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Simbi isingatsvinyike inoshandiswa zvakanyanya pamwe chete nesimbi dzayo dzakagadzirwa dzinoramba ngura mumamiriro ekunze nekuda kwepasivation layer ine chromium oxide. Kuora nekuora kwesimbi zvinowanzobatanidzwa nekuparadzwa kwezvikamu izvi, asi kashoma pachiyero chidiki, zvichienderana nekwakabva kusawirirana kwepamusoro. Mubasa iri, nanoscale surface chemical heterogeneity inowanikwa ne spectroscopic microscopy uye chemometric analysis isingatarisirwi inotonga kuora nekuora kwecold rolled cerium modified super duplex stainless steel 2507 (SDSS) panguva yekupisa kwayo. Kunyangwe X-ray photoelectron microscopy yakaratidza kufukidza kwakafanana kweCr2O3 layer yechisikigo, cold rolled SDSS yakaratidza mhedzisiro isina kunaka yekusagadzikana nekuda kwekupararira kweFe3+ rich nanoislands paFe/Cr oxide layer. Ruzivo urwu paatomu runopa kunzwisisa kwakadzama kwekuora kwesimbi isingatsvinyike uye kunotarisirwa kubatsira kurwisa ngura yesimbi dzakafanana dzine alloy.
Kubva pakagadzirwa simbi isina ngura, kuramba ngura kweferrochromium alloys kwave kuchinzi kunokonzerwa nechromium, iyo inoumba oxide/oxyhydroxide yakasimba inoratidza maitiro ekuzorora munzvimbo zhinji. Zvichienzaniswa nesimbi dzisina ngura dzemazuva ano (austenitic neferritic), simbi dzisina ngura dzakasimba (SDSS) dzine kuramba ngura zviri nani dzine hunhu hwepamusoro hwemakanika1,2,3. Simba remakanika rakawedzerwa rinobvumira magadzirirwo akareruka uye akapfava. Kusiyana neizvi, SDSS inodhura ine kuramba ngura kwakanyanya, zvichikonzera hupenyu hwakareba hwebasa uye mashandisirwo akakura mukutonga kusvibiswa, midziyo yemakemikari, uye indasitiri yemafuta negesi iri kunze kwenyika4. Zvisinei, huwandu hushoma hwekupisa kwekurapa kupisa uye kusagadzirwa zvakanaka zvinokanganisa kushandiswa kwayo kwakakura. Nokudaro, SDSS yakagadziriswa kuti ivandudze hunhu hwataurwa pamusoro apa. Semuenzaniso, kugadziriswa kweCe uye kuwedzerwa kwakanyanya kweN 6, 7, 8 kwakaunzwa muna 2507 SDSS (Ce-2507). Kuwanda kwakakodzera kwe0.08 wt.% rare earth element (Ce) kune mhedzisiro yakanaka pahunhu hweDSS, sezvo ichivandudza kunatswa kwegorosi uye simba remuganhu wegorosi. Kusapera nekuora, simba rekudhonza uye simba regoho, uye kushanda kwekupisa zvakavandudzwawo9. Nitrogen yakawanda inogona kutsiva nickel inodhura, zvichiita kuti SDSS ive nemutengo wakaderera10.
Munguva pfupi yapfuura, SDSS yakachinjwa nepurasitiki patembiricha dzakasiyana-siyana (tembiricha yakaderera, inotonhora uye inopisa) kuti iwane hunhu hwakanaka hwemakanika6,7,8. Zvisinei, kuramba kwakanaka kweSDSS kunokonzerwa nekuvapo kwefirimu diki re oxide pamusoro, iro rinokanganiswa nezvinhu zvakawanda, zvakaita sekuvapo kwezvikamu zvakawanda zvine miganhu yakasiyana yetsanga, precipitates isingadiwe uye maitiro akasiyana. chimiro chemukati chisina kufanana chezvikamu zvakasiyana-siyana zve austenitic ne ferritic chakachinjwa 7. Nokudaro, kudzidza nezvehunhu hwe microdomain yemafirimu akadaro padanho rechimiro chemagetsi kwakakosha zvikuru pakunzwisisa ngura yeSDSS uye kunoda matekiniki akaoma ekuyedza. Kusvika parizvino, nzira dzinonzwa pamusoro dzakadai seAuger electron spectroscopy11 uye X-ray photoelectron spectroscopy12,13,14,15 pamwe ne X-ray photoelectron photoelectron system yakaoma inosiyanisa, asi kazhinji inokundikana kuparadzanisa, mamiriro emakemikari echinhu chimwe chete munzvimbo dzakasiyana munzvimbo pane nanoscale. Zvidzidzo zvinoverengeka zvechangobva kuitwa zvakabatanidza oxidation yechromium yemuno nemaitiro ekuora akaonekwa esimbi 17 dze austenitic stainless, simbi 18 dze martensitic stainless, uye SDSS 19, 20. Zvisinei, zvidzidzo izvi zvakanyanya kutarisa pamhedzisiro yeCr heterogeneity (semuenzaniso, Cr3+ oxidation state) pakudzivirira ngura. Kusiyana kwemativi mumamiriro ekuoxidation ezvinhu kunogona kukonzerwa nemakomponi akasiyana ane zvinhu zvakafanana, senge iron oxides. Makomponi aya anogara nhaka saizi diki yakagadziriswa nethermomechanically iri pedyo, asi yakasiyana mukugadzirwa uye mamiriro ekuoxidation16,21. Nokudaro, kuratidza kuparadzwa kwemafirimu e oxide uye kukanda gomba kunoda kunzwisisa kusawirirana kwepamusoro pachiyero che microscopic. Pasinei nezvinodiwa izvi, kuongororwa kwehuwandu kwakadai se lateral oxidation heterogeneity, kunyanya yesimbi pa nano/atomic scale, kuchiri kushomeka uye kukosha kwayo pakudzivirira ngura kuchiri kusaongororwa. Kusvika nguva pfupi yadarika, mamiriro emakemikoro ezvinhu zvakasiyana-siyana, zvakaita seFe neCa, aitsanangurwa nehuwandu pamasampuli esimbi achishandisa soft X-ray photoelectron microscopy (X-PEEM) munzvimbo dze nanoscale synchrotron radiation. Pamwe chete nematekiniki eX-ray absorption spectroscopy (XAS) anonzwa makemikari, X-PEEM inogonesa kuyerwa kweXAS ne high spatial and spectral resolution, ichipa ruzivo rwekemikoro nezve elemental composition uye chemical state yayo ne spatial resolution kusvika pa nanometer scale 23. Kuongororwa uku kwe spectroscopic kwenzvimbo yekutanga pasi pe microscope kunorerutsa kuyedzwa kwekemikoro yemuno uye kunogona kuratidza spatial schanging dzekemikoro dzisina kumboongororwa muFe layer.
