestcavitiesexhibitingcoalescence.

Thedifferentstagescorrespondtothelargestporebeforecoalescence.

Thespatialorientationofacavity inthepresentwork ischaracterizedbytheangle

between themajorsemiaxisof theequivalentellipsoidand thezaxis (i.e. loading

direction). Figure 20displays a 3D graphof thepolar angleof cavitiesduring the

creep test for all cavities, revealing a smooth change of the cavity orientation

distribution.Suchachangeingeneralcavityorientationwouldindicatetheonsetof

enhanced cavity growth and linkupperpendicular to the stressdirectionwhich is

essentialfordamagingduringtertiarycreep.

Page40of97

Figure20.Evolutionofthespatialorientationofcavities.

Thequantitativeanalysesperformedrevealedthatthedistributionofcreepcavities

with respect to size, shape, andorientationdependson the time the samplehas

been exposed to high temperature creep. The largest cavities were formed by

coalescence of two or more voids resulting in a complex shape. The cavity

population tended to be elongated perpendicularly to the loading direction. The

quantitativedataobtainedcanprovideabasisforavalidationofthedescriptionof

creepdamagebynumericalmethods.

4.1.7. Insitu tomography of damage development of carbonfiber

reinforcedcomposites

Therearemanyvariantsof fiber reinforcedpolymerssuchascarbonorglass fiber

reinforced;straight,wovenor3Dbraidedfiberreinforced;withfibersandparticles

as reinforce;withhollow fibersormicrocapsules for selfhealingmaterials;hybrid

carbon and glass, and the list goes on. The amount of variables thatmight be

changed in onematerial is huge. An example is the ply stacking sequencewhich

determinesthefailuremechanismsthatwillbeactivateduponloading.Inparticular,

carbonfiberreinforcedpolymers(CFRPs)arewidelyused instructuralcomponents

owingtotheirhighspecificmechanicalproperties.However,CFRPspresentseveral

failuremechanisms that coexist in the same laminate and, therefore, improved

understandingofdamageevolutionandeventualfailureisstillneeded.

InsituSXCTwasperformedon[+45/45/+45]sCFRPsubjectedtotensileloading.The

experimentswereperformedat the ID15Abeamlineof theEuropeanSynchrotron

RadiationFacility.A14bitFReLoN(fastreadoutlownoise)CCDcamerawithafield

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ofviewof1.2x1.1mmandaneffectivepixelsizeof(1.4mm)2wasused.Thespatial

resolutionwas about 2mm (the fullwidth at halfmaximum of the point spread

function).Apinkbeamwithmaximum intensityat~30keVwasused.Sixhundred

radiographieswererecordedbetween0and180resulting inatotalscantimeof

2min per tomogram. Ten scans were recorded at increasingly applied load. A

combinationofabsorptionandphasecontrastwasobtainedbyplacingthesampleat

~40mmfromthedetector.

The evolution ofmatrix cracking is shown qualitatively in Figure 21 for different

deformation steps. Each individual crack is shown in a different color. The initial

cracks grewwith the applied load, extending over thewhole section of the plies

beforefracture.Almostallthecracksbecame interconnectedathigh loads,sothat

themajorityof thedamagedisplaysasinglecolor.Noneof thepreexistingcracks

interactedduringdeformationwith theporesobserved in Figure21d).The crack

frontsandtheshapeofindividualcracksweregenerallyuneven.

The interlaminar crack growth shows a combination of cusp formation and

matrix/fibredebondinginfrontofthecracktip.Thecracksaresubjectedtoamode

IIshear loadingandcuspsdevelopperpendiculartotheprincipalstress,coincident

withtheloadingdirection.Asdeformationprogresses,cuspscoalesceandcontribute

tothepropagationofthecrack.

Themajor damagemechanisms and the sequence of occurrenceswere identified

and quantified. The extracted information can be used to validate and enhance

damagepredictionmodels.

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Figure21.Damagepropagationin45plies.

Differentcrackcoloursindicatetheirconnectivity(adaptedfrom[17]).

4.2. Materialscience

4.2.1. ResinmicroflowbyXraycomputedtomography

Highperformancecompositeshavetobemanufacturedinautoclavetoensurethat

theyareporefreebutthisleadstohighprocessingcostsandthereisalargeinterest

in the optimization of outofautoclave processing techniques. Vacuum Assisted

ResinTransferMolding (VARTM) isaveryappealingprocessdueto itsrelative low

cost and thepossibility toprocess largepanels. In thisprocess, the liquid resin is

infiltrated intoaplasticbagcontainingthe fiberpreformthat layonarigidmould.

