Bayyana Tasirin Nanoscale Chemical Inhomogeneity akan Lalacewar Cerium-Modified 2507 Super Duplex Bakin Karfe

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Bakin karfe da aka yi amfani da shi da yawa da nau'ikansa da aka yi suna da juriya ga lalatawa a cikin yanayi na yanayi saboda ramin wucewa da ke kunshe da chromium oxide.Lalacewa da yashewar ƙarfe a al'adance suna da alaƙa da lalata waɗannan yadudduka, amma da wuya a matakin ƙananan ƙananan, ya danganta da asalin rashin daidaituwa na saman.A cikin wannan aikin, nau'in nau'in nau'in sinadarai na nanoscale wanda aka gano ta spectroscopic microscopy da bincike na chemometric ba zato ba tsammani ya mamaye bazuwar da lalatawar cerium mai sanyi wanda aka gyara super duplex bakin karfe 2507 (SDSS) yayin yanayin lalacewarsa mai zafi.wani bangaren.Ko da yake X-ray photoelectron microscopy ya nuna in mun gwada da uniform ɗaukar hoto na halitta Cr2O3 Layer, sanyi birgima SDSS nuna matalauta passivation sakamakon saboda a gida rarraba Fe3+ arziki nanoislands a kan Fe/Cr oxide Layer.Wannan ilimin a matakin atom ɗin yana ba da zurfin fahimta game da lalata bakin karfe kuma ana tsammanin zai taimaka wajen yaƙi da lalata nau'ikan ƙarfe masu ƙarfi iri ɗaya.
Tun da aka ƙirƙira bakin ƙarfe, juriya na lalata na ferrochromium gami an danganta shi da chromium, wanda ke samar da oxide mai ƙarfi / oxyhydroxide mai ƙarfi wanda ke nuna halayen wucewa a yawancin mahalli.Idan aka kwatanta da na al'ada (austenitic da ferritic) bakin karfe, super duplex bakin karfe (SDSS) tare da mafi lalata juriya suna da m inji Properties1,2,3.Ƙarfafa ƙarfin injina yana ba da izinin ƙira mai sauƙi da ƙarami.Sabanin haka, SDSS na tattalin arziki yana da babban juriya ga ramuka da lalata, wanda ke haifar da tsawon rayuwar sabis da faffadan aikace-aikace a cikin sarrafa gurɓata, kwantena sinadarai, da masana'antar mai da iskar gas4.Duk da haka, kunkuntar kewayon zafi magani yanayin zafi da rashin tsari tsari hana ta fadi da m aikace-aikace.Saboda haka, an gyara SDSS don inganta abubuwan da ke sama.Misali, an gabatar da gyare-gyaren Ce da ƙarin ƙarin N 6, 7, 8 a cikin 2507 SSS (Ce-2507).Matsayin da ya dace na 0.08 wt.% ƙarancin ƙasa (Ce) yana da tasiri mai fa'ida akan kaddarorin injinan DSS, yayin da yake haɓaka haɓakar hatsi da ƙarfin iyakar hatsi.Juriya da sawa da lalata, ƙarfin juriya da ƙarfin samarwa, da aiki mai zafi kuma an inganta su9.Yawancin nitrogen na iya maye gurbin abubuwan da ke cikin nickel masu tsada, yana sa SDSS ya fi tasiri-tasiri10.