Chidzidzo ichi chinowedzera zvakanakira zvePEEM pakuona kusiyana kwemakemikari pa nanoscale uye chinopa nzira yekuongorora pamusoro peatomu yekunzwisisa maitiro ekuora kweCe-2507. Inoshandisa K-means cluster chemometric data24 kuronga huwandu hwemakemikari epasi rose (heterogeneity) yezvinhu zvinobatanidzwa, nemamiriro avo emakemikari anoratidzwa muchimiro chenhamba. Kusiyana nenyaya yechinyakare yekuora kunokonzerwa nekuputsika kwefirimu rechromium oxide, kusashanda zvakanaka kwepari zvino uye kusakwanisa kuramba ngura zvakanaka zvinokonzerwa nezvitsuwa zveFe3+ zvakapfuma zviri pedyo neFe/Cr oxide layer, izvo zvinogona kunge zviri mugumisiro weprotective oxides. Panzvimbo pekuputsika, firimu rinoumbwa rinokonzera ngura.
Maitiro ekuparadza eSDSS 2507 akakanganisika akatanga kuongororwa achishandisa zviyero zve electrochemical. Pamufananidzo 1 inoratidza makomba eNyquist neBode esampuli dzakasarudzwa mu acidic (pH = 1) aqueous solutions yeFeCl3 patembiricha yemumba. Electrolyte yakasarudzwa inoshanda semushonga wakasimba we oxidizing, ichiratidza maitiro epassivation film yekuputsika. Kunyangwe zvinhu zvisina kugadzikana mu room temperature pitting, ongororo idzi dzakapa ruzivo rwezviitiko zvinogona kukundikana uye maitiro e post-corrosion. Dunhu rakafanana (Mufananidzo 1d) rakashandiswa kuenderana ne electrochemical impedance spectroscopy (EIS) spectra, uye mhedzisiro inoenderana inoratidzwa muTafura 1. Half circles dzisina kukwana dzakaonekwa pakuyedzwa solution yakagadziriswa uye inopisa worked samples, nepo compiled half circles dzakatenderedzwa dzichitonhora (Mufananidzo 1b). MuEIS spectrum, semicircle radius inogona kutariswa se polarization resistance (Rp)25,26. Rp yeSDSS yakagadziriswa muTafura 1 inenge 135 kΩ cm-2, zvisinei kune SDSS yakapiswa uye yakaputirwa inotonhora tinogona kuona kukosha kwakaderera kwe34.7 ne2.1 kΩ cm–2 zvichiteerana. Kudzikira uku kwakakosha muRp kunoratidza mhedzisiro yakaipa yekuchinja kwepurasitiki pakudzivirira ngura uye kuramba ngura, sezvakaratidzwa mumishumo yapfuura 27, 28, 29, 30.
a Nyquist, b, c Bode impedance uye phase diagrams, uye equivalent circuit model ye d, uko RS iri resistance ye electrolyte, Rp iri polarization resistance, uye QCPE ndiyo constant phase element oxide inoshandiswa kumodela non-ideal capacitance (n) . Kuyerwa kweEIS kwakaitwa pasina mutoro.
Ma constant ekutanga anoratidzwa muBode diagram uye high frequency plateau inomiririra electrolyte resistance RS26. Sezvo frequency ichidzikira, impedance inowedzera uye negative phase angle inowanikwa, zvichiratidza capacitance dominance. Phase angle inowedzera, ichichengetedza kukosha kwayo kukuru muhuwandu hwakafara hwefrequency, uye yobva yadzikira (Mufananidzo 1c). Zvisinei, muzviitiko zvese zvitatu izvi zvakanyanya kukosha kuchiri pasi pe90°, zvichiratidza maitiro asina kunaka e capacitive nekuda kwekupararira kwe capacitive. Saka, QCPE constant phase element (CPE) inoshandiswa kumiririra interfacial capacitance distribution inobva mukukombama kwesurface kana inhomogeneity, kunyanya maererano neatomic scale, fractal geometry, electrode porosity, non-uniform potential, uye surface dependent current distribution. Electrode geometry31,32. CPE impedance:
apo j iri nhamba yekufungidzira uye ω iri angular frequency. QCPE inguva isingachinji yakazvimirira inoenderana nenzvimbo yakavhurika ye electrolyte. n inhamba yesimba isina dimension inotsanangura kutsauka kubva pamaitiro akanaka e capacitor, kureva kuti kana n iri pedyo ne1, CPE iri pedyo ne capacitance yakachena, uye kana n iri pedyo ne zero, i resistance. Kutsauka kudiki kwe n, pedyo ne 1, kunoratidza maitiro asina kunaka e capacitive epamusoro mushure mekuedzwa kwe polarization. QCPE ye cold rolled SDSS yakakwira zvakanyanya kupfuura zvigadzirwa zvakafanana, zvinoreva kuti mhando yekumusoro haina kufanana zvakanyanya.
Zvichienderana nehukuru hwesimbi dzisingapindi ngura, huwandu hwakawanda hweSDSS hunowanzo kukonzera kuramba ngura kwakanyanya kweSDSS nekuda kwekuvapo kwefirimu rekudzivirira oxide risingapindi ngura pamusoro17. Iyi firimu inofamba kazhinji ine Cr3+ oxides uye/kana hydroxides, inonyanya kubatanidza Fe2+, Fe3+ oxides uye/kana (oxy) hydroxides 33. Pasinei nekufanana kwepamusoro, passivating oxide layer, uye pasina kuputsika kunoonekwa pamusoro, sezvinotsanangurwa nemifananidzo midiki,6,7 maitiro ekuora kweSDSS yakapiswa uye yakaputirwa nechando akasiyana uye nekudaro inoda kudzidza kwakadzama kwedeformation microstructure uye chimiro chechimiro chesimbi.
Maumbirwo esimbi isina tsvina yakakanganisika akaongororwa nehuwandu hwezvinhu uchishandisa maX-ray emukati nesynchrotron ane simba guru (Mifananidzo Yekuwedzera 1, 2). Ongororo yakadzama inopihwa muRuzivo Rwekuwedzera. Kunyangwe izvi zvichinyanya kufanana nerudzi rwechikamu chikuru, misiyano yakawanikwa muzvikamu zvehuwandu hwezvikamu, zvakanyorwa muTafura Yekuwedzera 1. Musiyano uyu unogona kunge uri nekuda kwechikamu chechikamu chakasiyana pamusoro nechikamu chehuwandu (XRD) zvichienderana nekudzika kwakasiyana kwekuonekwa nekushandisa X-ray diffraction ine masosi akasiyana-siyana esimba ezviitiko zvemaphoton. Chikamu chakakwira cheaustenite muzvienzaniso zvakaputirwa zvinotonhora, zvakatemwa neXRD kubva kunobva murabhoritari, zvinoratidza kuti pane passivation iri nani uye zvinozotevera kuramba kuri nani ngura35, nepo mhedzisiro yakarurama uye yehuwandu ichiratidza maitiro akasiyana muzvikamu. Pamusoro pezvo, kuramba ngura kwesimbi kunoenderanawo nehuwandu hwekugadziriswa kwezviyo, kuderedza saizi yezviyo, kuwedzera kwekushanduka kwemicroformations uye dislocation density inoitika panguva yekurapa kwethermomechanical36,37,38. Mienzaniso yakagadzirwa nekupisa inoratidza hunhu hwemagiraidhi akawanda, zvichiratidza kuti ine magiraidhi madiki, nepo mhete dzakatsetseka dzakaonekwa mumienzaniso yakaputirwa nechando (Mufananidzo Wekuwedzera 3) dzinoratidza kunatswa kwakakosha kwegiraidhi kusvika padiki pane imwe nguva yapfuura, izvo zvinofanirwa kubatsira pakuumbwa kwepasi pefirimu uye kuwedzera kwekusagadzikana kwengura. Kuwanda kwe dislocation density kunowanzobatanidzwa nekusagadzikana kwakaderera kune pitting, izvo zvinoenderana zvakanaka nekuyerwa kwe electrochemical.