The infiltration is assisted by the application of vacuum.However, the resin flow

through the fiber fabric is very complex and the key parameters that control the

nucleation,growthandcoalescenceofporesduringinfusionarenotwellunderstood.

Inaddition, the resin flow in the fabric takesplaceat twodifferent length scales:

macroscopic resin flowbetween the fiber towsprogresses rapidlywhilemicroflow

withinthefibertowsoccursatlowerspeed.Theinteractionbetweenmacroflowand

microflowisknowntobeacriticalfactorcontrollingthedevelopmentofporositybut

itisverydifficulttoanalyzeexperimentally.

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To provide the experimental evidence necessary to understand resin flow during

VARTM,aminiaturizeddevicethatreproducestheconditionsofVARTMprocesswas

developedand,at thesame time,allows tostudy the infiltrationatbothscalesby

meansofSXCT.Tothisend,highresolutionSXCTwasperformedatthefiberscaleto

analyzeinsituthemacroandmicroflowbehaviorandthedefectformationduring

the infusionprocess.TheexperimentswereperformedattheP05beamlineofthe

DESYSynchrotron.A14bitCCDcamerawitha fieldofviewof3.8x1.9mmandan

effectivepixelsizeof(1.25mm)2wasused.Thespatialresolutionwasabout2mm.A

monochromatic beam with 25 keV was used. Nine hundred radiographies were

recordedbetween0and180resultinginatotalscantimeof~2hspertomogram.

Due to the largemeasurement time the liquid flowhas tobe stoppedduring the

measurement. This could be avoided with a fast tomography setup and would

providerealtimeinformationaboutinfiltrationmechanisms.

Figure22showstheexperimentalsetupattheP05beamlineatDESYSynchrotron.

Theliquidisinfiltratedfromthetop(inlet)andthevacuumisappliedatthebottom

(outlet).Thefibertowspecimen,placedinavacuumbaginsidethePMMAtubewas

scannedbyXraysduringinfiltration.

Figure22.Experimentalsetuptostudyinsitutheinfiltration

processattheP05beamlineofDESYSynchrotron.

Figure 23 shows a reconstructed volume and a crosssection obtained by SXCT

showing the flow front (macroflow) around the tow and themicroflow inside the

tow.Thisuniqueexperimentalsetupprovidesthe informationtoanalyzetheresin

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flow in3dimensionsduring infiltrationatboththemicroscaleandthemacroscale,

aswellastoassessthedifferencesinpermeabilitybetweenbothregimes,beingthe

former several orders of magnitude lower than the latter. Moreover, the

experiments shows the conditions that give rise to regions that might remain

partially infiltratedduetotrappedairbubblesortodifferencesbetweencapillarity

andresinpressure,leadingtolowqualitypanels.Basedonthesedata,itispossible

to design optimized VARTM strategies to improve the quality and reduce the

processingcostofadvancedstructuralcomposites.

Figure23.(a)Crosssectionofthescannedfibertowspecimeninthevacuumbag.Wetglassfibersare

surroundedbythelightergreycolor.(a)3Dreconstructionoftheinfiltratedtow.

4.2.2. 3DmultiphasenetworksprovidinghightemperaturestrengthtoAlSi

pistonalloys

CastAlSialloysarewidelyused inautomotivecomponentssuchascylinderheads

andpistons.Thetemperatureriseinthecombustionchamberofadieselenginecan

reachup to~300400Cand, therefore,high temperaturestrength isan important

requirement forpistonalloys.Thehigh temperature strengthofcastAlSialloys is

providedbyatransferofloadfromtheductileAlmatrixtorigidandusuallyhighly

interconnected3DnetworksofeutecticSi.However, ifcastAlSialloysaresolution

treatedabove500C,theeutecticSirapidlydisintegratesandspheroidizesreducing

thestrengthofthealloy[79].Thelossinstrengthcanbereducedbytheadditionof

transitionelements such asNi andCu that form thermally stable rigid aluminides

[80,81].ThereasonsfortheimprovementofmechanicalpropertiesofAlSialloysby

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additions of Ni and Cu are stillmatter of scientific investigationswith important

technological implications.TheeffectofdifferentadditionsofNi,CuandFeonthe

hightemperaturestrengthofcastAlSipistonalloys is investigatedwithrespectto

the microstructural architecture formed by the aluminides and the eutectic Si.