Kwanan nan, SDSS ya zama nakasar filastik a yanayin zafi daban-daban (ƙananan zafin jiki, sanyi da zafi) don cimma kyawawan kaddarorin inji6,7,8.Duk da haka, kyakkyawan juriya na lalatawar SDSS shine saboda kasancewar fim ɗin oxide na bakin ciki a saman, wanda ke shafar abubuwa da yawa, irin su kasancewar matakai masu yawa tare da iyakokin hatsi daban-daban, abubuwan da ba a so da kuma halayen daban-daban.na ciki inhomogeneous microstructure na daban-daban austenitic da ferritic matakai an lalace 7 .Sabili da haka, nazarin abubuwan microdomain na irin waɗannan fina-finai a matakin tsarin lantarki yana da mahimmancin mahimmanci don fahimtar lalata SDSS kuma yana buƙatar dabarun gwaji masu rikitarwa.Har ya zuwa yanzu, hanyoyin da ke da hankali kamar su Auger electron spectroscopy11 da X-ray photoelectron spectroscopy12,13,14,15 da kuma tsarin photoelectron photoelectron X-ray mai wuya ya bambanta, amma sau da yawa ya kasa rabuwa, jihohin sinadarai iri ɗaya a wurare daban-daban a sararin samaniya akan nanoscale.Yawancin binciken da aka yi kwanan nan sun haɗu da iskar shaka na gida na chromium zuwa halayen lalata na 17 austenitic bakin karfe, 18 martensitic bakin karfe, da SDSS 19, 20. Duk da haka, waɗannan karatun sun fi mayar da hankali kan tasirin Cr heterogeneity (misali, Cr3 + jihar hadawan abu da iskar shaka) akan juriya na lalata.Bambance-bambancen yanayi a cikin jahohin oxidation na abubuwa na iya haifar da su ta hanyar mahadi daban-daban masu abubuwa iri ɗaya, kamar baƙin ƙarfe oxides.Wadannan mahadi suna gadon ƙaramin girman da aka sarrafa ta thermomechanically kusa da juna, amma sun bambanta a cikin abun da ke ciki da yanayin oxidation16,21.Sabili da haka, bayyana lalata fina-finai na oxide sannan kuma pitting yana buƙatar fahimtar rashin daidaituwa na surface a matakin ƙananan ƙananan.Duk da waɗannan buƙatun, ƙididdigar ƙima kamar nau'in iskar oxygenation na gefe, musamman na baƙin ƙarfe akan sikelin nano/atomic, har yanzu ba a gano su ba kuma ba a gano mahimmancin su ga juriyar lalata ba.Har zuwa kwanan nan, yanayin sinadarai na abubuwa daban-daban, irin su Fe da Ca, an kwatanta su da ƙima akan samfuran ƙarfe ta amfani da microscopy na X-ray mai laushi mai laushi (X-PEEM) a cikin nanoscale synchrotron radiation wurare.Haɗe tare da fasaha mai mahimmanci na X-ray absorption spectroscopy (XAS), X-PEEM yana ba da damar aunawa XAS tare da girman sararin samaniya da ƙwanƙwasa, samar da bayanan sinadarai game da abun da ke ciki da yanayin sinadarai tare da ƙudurin sararin samaniya har zuwa sikelin nanometer 23.Wannan kallon kallo na wurin ƙaddamarwa a ƙarƙashin na'urar hangen nesa yana sauƙaƙe gwaje-gwajen sinadarai na gida kuma yana iya nuna sauye-sauyen sinadarai a baya da ba a gano su ba a cikin Layer Fe.
Wannan binciken yana faɗaɗa fa'idodin PEEM don gano bambance-bambancen sinadarai a cikin nanoscale kuma yana gabatar da hanyar bincike mai zurfi-matakin sararin samaniya don fahimtar halayen lalata na Ce-2507.Yana amfani da K-ma'anar cluster chemometric data24 don taswirar sinadarai na duniya (heterogeneity) na abubuwan da ke ciki, tare da jihohin sinadarai da aka gabatar a cikin wakilcin ƙididdiga.Ba kamar lalatawar al'ada da lalacewar fim ɗin chromium oxide ke haifarwa ba, ƙarancin wucewar halin yanzu da ƙarancin juriya na lalata ana danganta su zuwa wuraren da ke cikin yankin Fe3+ mai arzikin nanoislands kusa da Layer Fe/Cr oxide, wanda zai iya zama hari ta hanyar oxide mai karewa.Yana samar da fim a wurin kuma yana haifar da lalata.