Kuchinja kwemakemikari e microdomains yezvinhu zvepakutanga kwakadzidzwa zvakarongeka uchishandisa X-PEEM. Pasinei nekuwanda kwezvinhu zvinosanganisa, Cr, Fe, Ni, uye Ce39 zvakasarudzwa pano nekuti Cr ndiyo chinhu chakakosha pakuumbwa kwefirimu repassivation, Fe ndiyo chinhu chikuru musimbi, uye Ni inowedzera passivation uye inoenzanisa chimiro che ferrite-austenitic phase uye chinangwa chekugadzirisa Ce. Nekugadzirisa simba remwaranzi ye synchrotron, RAS yakaputirwa kubva pamusoro nezvinhu zvikuru zveCr (edge ​​​​L2.3), Fe (edge ​​​​L2.3), Ni (edge ​​​​L2.3) uye Ce (edge ​​​​M4.5). hot forming uye cold rolling Ce-2507 SDSS. Kuongororwa kwedata kwakakodzera kwakaitwa nekubatanidza energy calibration nedata rakabudiswa (semuenzaniso XAS 40, 41 paFe L2, 3 edges).
Pamufananidzo. Mufananidzo 2 unoratidza mifananidzo yeX-PEEM yemagetsi anopisa (Mufananidzo 2a) uye akaputirwa nechando (Mufananidzo 2d) Ce-2507 SDSS uye mipendero yeXAS inoenderana yeCr neFe L2,3 panzvimbo dzakanyorwa zvakasiyana. Mupendero weL2,3 weXAS unoongorora mamiriro e3d asina chinhu mushure meelectron photoexcitation pamazinga ekupatsanurana kwespin-orbit 2p3/2 (mupendero weL3) uye 2p1/2 (mupendero weL2). Ruzivo nezvemamiriro eCr aCr akawanikwa kubva kuXAS pamupendero weL2,3 muMufananidzo 2b, e. Kuenzanisa nevatongi. 42,43 yakaratidza kuti misoro mina yakaonekwa pedyo nemupendero weL3, inonzi A (578.3 eV), B (579.5 eV), C (580.4 eV) naD (582.2 eV), ichiratidza octahedral Cr3+, inoenderana neCr2O3 ion. Maspectra ekuyedza anobvumirana nekuverenga kwedzidziso kunoratidzwa mumapaneru b na e, akawanikwa kubva mukuverenga kwakawanda kwemunda wekristaro paCr L2.3 interface uchishandisa munda wekristaro we2.0 eV44. Nzvimbo dzese dziri mbiri dzeSDSS dzakagadzirwa nekupisa nedzakaputirwa nechando dzakaputirwa nechikamu chakafanana cheCr2O3.
Mufananidzo wekupisa weX-PEEM weSDSS yakakanganisika pakupisa unoenderana ne b Cr L2.3 edge uye c Fe L2.3 edge, d Mufananidzo wekupisa weX-PEEM weSDSS yakaputirwa nechando unoenderana ne e Cr L2.3 edge uye f Fe L2 .3 edge side (f). MaXAS spectra akarongwa panzvimbo dzakasiyana dzakanyorwa pamifananidzo yekupisa (a, d), mitsetse yeorenji ine madotsi mu (b) uye (e) inomiririra XAS spectra yakaedzwa yeCr3+ ine crystal field value ye2.0 eV. Pamifananidzo yeX-PEEM, shandisa palette yekupisa kuti uvandudze kuverenga kwemufananidzo, uko mavara kubva pabhuruu kusvika kutsvuku anoenderana nekusimba kweX-ray absorption (kubva pasi kusvika kumusoro).
Pasinei nemamiriro ezvinhu emakemikari ezvinhu izvi zvesimbi, mamiriro emakemikari ekuwedzera kwezvinhu zveNi neCe alloying kune ese ari maviri haana kuchinja. Mufananidzo wekuwedzera. Mifananidzo 5-9 inoratidza mifananidzo yeX-PEEM uye maXAS spectra anoenderana eNi neCe panzvimbo dzakasiyana pamusoro pezvinhu zvakapiswa uye zvakaputirwa nechando. Ni XAS inoratidza mamiriro e oxidation eNi2+ pamusoro pese pakaenzana pezvinhu zvakapiswa uye zvakaputirwa nechando (Kukurukurirana Kwekuwedzera). Zvinofanira kucherechedzwa kuti, pamienzaniso yakapiswa, chiratidzo cheXAS cheCe hachina kuonekwa, nepo pamienzaniso yakaputika nechando, spectrum yeCe3+ yakaonekwa. Kuonekwa kwemavara eCe mumienzaniso yakaputika nechando kwakaratidza kuti Ce inonyanya kuonekwa muchimiro che precipitates.
MuSDSS yakakanganisika nekupisa, hapana shanduko yenzvimbo muXAS pamucheto weFe L2,3 yakaonekwa (Mufananidzo 2c). Zvisinei, Fe matrix micro-regionally inochinja mamiriro ayo emakemikari panzvimbo nomwe dzakasarudzwa zvisina kurongeka dzeSDSS yakaputirwa nechando, sezvakaratidzwa muMufananidzo 2f. Pamusoro pezvo, kuti tiwane pfungwa chaiyo yekuchinja kwemamiriro eFe panzvimbo dzakasarudzwa muMufananidzo 2f, zvidzidzo zvepanzvimbo zvakaitwa (Mufananidzo 3 neMufananidzo Wekuwedzera 10) umo nzvimbo diki dzakatenderera dzakasarudzwa. XAS spectra yeFe L2,3 edge yeα-Fe2O3 systems uye Fe2+ octahedral oxides dzakagadzirwa nekuverenga kwakawanda kwecrystal field uchishandisa minda yecrystal ye1.0 (Fe2+) uye 1.0 (Fe3+)44. Tinoona kuti α-Fe2O3 uye γ-Fe2O3 dzine symmetries dzakasiyana dzemuno45,46, Fe3O4 ine musanganiswa weFe2+ & Fe3+,47, uye FeO45 seFe2+ oxide yakaparadzaniswa (3d6). Tinoona kuti α-Fe2O3 uye γ-Fe2O3 dzine symmetries dzakasiyana dzemuno45,46, Fe3O4 ine musanganiswa weFe2+ & Fe3+,47, uye FeO45 seFe2+ oxide yakaparadzaniswa (3d6).Cherechedza kuti α-Fe2O3 uye γ-Fe2O3 dzine symmetries dzakasiyana dzemuno45,46, Fe3O4 inosanganisa Fe2+ neFe3+,47 neFeO45 muchimiro che formally divalent oxide Fe2+ (3d6).Cherechedza kuti α-Fe2O3 uye γ-Fe2O3 dzine ma symmetries akasiyana emunharaunda45,46, Fe3O4 ine musanganiswa weFe2+ neFe3+,47 uye FeO45 inoshanda seye formal divalent Fe2+ oxide (3d6). Ma ions ese eFe3+ mu α-Fe2O3 ane nzvimbo dzeOh chete, nepo γ-Fe2O3 inowanzo miririrwa neFe3+ t2g [Fe3+5/3V1/3]eg O4 spinel ine nzvimbo dzisina chinhu mu semuenzaniso nzvimbo. Nokudaro, ma ions eFe3+ mu γ-Fe2O3 ane nzvimbo dzeTd neOh. Sezvambotaurwa mupepa rapfuura,45 kunyangwe chiyero chesimba chezviviri chakasiyana, chiyero chavo chesimba eg/t2g chiri ≈1, nepo muchiitiko ichi chiyero chesimba chakacherechedzwa eg/t2g chiri 1. Izvi zvinobvisa mukana wekuti mumamiriro ezvinhu aripo pari zvino chete ndiFe3+ iripo. Tichifunga nezveFe3O4 neFe2+ neFe3+, chinhu chekutanga, chinozivikanwa nekuva nemucheto weL3 usina simba (wakasimba) weFe, chinoratidza huwandu hudiki (hwakakura) hwemamiriro eT2g asina vanhu. Izvi zvinoshanda kuFe2+ (Fe3+), izvo zvinoratidza kuti chinhu chekutanga chekuwedzera chinoratidza kuwedzera kwehuwandu hweFe2+47. Mhedzisiro iyi inoratidza kuti kugara pamwe chete kweFe2+ neγ-Fe2O3, α-Fe2O3 uye/kana Fe3O4 kunotonga pamusoro pezvinhu zvinosanganiswa zvinotonhora.