Therefore, absorption and phase contrast synchrotron microtomography was

appliedtosamplesofthealloysAlSi12,ASi12Ni,AlSi12Cu5Ni1andAlSi12Cu5Ni2 in

ascastconditionandaftersolutiontreatmentusingtheID19beamline.

Figure24showsthelargestparticlesoftheeutecticSiandofthealuminideswithin

theconsideredvolumesforthestudiedalloysafter4hsolutiontreatmentat490C.

Thetomographicresultsshowthatthe interconnectivityoftheeutecticSi ishighly

conserved after the solution treatment for the aluminidecontaining alloys (Figure

24b,eandf).

Figure25showstheevolutionoftheproofstress,0.2,at300Casafunctionofthe

solutiontreatmenttimeat490C.Thesolutiontreatmentcausesadecrease inthe

hightemperaturestrengthoftheinvestigatedalloyswithinthefirst4h.

ThealuminidecontainingalloysexhibithigherstrengthsthantheAlSi12alloydueto

the larger volume fraction of rigid phases, amounting to 1824%, the high

interconnectivityofthealuminidesandtheirhighcontiguitywiththeeutecticSi.The

alloys AlSi12Ni1 and AlSi10Cu5Ni1 contain ~8vol.% of aluminides. However, the

aluminides in theAlSi10Cu5Ni1 alloy present a higher degree of interconnectivity

(~94% in ascast condition and ~75% after stabilization) than the AlSi12Ni1 alloy

(~60% in ascast condition and ~50% after stabilization). Xray diffraction analysis

revealed that the addition of Cu produces various aluminides increasing the

contiguity: Al7Cu4Ni, Al2Cu, Al4Cu2Mg8Si7 and AlSiFeNiCu. ~90% of all the

aluminides and all the eutectic Si are forming a highly interconnected rigid 3D

structure inAlSi10Cu5Ni1which increasesthehightemperaturestrengthby~100%

withrespecttotheCufreealloyAlSi12Ni(Figure25).

ThepistonalloysAlSi10Cu5Ni1andAlSi10Cu5Ni2showsimilarstrengthintheascast

condition.AlSi10Cu5Ni2containsmorealuminides(~13vol.%)and itretainsa~15%

higherstrength levelthanAlSi10Cu5Ni1afterthesolutiontreatment.Furthermore,

the3Dnetworkoftherigidphasesispracticallyfullpreserved(~97%)duringsolution

treatment of the AlSi10Cu5Ni2 (Figure 24d, f), owing to the larger degree of

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contiguitybetweenthealuminidesandeutecticSi.Thisresultsinanextraincreaseof

loadtransferfromtheAlmatrixtothereinforcing3DnetworkofaluminidesandSi

whichismoreimportantathightemperatureswherethematrixbecomesrelatively

softer.

The results indicate that the design of cast AlSi alloys for high temperature

applications requires a deep understanding of their 3D architecture and the

mechanisms governing its evolution with temperature and time. Synchrotron

microtomography is a powerful tool to achieve these tasksmainly due its non

destructivenature,suitablesamplesizetoresolutionratioandthepossibilitytouse

phasecontrasttorevealtheeutecticSiembeddedintheAlmatrix.

Figure24.3DstructuresofaluminidesandSiafter4hofsolutiontreatment:a)SiinAlSi12,b)Siand

aluminidesinAlSi12Ni,c)aluminidesinAlSi10Cu5Ni1,d)aluminidesinAlSi12Cu5Ni2,e)Siin

AlSi10Cu5Ni1andf)SiinAlSi10Cu5Ni2.

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Figure25.Proofstress0.2at300Cfortheinvestigatedalloys

asafunctionofthesolutiontreatmenttime.

4.2.3. Submicrometerholotomographyofmultiphasemetals

Themicrostructural characterization ofmultiphasematerials by conventional 2D

metallographycanbeinsufficientif,forinstance,connectivitybetweenphasesexists,

or the orientation of constituents varies throughout the volume. For this, 3D

characterisationtoolsareneeded.Synchrotronmicrotomographyhasshowntobea

powerful technique to reveal the architecture of materials. Furthermore, the

coherence of the beam can be exploited applying quantitative phase contrast

tomographyorholotomography[82]toimagecomponentswithsimilarattenuation.

Thespatialresolutionachievablebyparallelbeamsynchrotronmicrotomography is

about1m.Thiscanbeimprovedusingmagnifyingoptics[83].Thishassofarbeen

achieved for samples with diameters

Page48of97

sizesof60nmand51nmwereusedfortheAlalloyandTialloys,respectively.Phase

retrieval forholotomographywasachieved from recordings at four focalpointto

sampledistances.