An fara kimanta halayen lalata na SDSS 2507 ta hanyar amfani da ma'aunin lantarki.A kan fig.Hoto 1 yana nuna Nyquist da Bode curves don zaɓaɓɓun samfurori a cikin acidic (pH = 1) mafita mai ruwa na FeCl3 a dakin da zafin jiki.Electrolyte da aka zaɓa yana aiki azaman wakili mai ƙarfi mai ƙarfi, yana nuna halayen fim ɗin wucewa don rushewa.Ko da yake kayan ba su sami kwanciyar hankali da zafin jiki ba, waɗannan nazarin sun ba da haske game da yuwuwar aukuwar gazawa da hanyoyin lalata.An yi amfani da ma'auni daidai (Fig. 1d) don dacewa da nau'in nau'i na electrochemical impedance spectroscopy (EIS), kuma an nuna sakamakon da ya dace a cikin Table 1. Ƙirar da ba ta cika ba ta bayyana lokacin da aka gwada maganin da aka bi da kuma samfurori masu zafi masu zafi, yayin da madaidaicin da'irori masu dacewa sun kasance sanyi (Fig. 1b).A cikin bakan EIS, za a iya la'akari da radius na semicircle azaman juriya na polarization (Rp) 25,26.Rp na bayani da aka bi da SDSS a cikin Tebur 1 yana kusan 135 kΩ cm-2, duk da haka don aiki mai zafi da sanyi mai birgima SDSS muna iya ganin ƙimar ƙananan ƙimar 34.7 da 2.1 kΩ cm-2 bi da bi.Wannan gagarumin raguwa a cikin Rp yana nuna mummunan tasirin nakasar filastik akan wucewa da juriya na lalata, kamar yadda aka nuna a cikin rahotannin da suka gabata 27, 28, 29, 30.
a Nyquist, b, c Bode impedance da zane-zane na zamani, da kuma daidaitaccen samfurin kewaye don d, inda RS shine juriya na electrolyte, Rp shine juriya na polarization, kuma QCPE shine madaidaicin kashi kashi oxide da ake amfani da shi don yin samfurin da ba daidai ba capacitance (n) .An gudanar da ma'aunin EIS ba tare da yuwuwar ɗaukar nauyi ba.
Ana nuna madaidaitan oda na farko a cikin zanen Bode kuma babban mitar plateau yana wakiltar juriyar electrolyte RS26.Yayin da mitar ke raguwa, impedance yana ƙaruwa kuma an sami kusurwa mara kyau, yana nuna rinjayen ƙarfin aiki.Matsakaicin lokaci yana ƙaruwa, yana riƙe da ƙimarsa mafi girma a cikin kewayon mitar mitoci kaɗan, sannan ya ragu (Fig. 1c).Duk da haka, a cikin dukkan lokuta uku wannan matsakaicin ƙimar har yanzu bai wuce 90 ° ba, yana nuna halin da bai dace ba saboda tarwatsawar capacitive.Saboda haka, da QCPE m lokaci kashi (CPE) da ake amfani da su wakilci interfacial capacitance rarraba samu daga surface roughness ko inhomogeneity, musamman cikin sharuddan atomic sikelin, fractal lissafi, electrode porosity, wadanda ba Uniform m, da kuma surface dogara halin yanzu rarraba.Geometry na Electrode31,32.CPE impedance:
inda j shine lambar hasashe kuma ω shine mitar angular.QCPE mitar ce mai zaman kanta ta yau da kullun daidai gwargwado ga wurin buɗewa mai aiki na electrolyte.n lambar wutar lantarki ce marar girma wacce ke bayyana karkacewa daga madaidaicin halayen capacitive na capacitor, watau kusa da n shine 1, mafi kusancin CPE shine mafi girman capacitance, kuma idan n yana kusa da sifili, juriya ce.Ƙananan karkata na n, kusa da 1, yana nuna rashin ingantacciyar halayya mai ƙarfi ta saman bayan gwajin polarization.QCPE na SDSS mai sanyi yana da girma fiye da samfuran kamanni, wanda ke nufin cewa ingancin saman ba shi da daidaituwa.