Mifananidzo yakakura yemifananidzo yekupisa ye photoelectron yeXAS spectra (a, c) uye (b, d) ichiyambuka mupendero weFe L2,3 panzvimbo dzakasiyana-siyana mukati menzvimbo dzakasarudzwa 2 neE muMifananidzo 2d.
Data rekuyedza rakawanikwa (Mufananidzo 4a neMufananidzo Wekuwedzera 11) rakarongwa uye rakaenzaniswa nedata remakemikari akachena 40, 41, 48. Mhando nhatu dzakasiyana dzeFe L-edge XAS spectra dzakaonekwa nekuyedza (XAS-1, XAS-2 uye XAS-3: Mufananidzo 4a). Kunyanya, spectrum 2-a (inoratidzwa seXAS-1) muMufananidzo 3b ichiteverwa nespectrum 2-b (yakanyorwa seXAS-2) yakaonekwa pamusoro penzvimbo yese yekuona, nepo maspectra akaita seE-3 akaonekwa mumufananidzo 3d (akanyorwa seXAS-3) akaonekwa panzvimbo dzakatarwa. Semutemo, maparameter mana akashandiswa kuziva mamiriro aripo evalence mumuenzaniso uri kudzidzwa: (1) hunhu hwespectral L3 neL2, (2) nzvimbo dzesimba dzehunhu hweL3 neL2, (3) musiyano wesimba L3-L2., (4) L2/L3 intensity ratio. Zvichienderana nezvakaonekwa (Mufananidzo 4a), zvikamu zvitatu zveFe, zvinoti, Fe0, Fe2+, uye Fe3+, zviripo pamusoro peSDSS iri kuferefetwa. Chiyero chesimba chakaverengerwa L2/L3 chakaratidzawo kuvapo kwezvikamu zvitatu izvi.
maSpektara eXAS akaenzaniswa eFe ane data rekuyedza rakaonekwa katatu (mitsara yakasimba XAS-1, XAS-2 uye XAS-3 inoenderana ne2-a, 2-b uye E-3 muMufananidzo 2 ne3) Kuenzanisa , Octahedrons Fe2+, Fe3+ ine crystal field values ​​​​ye1.0 eV uye 1.5 eV, zvichiteerana, data rekuyedza rakayerwa ne bd (XAS-1, XAS-2, XAS-3) uye data reLCF rakagadziriswa rinoenderana (mutsara mutema wakasimba), uye zvakare muchimiro cheXAS-3 spectra ine Fe3O4 (mamiriro akasanganiswa eFe) uye Fe2O3 (pure Fe3+) standards.
Kubatanidzwa kwemutsara (LCF) kwematanho matatu 40, 41, 48 kwakashandiswa kuyera kuumbwa kwesimbi oxide. LCF yakashandiswa kune matatu akasarudzwa eFe L-edge XAS spectra anoratidza musiyano wepamusoro, kureva XAS-1, XAS-2 uye XAS-3, sezvakaratidzwa muMufananidzo 4b–d. Kune maLCF fittings, 10% Fe0 yakafungwa muzviitiko zvese nekuda kwekuti takaona chikamu chidiki mudata rese, uye zvakare nekuda kwekuti simbi yesimbi ndiyo chinhu chikuru chesimbi. Zvechokwadi, kudzika kweprobation kweX-PEEM yeFe (~6 nm)49 kwakakura kupfuura ukobvu hweoxidation layer hunofungidzirwa (zvishoma > 4 nm), zvichibvumira kuonekwa kwechiratidzo kubva ku iron matrix (Fe0) pasi pe passivation layer. Zvechokwadi, kudzika kweprobation kweX-PEEM yeFe (~6 nm)49 kwakakura kupfuura ukobvu hweoxidation layer hunofungidzirwa (zvishoma > 4 nm), zvichibvumira kuonekwa kwechiratidzo kubva ku iron matrix (Fe0) pasi pe passivation layer. Действительно, пробная глубина X-PEEM для Fe (~ 6 нм)49 больше, чем предполагаемая толщина слоя окисления (немного > 4 нзбина сигнал от железной матрицы (Fe0) под пассивирующим слоем. Zvechokwadi, kudzika kweprobe X-PEEM yeFe (~6 nm)49 kwakakura kupfuura ukobvu hunofungidzirwa hweoxidation layer (zvishoma >4 nm), izvo zvinoita kuti zvikwanisike kuona chiratidzo kubva ku iron matrix (Fe0) pasi pe passivation layer.事实上，X-PEEM 对Fe（~6 nm）49 的检测深度大于估计的氧化层厚度（略> 4 nm），允许检测來自钝化层下方的铁基体（Fe0）的信号.事实上 , X-PEEM 对 Fe （~ 6 nm） 49 的 检测 深度 大于 的 氧化层 厚度 略 略> 4 nm） 允杀 允手下方 铁基体 （fe0） 的。 信号 信号 信号 信号Фактически, глубина обнаружения Fe (~ 6 нм) 49 с помощью X-PEEM больше, чем предполагаемая толщина оксидного слоя (немного > 4 обнаруживать сигнал от железной матрицы (Fe0) ниже пассивирующего слоя. Kutaura zvazviri, kudzika kwekuonekwa kweFe (~6 nm) 49 neX-PEEM kwakakura kupfuura ukobvu hunotarisirwa hwe oxide layer (zvishoma > 4 nm), izvo zvinobvumira kuonekwa kwechiratidzo kubva ku iron matrix (Fe0) pasi pe passivation layer. .Kusanganiswa kwakasiyana-siyana kweFe2+ neFe3+ kwakaitwa kuti pave nemhinduro yakanakisisa yedata rekuyedza rakaonekwa. Pamufananidzo 4b panoratidza XAS-1 spectrum yekusanganiswa kweFe2+ neFe3+, uko huwandu hweFe2+ neFe3+ hwakafanana neinenge 45%, zvichiratidza mamiriro akasiyana eFe2. Kunyange zvazvo paXAS-2 spectrum, chikamu cheFe2+ neFe3+ chinova ~30% uye 60%, zvichiteerana. Fe2+ ​​iri pasi peFe3+. Chiyero cheFe2+ neFe3, chakaenzana ne1:2, zvinoreva kuti Fe3O4 inogona kuumbwa pachiyero chimwe chete pakati peFe ions. Pamusoro pezvo, paXAS-3 spectrum, chikamu cheFe2+ neFe3+ chinova ~10% uye 80%, izvo zvinoratidza kushandurwa kwakanyanya kweFe2+ kuenda kuFe3+. Sezvambotaurwa pamusoro apa, Fe3+ inogona kubva kuα-Fe2O3, γ-Fe2O3 kana Fe3O4. Kuti tinzwisise kwainonyanya kukonzera Fe3+, XAS-3 spectrum yakarongwa neFe3+ standards dzakasiyana muMufananidzo 4e, zvichiratidza kufanana nezvinodiwa zvese izvi pakufunga nezve B peak. Zvisinei, simba remapendekete epafudzi (A: kubva kuFe2+) uye B/A intensity ratio zvinoratidza kuti spectrum yeXAS-3 iri pedyo, asi haienderane ne spectrum yeγ-Fe2O3. Zvichienzaniswa ne bulk γ-Fe2O3, Fe 2p XAS peak yeA SDSS ine simba rakakwira zvishoma (Mufananidzo 4e), izvo zvinoratidza simba rakakwira reFe2+. Kunyangwe spectrum yeXAS-3 yakafanana neyeγ-Fe2O3, uko Fe3+ iripo munzvimbo dzeOh neTd, kuzivikanwa kwemamiriro akasiyana evalence uye kubatana chete pamucheto weL2,3 kana L2/L3 intensity ratio ichiri dambudziko. inyaya inoenderera mberi yekukurukurirana nekuda kwekuoma kwezvinhu zvakasiyana-siyana zvinokanganisa final spectrum41.
Pamusoro pekusiyana kwemaspectral mumamiriro emakemikari enzvimbo dzakasarudzwa dzatsanangurwa pamusoro apa, kusiyana kwemakemikari epasi rose kwezvinhu zvakakosha Cr naFe kwakaongororwawo nekuisa muzvikamu zvese zveXAS spectra zvakawanikwa pamusoro pemuenzaniso uchishandisa nzira yeK-means clustering. . Edge profiles Cr L yakagadzirirwa kuumba mapoka maviri akakodzera akapararira munzvimbo dzakapiswa uye dzakatonhora dzakaputirwa mumifananidzo inoratidzwa muMifananidzo 5. Zviri pachena kuti hapana shanduko dzemunzvimbo dzinoonekwa sedzakafanana, sezvo macentroid maviri eXAS Cr spectra akafanana. Aya maspectral shapes emaboka maviri akafanana neaya anoenderana neCr2O342, zvinoreva kuti maCr2O3 layers akapatsanurwa zvakaenzana paSDSS.
Cr L K-means edge region clusters, uye b ndiyo XAS centroids inoenderana. Mhedzisiro yekuenzanisa K-means X-PEEM ye cold-rolled SDSS: c Cr L2.3 edge region yeK-means clusters uye d inoenderana XAS centroids.
Kuti tiratidze mamepu emucheto eFeL akaomarara, ma clusters mana ne mashanu akagadziridzwa uye ma centroids akabatana nawo (spectral profiles) akashandiswa pasampuli dzakagadzirwa nekupisa nedzinotonhorera, zvichiteerana. Nokudaro, chikamu (%) cheFe2+ neFe3+ chinogona kuwanikwa nekuisa LCF inoratidzwa muMufananidzo 4. Pseudo potential sebasa reFe0 yakashandiswa kuratidza kusawirirana kwemakemikari emufirimu wepamusoro we oxide. Epseudo inofungidzirwa nemutemo wekusanganisa,
apo \(\rm{E}_{\rm{Fe}/\rm{Fe}^{2 + (3 + )}}\) yakaenzana \(\rm{Fe} + 2e^ – \ ku \rm {Fe}^{2 + (3 + )}\), 0.440 uye 0.036 V, zvichiteerana. Nzvimbo dzine mukana wakaderera dzine huwandu hwakakwira hweFe3+ compound. Kugoverwa kwemukana musampuli dzakagadziriswa nekupisa kune hunhu hwakarongwa nekuchinja kukuru kweinenge 0.119 V (Mufananidzo 6a, b). Kugoverwa uku kwemukana kwakabatana zvakanyanya nepamusoro penzvimbo (Mufananidzo 6a). Hapana dzimwe shanduko dzinoenderana nenzvimbo mukati me laminar dzakaonekwa (Mufananidzo 6b). Kusiyana neizvi, pakubatana kwema oxide akasiyana nezviri mukati zvakasiyana zveFe2+ neFe3+ mu SDSS yakaputirwa nechando, munhu anogona kuona hunhu husina kufanana hwemukana wepseudo (Mufananidzo 6c, d). MaFe3+ oxides uye/kana (oxy) hydroxides ndizvo zvinonyanya kukonzera ngura musimbi uye zvinopinda muokisijeni nemvura50. Muchiitiko ichi, zvitsuwa zvakapfuma muFe3+ zvinoonekwa sezviri munzvimbo uye zvinogona kuonekwa senzvimbo dzine ngura. Panguva imwe chete, gradient mumunda une potential, pane kukosha kwakakwana kwe potential, inogona kushandiswa sechiratidzo chekuwanikwa kwenzvimbo dzine corrosion. Kupararira kusina kuenzana kweFe2+ neFe3+ pamusoro peSDSS inotonhora kunogona kushandura chemistry yemuno uye kupa nzvimbo inoshanda zvakanyanya mukuputsika kwefirimu re oxide uye maitiro ekuora, nokudaro zvichibvumira ngura inoramba ichienderera ye matrix yesimbi iri pasi, zvichikonzera ngura yemukati. kusiyana kwezvimiro uye kudzikira kwezvimiro zvekudzivirira zve passivating layer.
Mapoka eK-means uye maXAS centroids anoenderana munzvimbo yeFe L2.3 emucheto yeX-PEEM ac nedf yeSDSS yakaputirwa nechando. a, d Mapoka eK-means cluster akaputirwa pamifananidzo yeX-PEEM. Pseudo potential yakaverengerwa (Epseudo) inotaurwa pamwe chete neK-means cluster plot. Kupenya kwemufananidzo weX-PEEM, seruvara rwuri muMufananidzo 2 kunoenderana nekusimba kweX-ray absorption.