Examplesofthreelightalloysarepresented.Theirmicrostructuresareshowninthe

scanningelectronmicrographs(SEM)atthetopofFigure26:

AlMg7Si4alloy:themicrostructureexhibitsafineternaryeutecticformedbyAl,Si

andMg2Siwithlamellarstructures>150nm.Ferichintermetallics(IM)appearwithin

theprimaryAl.

Ti10V2Fe3Alalloy (Ti1023): thealloycontains~30%ofhcpphasedistributed

withinbccgrainsnotobservablebyabsorptioncontrast.

Ti6Al4V (Ti64) alloy reinforcedwith 5vol% TiB needles (Ti64/TiB/5w): the Ti64

alloymatrixconsistsofgrainsseparatedbynarrowzonesandTiBneedles.

Holotomography is well adapted to these materials as there is low absorption

contrastbetweenthepresentphases.

Portions of the reconstructed holotomography slices are shown at the bottom of

Figure26.Thegreylevelscaleslinearlywiththeelectrondensityoftheconstituents

revealing all the phases observed in the SEMmicrographs. Volume views of the

minorityphasesareshowninFigure27.

AlMg7Si4:theternaryeutecticwith interconnectedSiMg2Sistructuresasthinas

~180nm (green)are identified.The IMparticlesandAlaremade transparent in

Figure27a).

Ti1023:grains>200nmareidentified.InFigure27b),aninterconnectedstructure

ofparticlesremainedfromanincompletebreakupofthelamellarstructureduring

preforging(blue),whilesecondarygrains(green)areembeddedinthephase.

Ti64/TiB/5w:theandphasesintheTi64matrixareidentifieddownto200nm.

In Figure 27c), TiB needles (green) are connected to irregularly shaped grains

(othercolours),forminganinterpenetratingstructurewithinthephase.

MagnifiedsynchrotronholotomographyusingKBopticswasusedtocharacterizethe

3Darchitecture of Al and Tialloy samples of ~0.4mm diameterwith energies of

17.5 and 29keV, respectively.Using the nanofocusing KBsystem for such a high

energy (29keV) is reported for the first time. This experimental setup combining

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synchrotron radiation, KB optics and holotomography opens a new level of

resolution (180nm) for nondestructive 3D imaging of representative samples of

multiphasemetals.

Althoughmagnified synchrotron holotomography is not planned in the proposed

beamline,theholotomographymethodologycanbeusedtocharacterizemultiphase

materialsaslongasthesizeofthephaseareabovetheresolutionofthetechnique.

However,themagnifyingopticssetupcouldbe included inafurtherupdateofthe

beamline.

Figure26.Top:scanningelectronmicrographsoftheinvestigatedmaterialsBottom:portionsofslices

ofholotomographyreconstructionsoftheinvestigatedmaterials.Fromlefttoright:AlMg7Si4alloy,

Ti1023alloyandTi64/TiB/5w.

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Figure27.Renderedvolumesoftheinvestigatedmaterials:a)interconnectedSiMg2Sistructure

(green)inAlMg7Si4;b)largerparticlesremainingfrompreforging(blue)andindividualsecondary

grains(semitransparentgreen)inTi1023;c)TiBneedles(green)andirregularlyshapedgrainsin

Ti64/TiB/5w(othercolours).

4.3. Lifesciencesandbiomedicine

In contemporary biomedical, aswell as clinical research, structural imaging has a

central role. Current approaches are focused in a multiscale methodology.

SynchrotronXraybased imagingprovide thepossibility to integrateseveralof the

required length scale, providing highresolution (submicrometre) detail in large

samples (tens of centimetres) [85]. SXCT with phasecontrast offers exciting

possibilitiestosupportSystemsMedicineresearch.Substructuresoforgans,oreven

whole (small) organisms, can be investigated, segmented and quantified from a

single3Ddataset.Thisalsoenablestoobtainthestructuraldatathatisrequiredfor

e.g.performingcomputationalmodellingoffunctionalorgan[86],suchasitisdone

inthecontextoftheVirtualPhysiologicalHuman[87].

PotentialapplicationsforahardXraytomographybeamlineatALBA:

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4.3.1. HighresolutionStructuralImagingofstatictissue:

Multiresolution imaging at the (sub)micrometre scale is essential in evaluating

structuralpropertiesandinducedchangesinalotofbiomedicaldomains.Theability

toimagelargevolumesoftissueatthisscaleoffersnovelinsightstowardsassessing

pathological remodeling aswell as towards providing data for e.g. computational

modeling.ExamplesofthisareprovidedinFigure28,Figure29,Figure30.