Daidaita da mafi yawan kaddarorin juriyar lalata na bakin karafa, babban abun ciki na Cr na SDSS gabaɗaya yana haifar da ingantaccen juriyar lalatawar SDSS saboda kasancewar fim ɗin kariya mai ƙarfi a saman17.Wannan fim mai wucewa yawanci yana da wadata a Cr3+ oxides da / ko hydroxides, galibi yana haɗa Fe2+, Fe3+ oxides da / ko (oxy) hydroxides 33 .Duk da wannan surface uniformity, passivating oxide Layer, kuma babu bayyane lalacewa a kan surface, kamar yadda ƙaddara ta microscopic images, 6,7 da lalata hali na zafi-aiki da sanyi-birgima SDSS ne daban-daban sabili da haka na bukatar zurfafa nazarin nakasu microstructure da kuma tsarin halayyar karfe.
An bincika ƙananan ƙananan ƙarfe na gurɓataccen ƙarfe ta ƙididdigewa ta amfani da hasken X-ray mai ƙarfi na ciki da synchrotron (Ƙarin Figures 1, 2).Ana ba da cikakken bincike a cikin Ƙarin Bayani.Ko da yake sun fi dacewa da nau'in babban lokaci, ana samun bambance-bambance a cikin juzu'in juzu'in juzu'i, waɗanda aka jera a cikin Ƙarin Teburin 1. Waɗannan bambance-bambancen ana iya haɗa su da ɓangarorin lokaci marasa daidaituwa a saman, da kuma ɓangarorin juzu'i da aka yi a zurfafa daban-daban.ganowa ta hanyar rarrabawar X-ray.(XRD) tare da hanyoyin makamashi daban-daban na abubuwan da suka faru na photons.Matsakaicin mafi girman adadin austenite a cikin samfuran birgima mai sanyi, wanda XRD ya ƙaddara daga tushen dakin gwaje-gwaje, yana nuna mafi kyawun wucewa da kuma mafi kyawun juriya na lalata35, yayin da ƙarin daidaitattun sakamako da ƙididdiga ke nuna sabanin yanayi a cikin ma'auni na lokaci.Bugu da ƙari, juriya na lalata na karfe kuma ya dogara da matakin gyaran ƙwayar hatsi, rage girman ƙwayar hatsi, karuwa a cikin microdeformations da raguwa da yawa da ke faruwa a lokacin jiyya na thermomechanical36,37,38.Abubuwan da ake yi na zafi suna nuna yanayin nau'in hatsi, yayin da aka lura da hatsi Micron-Sized (karin bayani.samuwar da karuwa na lalata juriya.Maɗaukakin ɓarna yawanci yana haɗuwa da ƙananan juriya ga rami, wanda ya yarda da ma'aunin lantarki.
Canje-canje a cikin jihohin sinadarai na microdomains na abubuwan firamare an yi nazarin su cikin tsari ta amfani da X-PEEM.Duk da ɗimbin abubuwan haɗakarwa, an zaɓi Cr, Fe, Ni da Ce39 a nan, tunda Cr shine maɓalli mai mahimmanci don samar da fim ɗin wucewa, Fe shine babban kashi a cikin ƙarfe, kuma Ni yana haɓaka haɓakawa da daidaita tsarin lokaci na ferrite-austenitic da manufar gyara Ce.Ta hanyar daidaita makamashi na radiation synchrotron, RAS an rufe shi daga saman tare da manyan siffofi na Cr (gefen L2.3), Fe (gefen L2.3), Ni (gefen L2.3) da Ce (gefen M4.5).zafi forming da sanyi mirgina Ce-2507 SDSS.An yi nazarin bayanan da suka dace ta hanyar haɗa daidaitawar makamashi tare da bayanan da aka buga (misali XAS 40, 41 akan Fe L2, gefuna 3).