Kuenzana kweCr asi mamiriro akasiyana emakemikari eFe anotungamira mukukuvadzwa kwakasiyana kwefirimu re oxide uye mapatani ekuora muCe-2507 yakapiswa uye yakaputirwa nechando. Hunhu uhwu hweCe-2507 yakaputirwa nechando hwakadzidzwa zvakanaka. Nezvekuumbwa kwema oxide nema hydroxide eFe mumhepo iri mukushanda uku kunenge kusina kusimba, maitiro acho ndeaya anotevera:
Maitiro ari pamusoro apa anoitika mumamiriro ezvinhu anotevera zvichibva pakuongorora kweX-PEEM. Bandauko diki rinoenderana neFe0 rinobatanidzwa nesimbi iri pasi. Maitiro esimbi yeFe nenharaunda anokonzera kuumbwa kweFe(OH)2 layer (equation (5)), iyo inowedzera chiratidzo cheFe2+ muFe L-edge XAS. Kuratidzwa kwenguva refu mumhepo kunogona kukonzera kuumbwa kweFe3O4 uye/kana Fe2O3 oxides mushure meFe(OH)252,53. Mhando mbiri dzakagadzikana dzeFe, Fe3O4 neFe2O3, dzinogonawo kuumbwa muCr3+ rich protective layer, iyo Fe3O4 inofarira chimiro chakafanana uye chinonamira. Kuvapo kwezvose izvi kunoguma nemamiriro akasiyana e oxidation (XAS-1 spectrum). XAS-2 spectrum inonyanya kuenderana neFe3O4. Kunyange zvazvo kuonekwa kweXAS-3 spectra munzvimbo dzinoverengeka kwakaratidza kushanduka kwakazara ku γ-Fe2O3. Sezvo kudzika kwekupinda kweX-rays dzakavhurika kuri 50 nm, chiratidzo chinobva pasi chinoita kuti A peak iwedzere.
XPA spectrum inoratidza kuti chikamu cheFe mufirimu re oxide chine chimiro chakaiswa pamwe chete neCr oxide layer. Kusiyana nezviratidzo zvekusagadzikana nekuda kwekusawirirana kweCr2O3 panguva yekuora, pasinei nechikamu chakafanana cheCr2O3 mubasa iri, kuramba kwakaderera kwekuora kunoonekwa munyaya iyi, kunyanya kune sampuli dzakaputirwa nechando. Maitiro akaonekwa anogona kunzwisiswa sekusawirirana kwemamiriro ekuoxidation kwemakemikari muchikamu chepamusoro (Fe), izvo zvinokanganisa mashandiro ekuora. Nekuda kwestoichiometry yakafanana yechikamu chepamusoro (iron oxide) nechikamu chezasi (chromium oxide)52,53 kudyidzana kuri nani (kunamatira) pakati pavo kunotungamira kutakurwa zvishoma nezvishoma kwemaion esimbi kana oxygen mu lattice, izvo, zvinotungamira mukuwedzera kwekurasika. Naizvozvo, chiyero chestoichiometric chinoenderera mberi, kureva mamiriro eoxidation eFe, chinodiwa pane kuchinja kwestoichiometric kamwe kamwe. SDSS yakachinja kupisa ine nzvimbo yakafanana, denser protective layer, uye kuramba kuri nani kwekuora. Nepo kune SDSS inotonhorera, kuvapo kwezvitsuwa zveFe3+-rich pasi pechikamu chekudzivirira kunokanganisa kusimba kwenzvimbo uye kunokonzera ngura yegalvanic ne substrate iri pedyo, izvo zvinotungamira kudonha kwakanyanya kweRp (Tafura 1). Iyo EIS spectrum uye kuramba kwayo ngura zvakaderera. Zvinogona kuonekwa kuti kupararira kwezvitsuwa zveFe3+ rich nekuda kwekuchinja kwepurasitiki kunonyanya kukanganisa kuramba ngura, inova budiriro mubasa iri. Saka, chidzidzo ichi chinopa mifananidzo ye spectroscopic microscopic yekudzikira kwekurasika kweSDSS samples dzakadzidzwa nenzira yekuchinja kwepurasitiki.
Pamusoro pezvo, kunyangwe kusanganisa zvinhu zvepasi zvisingawanzoonekwi musimbi dzine zvikamu zviviri kuchiratidza kushanda kuri nani, kudyidzana kwechinhu ichi chinowedzera nesimbi imwe neimwe maererano nemaitiro ekuora zvichienderana nedata re spectroscopic microscopy kuchiri kuomera. Kuonekwa kwezviratidzo zveCe (kuburikidza neXAS M-edges) kunoonekwa munzvimbo shoma chete panguva yekutenderera kunotonhora, asi kunonyangarika panguva yekushanduka kweSDSS, zvichiratidza kunaya kweCe musimbi, pane kusanganisa kwakafanana. Kunyangwe zvisiri kuvandudza zvakanyanya hunhu hwemakanika hweSDSS6,7, kuvapo kwezvinhu zvepasi zvisingawanzoonekwi kunoderedza saizi yezvinobatanidzwa uye kunofungidzirwa kuti kunodzivirira kudonha kwegomba munzvimbo yekutanga54.
Mukupedzisa, basa iri rinoburitsa pachena mhedzisiro yekusiyana kwenzvimbo pamusoro pengura ye2507 SDSS yakagadziriswa necerium nekuyera huwandu hwemakemikari ari muzvikamu zve nanoscale. Tinopindura mubvunzo wekuti sei simbi isingatsvedzeri ichiora kunyangwe iri pasi pe protective oxide layer nekuyera microstructure yayo, surface chemistry, uye signal processing uchishandisa K-means clustering. Zvave pachena kuti zvitsuwa zvakapfuma muFe3+, kusanganisira octahedral ne tetrahedral coordination pamwe chete ne mixed Fe2+/Fe3+, ndizvo zvinokonzera kukuvara nekuora kwe cold-rolled oxide film SDSS. Nanoislands inotongwa neFe3+ inotungamira mukusagadzikana kwekuora kunyangwe paine stoichiometric Cr2O3 passivating layer yakakwana. Kuwedzera pakufambira mberi kwemaitiro mukuona mhedzisiro yekusiyana kwemakemikari e nanoscale pakuora, basa riri kuenderera mberi rinotarisirwa kukurudzira maitiro einjiniya ekuvandudza kuramba kwekuora kwesimbi dzisingatsvedzeri panguva yekugadzira simbi.
Kugadzira ingot yeCe-2507 SDSS yakashandiswa muchidzidzo ichi, musanganiswa wakasanganiswa unosanganisira Fe-Ce master alloy yakavharwa nechubhu yesimbi yakachena yakanyungudutswa muchoto che 150 kg che medium frequency induction kuti igadzire simbi yakanyungudutswa ndokudururwa muchiumbwa. Makemikoro akayerwa (wt%) akanyorwa muSupplementary Table 2. Mangot anotanga agadzirwa kuita mabhuroko anopisa. Zvadaro akanyungudutswa pa1050°C kwemaminitsi makumi matanhatu kuti simbi iwane solution yakasimba, uye yozodzimwa mumvura kusvika patembiricha yemukamuri. Samples dzakadzidzwa dzakadzidzwa zvakadzama uchishandisa TEM neDOE kuti dzidzidze zvikamu, saizi yetsanga uye morphology. Ruzivo rwakadzama nezvesamples uye maitiro ekugadzira runogona kuwanikwa mune mamwe masosi6,7.