Elastine bres in the aortic wall

Fibre orientationchange

Falsetendon

Intramuralvessel

Coronory arteryostium

Aorticvalve

Tricuspidvalve

LV wall

Long.

Circ.

Long.

Figure28.Phasecontrastimagingofwhole(rodent)hearts.Besidetheanatomicaldetailatorgan

level,thedetailedfibrestructureinwhichmyocytesareorganisedcaneasilybeassessed.Additionally,

vesselscanbeobservedandextractedusingcomputationaltools[89].

Figure29.Imageofapretermrabbitpupthorax,focusingontheair/lungtissueinterface[90].

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Figure 30. Spatial resolution of histology, Xray phase tomography, and MRI microscopy

demonstratingthatresolutiondecreasesfromhistologyviaPCmCTtomMRI[91].

4.3.2. HighthroughputVirtualPathology

Whole organism assessment, as e.g. in

human autopsies or phenotyping of

geneticallymodifiedmodelorganisms,isstill

an essential source of information, both in

basic research as well as in clinical

understanding of diseases. Traditional

autopsieswoulddescribeand,insomecases

image, the whole organism and additional

detailed information would be provided

from destructive (microscopy) investigation

of specific organs or tissue samples.

However, this leads to different (sparse)

information at the different spatial

resolutions and an integration of organ and cellaggregate level is extremely

challenging,verytimeconsumingandexpensive.Thismeansthatwholeorganisms

areonly investigated in rarecases, suchas for specific researchprojectsore.g. in

human fetuseswhen thecauseofperinataldeath isunknown.Othermethods like

MRIareverytimeconsumingandwith limitedresolution,Figure31.SXCT inphase

Figure 31. A false positive MRI post

mortem, suggesting lung changes while

histologywasnormal.

Page53of97

contrastmode,togetherwithahighthroughputforsamplehandling,couldprovidea

way for fast (

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4.4. Historicalbuilding

4.4.1. Insitutomographyofthefluidmovementinsiderocks:applicationto

historicalbuildingconservation

Waterplaysa fundamental role in rockweatheringprocesses. Itspenetrationand

movementinsiderocksgreatlyinfluencesthenatureandintensityofthedamage.X

rayComputedTomography (XrayCT)beingaNonDestructiveTechnique (NDT), is

very useful in mapping water penetration. A General Electric HiVelocity QX/i

helicoidal scannerwas used for the studies in the following parameters: voltage

140kV;current150mA;exposuretime2s;resolution0.203mmx0.203mm,andslice

width0.625mm. Seriesof80virtualsectionswere imaged inparallelatspecified

time intervals. The obtained imageswere 512 x 512pixels in size. Image length:

50mm.

Xray CT provides good images of the internal structure of the samples: the

sedimentary layeringduetodifferences incompositionandporosity isclearlyseen

aswellasothermineralogical/texturalcharacteristics(Figure33).

Figure33.a)Uniformdistributionofthemineralsexcept in ironoxides layers(atthebottom).b)(1)

voidspaces;(2)finegrainedcarbonates;(3)largegrainedcarbonatesand(4)claysandironminerals.

ThemovementandpenetrationrateofwaterhasbeenmonitoredbyXrayCTduring

freewaterabsorptiontests(UNEEN13755(2002).Figure34a)showsthedifference

betweendryandwetzones intheinteriorofthesamplewhileFigure34b)showsa

3Drenderingofthevolumeillustratinghowthedryopenspacedecreasesduringthe

absorptiontest.

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Thecomparisonof80CTscansperiodicallytakenduringthewaterabsorptiontest

allowstheobservationofthewaterfrontmovementin3D.Thewatermovementis

related to thepetrographic characteristicsof the rock,mainly to the sedimentary

layeringthatcontrolsthedirectionofwaterpenetration.Waterabsorptiondepends

on the rock textureandporosity. Largeporesaregenerallynot connected.Water

penetratesthroughthelayerswithsmallerbutinterconnectedpores.

HounsfieldUnitnumbersprovide aquantitative approach for the identificationof

differentcompositionsandporosities,and thepenetrationrateofwater.MeanCT

values in Hounsfield units (HU), in ROIs (Region Of Interest) are measured at

different intervals of time during the water absorpt