A kan fig.Hoto na 2 yana nuna hotunan X-PEEM na aiki mai zafi (Fig. 2a) da sanyi-birgima (Fig. 2d) Ce-2507 SDSS da kuma daidaitattun XAS gefuna na Cr da Fe L2,3 a wurare masu alama.Gefen L2,3 na XAS yana bincikar jihohin 3d da ba a cika su ba bayan photoexcitation na lantarki a matakan rarraba-orbit 2p3/2 (L3 gefen) da 2p1/2 (L2 gefen).An samo bayani game da yanayin valence na Cr daga XAS a gefen L2,3 a cikin siffa 2b, e.Kwatanta da alkalai.42,43 ya nuna cewa an lura da kololuwa huɗu kusa da gefen L3, mai suna A (578.3 eV), B (579.5 eV), C (580.4 eV) da D (582.2 eV), yana nuna octahedral Cr3 +, daidai da ion Cr2O3.Siffofin gwaji sun yarda da ƙididdigar ƙididdiga waɗanda aka nuna a cikin bangarori b da e, waɗanda aka samo daga ƙididdige ƙididdiga masu yawa na filin crystal a Cr L2.3 interface ta amfani da filin crystal na 2.0 eV44.Dukansu saman na SDSS masu zafi da masu sanyi ana lulluɓe su da wani ƙaramin nau'in nau'in Cr2O3.
Hoton thermal na X-PEEM na nakasasshen SDSS na thermally daidai da b Cr L2.3 gefen da c Fe L2.3 gefen, d X-PEEM thermal image na sanyi birgima SDSS daidai da e Cr L2.3 gefen da f Fe L2 .3 gefen gefen (f).An ƙirƙira siginar XAS a wurare daban-daban waɗanda aka yiwa alama akan hotuna masu zafi (a, d), layukan masu dige orange a cikin (b) da (e) suna wakiltar simintin XAS na Cr3+ tare da ƙimar filin crystal na 2.0 eV.Don hotunan X-PEEM, yi amfani da palette na thermal don haɓaka iya karanta hoto, inda launuka daga shuɗi zuwa ja suka yi daidai da ƙarfin ɗaukar X-ray (daga ƙasa zuwa babba).
Ko da kuwa yanayin sinadarai na waɗannan ƙarfe na ƙarfe, yanayin sinadarai na abubuwan haɓaka Ni da Ce ga samfuran duka biyun bai canza ba.Ƙarin zane.Figures 5-9 suna nuna hotunan X-PEEM da madaidaicin sifofin XAS na Ni da Ce a wurare daban-daban a saman kayan aikin zafi da sanyi.Ni XAS yana nuna jahohin oxidation na Ni2+ a kan dukkan ma'aunin da aka auna na samfuran zafi da aka yi birgima (Ƙarin Tattaunawa).Ya kamata a lura cewa, a cikin yanayin samfurori masu zafi, ba a lura da siginar XAS na Ce ba, yayin da a cikin yanayin sanyi mai sanyi, an lura da nau'in Ce3 +.Duban alamun Ce a cikin samfuran sanyi-birgima ya nuna cewa Ce galibi yana bayyana a cikin sigar hazo.