Samples dze cylindrical (φ10 mm×15 mm) dzekupisa dzakagadziriswa kuitira kuti axis ye cylinder ienderane nekwakagadziriswa kwe block. Kudzvanywa kwekupisa kwakanyanya kwakaitwa patembiricha dzakasiyana dziri pakati pe 1000-1150°C uchishandisa Gleeble-3800 thermal simulator pa constant strain rate iri pakati pe 0.01-10 s-1. Samples dzisati dzagadziriswa, dzaipiswa pa 10 °C s-1 kwemaminitsi maviri pa tembiricha yakasarudzwa kubvisa gradient ye tembiricha. Mushure mekusvika pakufanana kwe tembiricha, sample yakachinjwa kusvika pa true strain value ye 0.7. Mushure mekugadziriswa, samples dzakadzimwa nemvura nekukurumidza kuchengetedza chimiro chakachinjwa. Sampuro yakaomeswa inochekwa ichienda kune kwayakagadziriswa. Pachidzidzo ichi, takasarudza sampuro ine hot strain condition ye 1050°C, 10 s-1 nekuti microhardness yakaonekwa yaive yakakwira kupfuura dzimwe sampuro7.
Mienzaniso mikuru (80 × 10 × 17 mm3) yeCe-2507 solid solution yakashandiswa muLG-300 three-phase asynchronous two-roll mill ine hunhu hwakanaka pakati pemamwe mazinga ese ekuchinja6. Kuderedzwa kwekusvuta uye ukobvu hwenzira yega yega ndeye 0.2 m·s-1 uye 5%, zvichiteerana.
Nzvimbo yekushandira yemagetsi yeAutolab PGSTAT128N yakashandiswa pakuyera electrochemical yeSDSS mushure mekukanda nechando kusvika pa90% muukobvu (1.0 yakaenzana ne true strain) uye mushure mekudzvanya kupisa pa1050°C kwe10 s-1 kusvika pa true strain ye0.7. Nzvimbo yekushandira ine cell ine maelectrode matatu ine calomel electrode yakaguta se electrode yekutarisa, graphite counter electrode, uye SDSS sample se electrode inoshanda. Masamples akachekwa kuita masilinda ane dhayamita ye11.3 mm, kumativi ayo waya dzemhangura dzakasungirirwa. Masamples akazogadziriswa ne epoxy, zvichisiya nzvimbo yakashama ye1 cm2 se electrode inoshanda (rutivi rwepasi rwe cylindrical sample). Chenjerera panguva yekuchenesa epoxy uye sanding ne polishing inotevera kuti isatsemuke. Nzvimbo dzekushanda dzakakuyiwa uye dzakapukutwa ne diamond polishing suspension ine saizi ye particle ye1 μm, dzakagezwa nemvura yakasanganiswa ne ethanol, uye dzakaomeswa mumhepo inotonhora. Pamberi pekuyera electrochemical, masamples akapukutwa aiiswa mumhepo kwemazuva akati wandei kuti agadzire natural oxide film. Mhinduro yemvura yeFeCl3 (6.0 wt%), yakagadzika kusvika pH = 1.0 ± 0.01 neHCl zvichienderana neASTM, inoshandiswa kukurumidzisa ngura yesimbi isingatsvedzi55 nekuti inoparadza kana paine ma chloride ions ine simba rakasimba re oxidizing uye pH yakaderera. Environmental standards G48 naA923. Nyikai sampuro mu test solution kweawa imwe chete kuti musvike pedyo ne steady state musati maita chero zviyero. Kune solid-solution, hot-formed, uye cold-rolled sampuro, impedance measurements dzakaitwa pa open circuit potentials (OPC) ye0.39, 0.33, uye 0.25 V, zvichiteerana, mu frequency range kubva pa1 105 kusvika 0.1 Hz ne amplitude ye5 mV. Miedzo yese yemakemikari yakadzokororwa kanenge katatu pasi pemamiriro akafanana kuti ive nechokwadi chekuti data rinodzokororwazve.
Pakuyerwa kweHE-SXRD, mabhuroko esimbi ane rectangular duplex ane 1 × 1 × 1.5 mm3 akayerwa kuti aone kuti chidimbu che beam phase cheBrockhouse high-energy wiggler chiri paCLS, Canada56 chakaita sei. Kuunganidzwa kwedata kwakaitwa muDebye-Scherrer geometry kana transmission geometry patembiricha yemumba. X-ray wavelength yakayerwa neLaB6 calibrator i0.212561 Å, iyo inoenderana ne58 keV, iyo yakakwira zvikuru kupfuura iyo yeCu Kα (8 keV) inowanzoshandiswa seyero reX-ray remurabhoritari. Sampuro iyi yaive kure ne740 mm kubva kune detector. Vhoriyamu yekuona yesampuro yega yega i0.2 × 0.3 × 1.5 mm3, iyo inotsanangurwa nehukuru hwe beam uye ukobvu hwesampuro. Data rese rakaunganidzwa pachishandiswa Perkin Elmer area detector, flat panel X-ray detector, 200 µm pixels, 40×40 cm2 pachishandiswa nguva yekuratidzwa kwe 0.3 s uye 120 frames.
Kuyerwa kweX-PEEM kwemamodheru maviri akasarudzwa kwakaitwa paBeamline MAXPEEM PEEM end station muMAX IV laboratory (Lund, Sweden). Masampuleti akagadzirwa nenzira imwecheteyo yekuyerwa kwemagetsi. Masampuleti akagadzirwa akachengetwa mumhepo kwemazuva akati wandei uye akabviswa mweya mukamuri revacuum rakakwirira kwazvo asati apiswa nemwaranzi ne synchrotron photons. Simba rekugadzirisa kwemutsara we beam rakawanikwa nekuyera ion yield spectrum munzvimbo ye excitation kubva kuN 1 s kusvika 1\(\pi _g^ \ast\) pedyo ne hv = 401 eV mu N2 nekuvimba kwesimba re photon pa E3/2 , 57. Approximation spectra yakapa ΔE (upamhi hwemutsara we spectral) hweinenge 0.3 eV muhuwandu hwesimba rakayerwa. Saka, resolution yesimba re beamline yakafungidzirwa kuva E/∆E = 700 eV/0.3 eV > 2000 uye flux ≈1012 ph/s nekushandisa modified SX-700 monochromator ine Si 1200-line mm−1 grating yeFe 2p L2,3 edge, Cr 2p L2,3 edge, Ni 2p L2,3 edge, uye Ce M4,5 edge. Saka, resolution yesimba re beamline yakafungidzirwa kuva E/∆E = 700 eV/0.3 eV > 2000 uye flux ≈1012 ph/s nekushandisa modified SX-700 monochromator ine Si 1200-line mm−1 grating yeFe 2p L2.3 edge, Cr 2p L2.3 edge, Ni 2p L2.3 edge, uye Ce M4.5 edge. Таким образом, энергетическое разрешение канала пучка было оценено как E/∆E = 700 эВ/0,3 эВ > 2000 и поток ≈1012 модифицированного монохроматора SX-700 с решеткой Si 1200 штрихов/мм для Fe кромка 2p L2,3, кромка Cr 2p L2,3, кромка Ni 2p L2, кромка Ni 2p L2, 3, кромка Ni 2p L2,3 Saka, simba rekugadzirisa remugero we beam rakafungidzirwa seE/∆E = 700 eV/0.3 eV > 2000 uye flux ≈1012 f/s uchishandisa modified SX-700 monochromator ine Si grating ye1200 lines/mm yeFe edge 2p L2 ,3, Cr edge 2p L2.3, Ni edge 2p L2.3, uye Ce edge M4.5.