Applications of Synchrotron Light to Scattering and Diffraction in Materials and Life Sciences

330 Pages·2009·10.426 MB·English

by  M.C. García-Gutiérrez, D.R. Rueda (auth.), Marian Gomez, Aurora Nogales, Mari Cruz Garcia-Gutierrez, T.A. Ezquerra (eds.)

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T.A. Ezquerra
M.C. Garc´ıa-Gutie´rrez
A. Nogales
M.A. Go´mez (Eds.)
Applications of Synchrotron
Light to Scattering
and Diffraction in Materials
and Life Sciences
123
T.A.Ezquerra MariCruzGarc´ıa-Gutie´rrez
CSICMadrid CSICMadrid
Inst.EstructuradelaMateria Inst.EstructuradelaMateria
Serrano,119 Serrano,121
28006Madrid 28006Madrid
Spain Spain
[email protected]
AuroraNogales MarianGo´mez
CSICMadrid CSIC
Inst.EstructuradelaMateria Inst.CienciayTecnologia
Serrano,121 dePolimeros
28006Madrid JuandelaCierva,3
Spain 28006Madrid
Spain
Ezquerra, T.A., et al. (Eds.), Applications of Synchrotron Light to Scattering and
Diffraction in Materials and Life Sciences, Lect. Notes Phys. 776 (Springer, Berlin
Heidelberg2009),DOI10.1007/978-3-540-95968-7
ISBN 978-3-540-95967-0 e-ISBN 978-3-540-95968-7
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Preface
Inafirstapproximation,certainlyrough,onecandefineasnon-crystallinematerials
those which are neither single-crystals nor poly-crystals. Within this category, we
canincludedisorderedsolids,softcondensedmatter,andlivesystemsamongothers.
Contrary to crystals, non-crystalline materials have in common that their intrinsic
structurescannotbeexclusivelydescribedbyadiscreteandperiodicalfunctionbut
byacontinuousfunctionwithshortrangeoforder.Structurallythesesystemshave
incommontherelevanceoflengthscalesbetweenthosedefinedbytheatomicand
themacroscopicscale.Inasimplefluid,forexample,mobilemoleculesmayfreely
exchange their positions, so that their new positions are permutations of their old
ones. By contrast, in a complex fluid large groups of molecules may be intercon-
nected so that the permutation freedom within the group is lost, while the per-
mutation between the groups is possible. In this case, the dominant characteristic
length, which may define the properties of the system, is not the molecular size
but that of the groups. A central aspect of some non-crystalline materials is that
they may self-organize. This is of particular importance for Soft-matter materials.
Self-organizationischaracterizedbythespontaneouscreationofregularstructures
at different length scales which may exhibit a certain hierarchy that controls the
propertiesofthesystem.
X-ray scattering and diffraction have been for more than a hundred years an
essentialtechniquetocharacterizethestructureofmaterials.Quiteoftenscattering
anddiffractionphenomenaexhibitedbynon-crystallinematerialshavebeenreferred
toasnon-crystallinediffraction.Non-crystallinematerialsmayexhibitweakX-ray
scatteringpowermainlydueeithertoalowleveloforderortolittleelectronicden-
sitycontrast.Again,thelasteffectisespeciallyimportantforsoft-mattermaterials
whichfrequentlyarecomposedoflightatomsandagreatamountofwater.Forin-
stance,itisknownthattypicaldiluteproteinsolutionscatters1photonevery105in-
cidentphotons.ThisexampleimmediatelyillustratethenecessityofpowerfulX-ray
sourcesofferinghighphotonfluxes.Theinitialuseoffirst-generationsynchrotron
lightinthe1960softhe20thcenturyfordiffractionexperimentsopeneduptremen-
dousexpectationsforthescientificcommunityinvolvedinnon-crystallinematerials.