A cikin SDSS nakasar thermally, babu wani canji na gida a cikin XAS a gefen Fe L2,3 (Fig. 2c).Koyaya, ƙaramin yanki na Fe matrix yana canza yanayin sinadarai a wurare bakwai da aka zaɓa na SDSS mai sanyi, kamar yadda aka nuna a hoto 2f.Bugu da ƙari, don samun cikakken ra'ayi game da canje-canje a cikin jihar Fe a wuraren da aka zaɓa a cikin siffa 2f, an gudanar da nazarin sararin samaniya (Fig. 3 da Ƙarin Fig. 10) inda aka zaɓi ƙananan yankuna masu madauwari.Siffar XAS na Fe L2,3 gefen α-Fe2O3 tsarin da Fe2+ octahedral oxides an tsara su ta hanyar lissafin filin kristal da yawa ta amfani da filayen crystal na 1.0 (Fe2 +) da 1.0 (Fe3 +)44. Mun lura cewa α-Fe2O3 da γ-Fe2O3 suna da alamomin gida daban-daban45,46, Fe3O4 yana haɗuwa da duka Fe2 + & Fe3 +, 47, da FeO45 a matsayin Fe2+ oxide na yau da kullun (3d6). Mun lura cewa α-Fe2O3 da γ-Fe2O3 suna da alamomin gida daban-daban45,46, Fe3O4 yana da haɗuwa da duka Fe2 + & Fe3 +,47, da FeO45 a matsayin Fe2+ oxide na yau da kullun (3d6).Lura cewa α-Fe2O3 da γ-Fe2O3 suna da alamomin gida daban-daban45,46, Fe3O4 ya haɗu da Fe2 + da Fe3 +,47 da FeO45 a cikin nau'i na divalent oxide Fe2+ (3d6).Lura cewa α-Fe2O3 da γ-Fe2O3 suna da alamomin gida daban-daban45,46, Fe3O4 yana da haɗin Fe2 + da Fe3 +,47 da FeO45 suna aiki azaman divalent Fe2+ oxide (3d6).Duk Fe3+ ions a cikin α-Fe2O3 suna da matsayi Oh kawai, yayin da γ-Fe2O3 yawanci ana wakilta ta Fe3+ t2g [Fe3+5/3V1/3] misali O4 spinel tare da guraben aiki a misali matsayi.Saboda haka, Fe3+ ions a cikin γ-Fe2O3 suna da duka Td da Oh matsayi.Kamar yadda aka ambata a cikin takarda da ta gabata, 45 ko da yake girman girman su biyun ya bambanta, girman girman su misali / t2g shine ≈1, yayin da a cikin wannan yanayin yanayin ƙarfin da aka lura misali / t2g yana kusan 1. Wannan ya cire yiwuwar cewa a halin da ake ciki kawai Fe3 + ne kawai.Yin la'akari da yanayin Fe3O4 tare da Fe2 + da Fe3 +, fasalin farko da aka sani yana da rauni (ƙarfi) L3 gefen Fe yana nuna ƙarami (mafi girma) jihar t2g.Wannan ya shafi Fe2+ (Fe3+), wanda ke nuna cewa fasalin farko na karuwa yana nuna karuwa a cikin Fe2+47.Waɗannan sakamakon sun nuna cewa zaman tare na Fe2+ da γ-Fe2O3, α-Fe2O3 da/ko Fe3O4 sun mamaye saman da aka yi sanyi na abubuwan da aka haɗa.
Girman hotunan hoto na thermal na hoto na XAS Spectra (a, c) da (b, d) ketare gefen Fe L2,3 a wurare daban-daban na sararin samaniya a cikin zaɓaɓɓun yankuna 2 da E a cikin Figs.2d.
Bayanan gwaji da aka samo (Fig. 4A da ƙarin Fig. 11) An kwatanta da kuma idan aka lura da bayanan masu tsabta 40, 48, Xas-2 da Xas-3: Fig. 4A).Musamman ma, bakan 2-a (wanda aka nuna a matsayin XAS-1) a cikin siffa 3b wanda ya biyo baya 2-b (labeled XAS-2) an lura da shi a kan dukan yankin ganowa, yayin da aka lura da nau'i-nau'i kamar E-3 a cikin adadi na 3d (labeled XAS-3) a wasu wurare.A matsayinka na mai mulki, an yi amfani da sigogi guda hudu don gano jihohin da ke cikin valence a cikin samfurin da aka yi nazari: (1) halayen yanayi L3 da L2, (2) matsayi na makamashi na halayen L3 da L2, (3) bambancin makamashi L3-L2., ( 4) L2/L3 girman rabo.Dangane da abubuwan gani na gani (Fig. 4a), dukkanin abubuwan da aka gyara guda uku na Fe, wato, Fe0, Fe2+, da Fe3+, suna nan akan saman SDSS da ake nazari.Ƙididdigar ƙarfin ƙididdigewa L2/L3 kuma ya nuna kasancewar dukkan abubuwa uku.
