Exploring Glass Surface With HighExploring Glass Surface .
Exploring glass surface with high-resolution XPSand LEIS:EExamplesl off FundamentalF dt l StudiesSt di andd ApplicationsA li tiAndriy KovalskiyMaterials Science & Engineering DepartmentLehigh University, PACo-authors: Himanshu Jain, Bruce Koel, Alfred Miller, Miroslav Vlcek,Roman Golovchak, Keisha Antoine, Maria Mitkova“The surface was invented by the devil”Wolfgang Pauli
Glass structure – lack of translational symmetryAVdoleorcpe iduSuliqBuidqiLEFGlassGCrystalCDTroom Tgmin TgrangeTgmaxTcrystHigh-resolution XPS:one of the fundamental structural methods in glass scienceOther methods:Raman/FTIR spectroscopy, EXAFS, NMRT
State of the art high resolution XPS vs “normal” XPSSe-Se-Se30000Se25000As40Se6020000Se 3d2000012000As40Se60As Se g energy , eV525105857565554Binding energy , eV5352045444342Binding energy , eV4140
Structure of fresh cut of glass vs freshly deposited thin filmAs3d core levelAs2S3 bulk12000S 2p2 core llevell18000Counts15000CountsAs2S3 0001650461641631621611604544434241Binding energy, eVBinding energy, eVBulk As2S31000016 % within S-S84 % AsS3/2S2p60006000As 3d5000CouuntsCoounts80007000400085 % AsS3/2300015 % As-As2000400010002000165164163162161Binding energy (eV)045444342Binding energy (eV)Freshly deposited As2S3 film41
Thin films: photostructural transformations by XPSArray of Fresnel lenses withfocal point 300 μmFresnel lens with focalpoint 5.38 mmIR laser beam (1.55 μm) focusedby Fresnel lens on Si substrate
Photooxidation on the surface of ChGOxidation in air strongly depends on Ge contentIntenssity (counts//sec)600500Ge Se thin film2 3Ge 3d core level400300distributedGe-O bondsGe withinethane-like units200Ge oxide10003634332330Binding energy (eV)Strong oxidation in air288Intensity (counts/sec)500400Ge3Se7 thin film exposed to airGe 3d core levelGe within GeSe4300200100033323130Binding energy (eV)No oxidation in air29
E-beam Patterning of Chalcogenide GlassesWhat is the resolution limit for ChG?17 nm 20 nm7 nmFinest structural features onlglassesDirect observation of separate ebeam spotsWet Etching in Amine Solution
Structural Origin of E-beam Patterning of Chalcogenide ass substrate CrAs4s(nb)CPS10As4s((nb)) As4p(b) S3p(lp)( p)glass substrate diation (dose I)2030030252015105250151050Binding energy (eV)Binding energy (eV)As35S651020As35S65glass substrate Crglass substrate lectron-irradiation (dose II)250freshelectron-irradiation (dose III)003025201510Binding energy (eV)50252015105Binding energy (eV)0
Gray Scale Lithography based on Ag Photodiffusionin Chalcogenide Glass Thin FilmsMotivation: 3-D profiles in photoresist film for development ofmicroturbine compressor with smooth bladesExample of complex shape structure on the surface– negative dry etchingSi substrate to ChG thickness transfer ratio of 10 is achieved
Gray Scale Lithography based on Ag Photodissolutioninto Chalcogenide Glass Thin Films3000025000- Ag dissolves into As-S glass in step like mode20000Counts- depth of dissolution - function of exposure doseS2p93 % AsS3/2150007 % Ag-S100005000165164163162161160Binding energy (eV)Control of compositionKinetics of X-ray-induced silver dissolution fromthe surface of a-As2S3 thin film by high-resolution XPS45Ag (7 nm)/As2S3 (50 nm) bi-layer,40Ag, aat. %Profilogram demonstrating the change of etching depthwith gradual variation of transparency of mask fragments.films deposited and irradiated at UHV,no contact with air353025201501020304050607080t, minKinetics of X-ray-induced Ag dissolution
Ag Photodiffusion into As2S3Influence of surface oxidation?ChG Surface after Photodiffusionand Treatment in HNO3 solutionSpikes are due to: oxide clusters which etch differentlydifferently.
Ag Photodiffusion into ChGCompare final productsAg/As/ 2S3 X-ray irradiated exposed to airAg/As2S3 X-ray irradiated in vacuumAg/As2S3 X-ray irradiated in vacuumAg/As2S3 X-ray irradiated exposed to air10000Inntensity (counts/sec)Inntensity (counts/sec)4000As 3d core level3000200010008000600040002000046444240S 2p core level380165164Binding energy (eV)163162161160159158Binding energy (eV)x 10340FINAL PRODUCTS off AAg diffdiffusioniini vacuum andd air:i3530 S chemical environment is similar, except that formationof ternary is slowed down by arsenic oxidation25A 3d5/2Agvacuumair201510 As chemical environment differs drastically:- phase separation due to oxidation in air;- some clustering of As in vacuum Ag chemical environment slightly differs due to As50370369368367Binding Energy (eV)C asaXPS (T hi s string can be edited i n CasaXPS.DEF/Print FootNote.txt )366365
Strong Glasses for SolarEnergyConcentrated Solar Thermal(CST)Photovoltaics: Increasedstrength to weight (thickness) topermit larger thin film modulesizeMethods: XPS, LEIS
Sodium silicate glasses – breaking pathSampleNaOSiNa/SiBO/NBOSodiumdisilicate, 902155240 8750.875222.2Sodiumdisilicate, 251959220.862.3Sodiumdisilicate heattreated, 902055250.802.3Sodiumdidisilicate heattreated, 252154250.842.2Sodiumtrisilicate, 901460260.543.0Sodiumtrisilicate, 252456201.202.4
Ion-TOF low energy ion scattering: first resultsNa2OO-2SiO2SiO2 fractured100140OSiO2 fracturedNa120O80LEIS sygnal (a.u.)LLEEIS sygnal (a.u.)100Si60408060Si40202000800100012001400Energy (eV)1600180020008001000000120000140000Energy (eV)160060018008002000000
Low Energy Ion Scattering: Preliminary resultsSampleSiO2fracturedNa2O 2SiO2fracturedNa2O 2SiO2treated 1 hatt 620 C, CfracturedNa2O 3SiO2fracturedSi, at. % O, at. %Na, at. %Na/Si3565--817759.45247114.23197826 026.0
Conclusions
Binding Energy ReferencingSurface charge energy Ech can be determined by electrically calibrating theinstrument to a spectral feature.C1s at 284.8 eVAu4f7/2 at 84.0 eVx 10190Se 3d80without Auwith Au7060Ge 3dCPS5040302010055504540Binding Energy (eV)CasaXPS (T his string can be edited in CasaXP S.DEF/PrintFootNote.txt)3530Ge3Se7 – ideal referencing of Ge 3d to Au 4f7/2
3 X-ray irradiated in vacuum s/sec) 8000 10000 S 2p core level Ag/As 2 S 3 X-ray irradiated in vacuum Ag/As 2 S 3 X-ray irradiated exposed to air s/sec) 1000 2000 n tensity (count 2000 4000 6000 n tensity (count x 10 3 40 46 44 42 40 38 0 I Binding energy (eV) 165 164 163 162 161 160 159 158 0 I Binding energ
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