Many of these expectations have been fulfilled along the time as demonstrated by
v
vi Preface
theincreasingamountofthird-generationsynchrotronfacilitiesavailableintheac-
tuality and by those which are under construction all around the world. This fact
makesthatsynchrotronlightisbecomingmostandmostpopularevenamongnon-
synchrotronradiationspecialists.Obviouslythisisadesirable“side-effect”consid-
eringthetremendousamountofinvestmentdoneatbothnationalandtrans-national
level in these facilities. Accordingly, it is expected an increasing amount of syn-
chrotron users aiming to use scattering and diffraction techniques to elucidate a
broadvarietyofsystemsandproblems.
ThepresentvolumeofLectureNotesinPhysics,entitledApplicationsofSyn-
chrotron Light to Scattering and Diffraction in Materials and Life Sciences,
originates from the necessity to bridge the gap between beam-line manuals and
highlyspecializedtextbooks.Thecollectionofcontributionspresentedinthisbook
attemptstocovermostoftheaspectsinwhichthecombinationofsynchrotronlight
with scattering and diffraction techniques can be very helpful in order to provide
essentialinformationonthestructureoflargemolecularassembliesinlow-ordered
environments. Contributors have been selected based on their engagement as ad-
vancedsynchrotronusersaimingtopresentcontributionsascloseaspossibletothe
beam-linework.Specialemphasiswasdoneonincludingcontributorswhoarein-
volved on the management and day-by-day activity of representative beam-lines
devoted to Non-crystalline Diffraction as they are ID2, ID13, and BM26 at the
European Synchrotron Radiation Facility(ESRF) (France), X27C at the National
SynchrotronLightSource(NSLS)(USA)andNCD(port-11)atALBA(Spain).The
bookhasbeendividedintotwomainsectionscomprisingfundamentsandapplica-
tions. The first section contains a first chapter dedicated to introduce the reader to
the bases of synchrotron radiation, light sources and beam-lines and a second one
presenting the fundaments of scattering by soft-matter.Considering the increasing
applicationofscatteringanddiffractiontonanomaterials,thirdandfourthchapters
focus on the use of grazing incidence and microfocus in X-ray scattering, respec-
tively. The application section has been divided into two parts dealing with ma-
terials science (Part II) and life sciences (Part III). In part II an attempt has been
madetoincludeexamplesofapplicationsonnon-crystallinediffractioninbroadse-
lection of representative non-crystalline materials including hard and soft colloids
(Chaps.5and6),liquid-crystallinepolymers(Chap.7),nanocomposites(Chap.8)
and carbon fibres (Chap. 9). Additionally chapters 5 and 10 emphasize potential
advantage ofcombiningnon-crystallinediffractionwithothertechniques likeEX-
AFS,dielectricspectroscopyorcalorimetry.InpartIII,twomainchaptersdealwith
the application of X-ray scattering to elucidate protein shapes in solution by us-
ing either conventional X-rays (Chap. 11) or synchrotron light (Chap. 12). These
twochaptersemphasizehowconventionalX-raysandsynchrotronradiationarefar
frombeingantagonists.Finally,Chaps.13and14presentthepotentialuseofX-ray
scattering to medical diagnosis and to elucidate the biophysics of natural muscle
dynamics.
We hope that this issue of Lecture Notes in Physics may contribute to a more
general understanding about the combination of synchrotron light with scattering
Preface vii
and diffraction techniques in non-crystalline materials. Moreover, we expect that,
by presenting a snap-shot of the state of the art in this field, the community of
synchrotronusersinterestedinthesetopicsmayeventuallybeenlarged.
Madrid, TiberioA.Ezquerra
February2008 MariCruzGarc´ıa-Gutie´rrez
AuroraNogales
Mar´ıanGo´mez
Acknowledgments
The initial idea for this book originated from a series of Workshops on “Appli-
cations of Synchrotron Light to Non-crystalline Diffraction in Materials and Life
Sciences” held in Madrid at the Instituto de Estructura de la Materia, CSIC , in
2005and2007.WeareindebtedtotheCOSTACTIONP12“StructuringofPoly-
mers”,CSIC,Telefo´nica,BrukerBioscience,Asociacio´ndeUsuariosdeSincrotro´n
de Espanˆa (AUSE), Comunidad de Madrid and Red Tema´tica de Radiacio´n Sin-
crotro´ndelCSIC,forsupporttothecelebrationoftheseWorkshops.WethankProf.