因此，光束线能量分辨率估计為E/ΔE = 700 eV/0.3 eV > 2000 和通量≈1012 ph/s,通过使用带有1Si 120mm光栅的改进的SX-700 单色器用于Fe 2p L2,3 边缘、Cr 2p L2,3 边缘、Ni 2p L2,3 边缘和Ce M4,5 边缘.因此 , 光束线 能量 分辨率 為 為 為 δe = 700 EV/0.3 EV> 2000 和 ≈1012 PH/S , 使用 带有 带有 10 × 12 mm .改进 的 SX-700 单色器 于 于 用 用 用 Fe 2p L2.3 边缘、Cr 2p L2.3 边缘、Ni 2p L2.3 边缘和Ce M4.Saka, kana uchishandisa modified SX-700 monochromator ine 1200 line Si grating. 3, Cr edge 2p L2.3, Ni edge 2p L2.3 uye Ce edge M4.5.Simba re photon rinoskenwa mumatanho e 0.2 eV. Pasimba rega rega, mifananidzo yePEEM yakarekodhwa uchishandisa fibre-coupled TVIPS F-216 CMOS detector ine 2 x 2 bin, iyo inopa resolution ye 1024 x 1024 pixels munzvimbo ye 20 µm yekuona. Nguva yekuratidzwa kwemifananidzo yaive 0.2 s, avhareji yemafuremu gumi nematanhatu. Simba remufananidzo we photoelectron rinosarudzwa nenzira yekupa chiratidzo chepamusoro che secondary electron. Kuyerwa kwese kwakaitwa panguva yakajairika uchishandisa linearly polarized photon beam. Ruzivo rwakawanda nezvekuyerwa runogona kuwanikwa muchidzidzo chakapfuura. Mushure mekudzidza total electron yield (TEY) detection mode uye kushandiswa kwayo mu X-PEEM49, kudzika kwekuyedzwa kwenzira iyi kunofungidzirwa kuva 4-5 nm yechiratidzo che Cr uye 6 nm ye Fe. Kudzika kwe Cr kuri pedyo zvikuru nekukora kwe oxide film (~4 nm)60,61 nepo kudzika kwe Fe kuri kukuru kupfuura ukobvu. XRD inounganidzwa pamucheto weFe L isanganiswa yeXRD yema iron oxides neFe0 kubva mu matrix. Muchiitiko chekutanga, simba rema electron anoburitswa rinobva kumarudzi ese ema electron anogoneka anobatsira kuTEY. Zvisinei, chiratidzo chesimbi chakachena chinoda simba re kinetic rakawanda kuti ma electron apfuure nepakati pe oxide layer kuenda pamusoro uye aunganidzwe ne analyzer. Muchiitiko ichi, chiratidzo cheFe0 chinonyanya kukonzerwa nema electron eLVV Auger, pamwe nema electron echipiri anoburitswa nawo. Pamusoro pezvo, simba reTEY rinopihwa nema electron aya rinoora panguva yekubuda kwema electron, zvichideredza zvakanyanya mhinduro yeFe0 spectral mu iron XAS map.
Kubatanidza data mu data cube (data reX-PEEM) idanho guru mukutsvaga ruzivo rwakakodzera (makemikari kana physical properties) nenzira ine mativi akawanda. K-means clustering inoshandiswa zvakanyanya munzvimbo dzakasiyana siyana, kusanganisira machine vision, image processing, unsupervised pattern recognition, artificial intelligence, uye classificatory analysis. Semuenzaniso, K-means clustering yakashanda zvakanaka mu clustering hyperspectral image data. Panyaya iyi, kune multi-feature data, K-means algorithm inogona kuvaisa mumapoka zviri nyore zvichienderana neruzivo nezvehunhu hwavo (photon energy properties). K-means clustering i iterative algorithm yekuparadzanisa data mumapoka eK asingapindirani (clusters), uko pixel yega yega iri yeboka rakati zvichienderana nekugoverwa kwe spatial kwe chemical inhomogeneity mu microstructural composition yesimbi. K-means algorithm inosanganisira matanho maviri: mudanho rekutanga, K centroids dzinoverengerwa, uye mudanho rechipiri, poindi yega yega inopihwa cluster ine centroids dziri pedyo. Pakati pegiravhiti yeboka (centre of gravity) panotsanangurwa se arithmetic mean yedata points (XAS spectrum) yeboka iroro. Kune madaro akasiyana-siyana ekutsanangura macentroid ari pedyo seEuclidean distance. Pamufananidzo wekuisa px,y (apo x na y vari resolution muma pixels), CK ndiyo pakati pegiravhiti yeboka; mufananidzo uyu unogona kupatsanurwa (kuiswa mu cluster) kuita ma cluster eK uchishandisa K-means63. Matanho ekupedzisira eK-means clustering algorithm ndeaya:
Danho rechipiri. Verenga huwandu hwemapikiseli ese zvichienderana ne centroid iripo. Semuenzaniso, inoverengerwa kubva padhara reEuclidean d pakati pepakati ne pixel yega yega:
Danho rechitatu: Isa pixel yega yega ku centroid iri pedyo. Wobva waverengazve nzvimbo dzeK centroid seizvi:
Danho rechina. Dzokorora maitiro aya (equations (7) uye (8)) kusvika macentroid asangana. Mhedzisiro yekupedzisira yemhando ye clustering inoenderana zvakanyanya nesarudzo yakanakisa yemacentroid ekutanga. Kune chimiro chedata rePEEM chemifananidzo yesimbi, kazhinji X (x × y × λ) icube yedata re3D array, nepo ma x ne y axes achimiririra ruzivo rwenzvimbo (pixel resolution) uye λ axis inoenderana nemufananidzo we photon. energy spectral. Iyo K-means algorithm inoshandiswa kuongorora nzvimbo dzinofarira mu data re X-PEEM nekuparadzanisa ma pixel (ma clusters kana ma sub-blocks) zvichienderana ne spectral features avo uye kubvisa ma centroid akanakisa (XAS spectral profiles) ye analyte. cluster yega yega). Inoshandiswa kudzidza spatial distribution, local spectral changes, oxidation behavior, uye chemical states. Semuenzaniso, K-means clustering algorithm yakashandiswa kune Fe L-edge neCr L-edge regions mu hot-worked ne cold-rolled X-PEEM. Nhamba dzakasiyana-siyana dzemaboka eK (nzvimbo dze microstructure) dzakaedzwa kuti paonekwe maboka akakodzera uye macentroid. Kana nhamba idzi dzaratidzwa, mapixel anoendeswa kune macentroid eboka anoenderana. Kugoverwa kwemavara ega ega kunoenderana nepakati peboka, zvichiratidza kurongeka kwenzvimbo kwezvinhu zvemakemikari kana zvepanyama. Macentroid akabviswa isanganiswa yakatsetseka yemaspectra akachena.
Ruzivo runotsigira mhedzisiro yechidzidzo ichi runowanikwa kana paine chikonzero chakanaka chekukumbirwa kubva kumunyori weWC.
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