Gu¨nterReiterforfruitfulcomments.
ix
Contents
1 BasesofSynchrotronRadiation,LightSources,andFeaturesof
X-RayScatteringBeamlines .................................. 1
M.C.Garc´ıa-Gutie´rrezandD.R.Rueda
1.1 Introduction.............................................. 1
1.2 SynchrotronRadiationSource............................... 5
1.3 MainComponentsofaSynchrotronRadiationSource........... 8
1.4 CharacteristicsoftheSynchrotronLight ...................... 10
1.5 UseofInsertionDevicestoImprovetheSynchrotronRadiation... 13
1.6 ExperimentalBeamline .................................... 16
1.7 SynchrotronRadiationFacilities............................. 18
References..................................................... 20
2 Scattering of Soft Condensed Matter: From Fundaments to
Application................................................. 23
N.Stribeck
2.1 Introduction.............................................. 23
2.2 ExperimentGeometryandReciprocalSpace .................. 24
2.3 MaterialsStructureandScatteringPattern..................... 29
2.4 OptionsforanAnalysisoftheScatteringIntensity.............. 31
2.5 FromtheMathematicalLaboratoryofScattering ............... 34
2.6 ApplicationtoMaterialswithFiberSymmetry................. 41
References..................................................... 58
3 ABasicIntroductiontoGrazingIncidenceSmall-AngleX-Ray
Scattering.................................................. 61
P.Mu¨ller-Buschbaum
3.1 Introduction.............................................. 61
3.2 GeneralPrinciples......................................... 63
3.3 Simplifications ........................................... 82
3.4 SummaryandOutlook ..................................... 83
3.5 Appendix–CriticalAnglesofPolymers ...................... 85
References..................................................... 86
xi
xii Contents
4 FundamentsofSoftCondensedMatterScatteringandDiffraction
withMicrofocusTechniques................................... 91
C.Riekel,M.Burghammer,R.Davies,R.Gebhardt,andD.Popov
4.1 Introduction.............................................. 91
4.2 Examplesforμ -SAXS/WAXSExperiments ................... 92
4.3 Techniques,Instrumentation,andDataAnalysis................ 94
4.4 RadiationDamageIssues...................................100
4.5 HowtoAccess3DInformation?.............................101
References.....................................................102
5 TheUseofScatteringandSpectroscopicSynchrotronRadiation
MethodsinMaterialsScience ................................. 105
W.Bras
5.1 Introduction..............................................105
5.2 NewTechniques ..........................................109
5.3 SomeExamples...........................................111
5.4 Conclusions..............................................130
References.....................................................131
6 SynchrotronSmall-AngleX-RayScatteringStudiesofColloidal
Suspensions ................................................ 133
T.Narayanan
6.1 Introduction..............................................133
6.2 GeneralPrinciples.........................................134
6.3 ApplicationsofSAXSMethods .............................144
6.4 SummaryandOutlook .....................................154
References.....................................................155
7 ApplicationsofSynchrotronX-RayDiffractiontotheStudyofthe
PhaseBehaviorinLiquidCrystallinePolymers .................. 157
E.Pe´rez,J.P.Ferna´ndez-Bla´zquez,A.Mart´ınez-Go´mez,A.Bello,M.L.
Cerrada,R.Benavente,andJ.M.Perenˆa
7.1 Introduction..............................................158
7.2 MesophaseStructuresandDiffractionProfiles .................159
7.3 TechniquesfortheAnalysisofthePhaseBehavior .............161
7.4 SynchrotronX-RayDiffractionStudiesofthePhaseBehaviorin
LiquidCrystallinePolymers ................................162
References.....................................................181
8 StructuralAnalysisofBiologicalandTechnicalNanocompositesby
X-RayScattering............................................ 183
P.Nawani,H.Zhou,B.Chu,C.Burger,andB.S.Hsiao
8.1 Introduction..............................................184
8.2 TheoreticalBackground....................................187
8.3 SAXSAnalysisofCollagen/MineralNanocomposites ..........190
8.4 AnalysisofPolymer–OrganoclayNanocomposites .............193