a Simulated XAS spectra na Fe tare da lura da uku daban-daban na gwaji data (m Lines XAS-1, XAS-2 da XAS-3 daidai da 2-a, 2-b da E-3 a cikin siffa 2 da 3) Kwatanta , Octahedrons Fe2 +, Fe3 + tare da crystal filin darajar 1.0 eV, da kuma mutunta data XAS-1. , XAS-3) da kuma daidaitattun bayanan LCF (layin baki mai ƙarfi), da kuma a cikin nau'i na XAS-3 spectra tare da Fe3O4 (jihar gauraye na Fe) da Fe2O3 (tsarki Fe3 +).
An yi amfani da haɗin kai tsaye (LCF) na ma'auni uku na 40, 41, 48 don ƙididdige abun da ke ciki na baƙin ƙarfe oxide.An aiwatar da LCF don zaɓaɓɓun nau'ikan nau'ikan Fe L-gefen XAS guda uku waɗanda ke nuna bambanci mafi girma, wato XAS-1, XAS-2 da XAS-3, kamar yadda aka nuna a cikin siffa 4b-d.Don kayan aiki na LCF, 10% Fe0 an yi la'akari da shi a duk lokuta saboda gaskiyar cewa mun lura da ƙaramin leji a cikin duk bayanan, kuma saboda gaskiyar cewa ƙarfe na ƙarfe shine babban ɓangaren ƙarfe. Lallai, zurfin gwaji na X-PEEM don Fe (~ 6 nm) 49 ya fi girma fiye da kauri da aka kiyasta oxidation Layer (dan kadan> 4 nm), yana ba da damar gano sigina daga matrix baƙin ƙarfe (Fe0) a ƙarƙashin Layer passivation. Lallai, zurfin gwaji na X-PEEM don Fe (~ 6 nm) 49 ya fi girma fiye da kauri da aka kiyasta oxidation Layer (dan kadan> 4 nm), yana ba da damar gano sigina daga matrix baƙin ƙarfe (Fe0) a ƙarƙashin Layer passivation. Действительно, пробная глубина X-PEEM для Fe (~ 6 нм ) оляет обнаружить сигнал от железной матрицы (Fe0) под пассивирующим слоем. Lallai, zurfin binciken X-PEEM na Fe (~ 6 nm) 49 ya fi girman da aka ɗauka na kauri na oxidation Layer (dan kadan> 4 nm), wanda ya sa ya yiwu a gano siginar daga matrix baƙin ƙarfe (Fe0) a ƙarƙashin Layer passivation.事实上,X-PEEM 对Fe(~6 nm)49方的铁基体(Fe0)的信号。事实上 , X-PEEM 对 Fe (~ 6 nm) 49 的 检测 深度 大于层 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 м), что позволяет обнаруживать сигнал от железной матрицы (Fe0) ниже пассивирующего слоя. A gaskiya ma, zurfin ganewar Fe (~ 6 nm) 49 ta X-PEEM ya fi girma fiye da kauri da ake tsammani na Layer oxide (dan kadan> 4 nm), wanda ke ba da damar gano siginar daga matrix na ƙarfe (Fe0) a ƙasa da Layer passivation. .An yi haɗe-haɗe daban-daban na Fe2+ da Fe3+ don nemo mafi kyawun mafita ga bayanan gwaji da aka lura.A kan fig.4b yana nuna bakan XAS-1 don haɗin Fe2+ da Fe3+, inda rabon Fe2+ da Fe3+ ya kasance kama da kusan 45%, yana nuna yanayin yanayin iskar shaka na Fe.Yayin da XAS-2 bakan, yawan Fe2+ da Fe3+ ya zama ~ 30% da 60%, bi da bi.Fe2+ ​​bai kai Fe3+ ba.Matsakaicin Fe2+ zuwa Fe3, daidai yake da 1:2, yana nufin cewa Fe3O4 za a iya samu a daidai wannan rabo tsakanin Fe ions.Bugu da ƙari, don bakan XAS-3, yawan Fe2 + da Fe3 + ya zama ~ 10% da 80%, wanda ke nuna babban juyi na Fe2 + zuwa Fe3 +.Kamar yadda aka ambata a sama, Fe3+ na iya zuwa daga α-Fe2O3, γ-Fe2O3 ko Fe3O4.Don fahimtar tushen da ya fi dacewa na Fe3 +, an tsara tsarin XAS-3 tare da ma'auni na Fe3 + daban-daban a cikin Hoto 4e, yana nuna kamance tare da ma'auni guda biyu lokacin la'akari da girman B.Koyaya, ƙarfin kololuwar kafada (A: daga Fe2+) da ƙimar ƙarfin B/A suna nuna cewa bakan XAS-3 yana kusa, amma bai dace da bakan γ-Fe2O3 ba.Idan aka kwatanta da girma γ-Fe2O3, Fe 2p XAS kololuwar A SDSS yana da ɗan ƙaramin ƙarfi (Fig. 4e), wanda ke nuna babban ƙarfin Fe2+.Kodayake bakan XAS-3 yayi kama da na γ-Fe2O3, inda Fe3 + ke kasancewa a matsayi na Oh da Td, gano nau'ikan jihohin valence daban-daban da daidaitawa kawai tare da gefen L2,3 ko girman girman L2 / L3 ya kasance batun ci gaba da bincike.tattaunawa saboda sarkar abubuwa daban-daban wadanda suka shafi bakan karshe41.
Baya ga bambance-bambancen ban mamaki a cikin yanayin sinadarai na yankunan da aka zaɓa na sha'awar da aka bayyana a sama, an kuma tantance nau'ikan sinadarai na duniya na mahimman abubuwan Cr da Fe ta hanyar rarraba duk sifofin XAS da aka samu akan saman samfurin ta amfani da hanyar tari na K-ma'ana.Bayanan bayanan martaba na Cr L sun samar da ingantattun gungu guda biyu da aka rarraba a sararin samaniya a cikin aikin da aka yi zafi da sanyi wanda aka nuna a cikin Figs.5. A bayyane yake cewa babu wani canje-canjen tsarin gida da aka tsinkayi makamancin haka, tunda centroids guda biyu na XAS Cr spectra suna kama da juna.Waɗannan sifofi na gungu biyu sun kusan kama da waɗanda suka yi daidai da Cr2O342, wanda ke nufin cewa yadudduka na Cr2O3 sun yi daidai da sarari akan SDSS.
Cr L K-yana nufin gungu na yanki, kuma b shine madaidaicin XAS centroids.Sakamakon K-yana nufin X-PEEM kwatankwacin SDSS mai sanyi: c Cr L2.3 yankin gefen K- yana nufin tari da d madaidaitan XAS centroids.
Don misalta ƙarin taswirorin gefen gefen FeL, ingantattun tari huɗu da biyar da kuma abubuwan da suka shafi centroids (bayanin bayanan martaba) an yi amfani da su don samfurori masu zafi da birgima, bi da bi.Saboda haka, ana iya samun kashi (%) na Fe2 + da Fe3 + ta hanyar dacewa da LCF da aka nuna a cikin Fig.4.An yi amfani da pseudoelectrode yuwuwar Epseudo azaman aikin Fe0 don bayyana rashin daidaituwar microchemical na fim ɗin oxide.Epseudo an kimanta shi ta hanyar ka'idar hadawa,
inda \(\rm{E}_{\rm{Fe}/\rm{Fe}^{2 + (3 + )}}\) yayi daidai da \(\rm{Fe} + 2e^ - \ zuwa \rm {Fe}^{2 + (3 + )}\), 0.440 da 0.036 V, bi da bi.Yankunan da ke da ƙananan yuwuwar suna da babban abun ciki na fili na Fe3+.Rarraba mai yuwuwar rarrabawa a cikin samfuran da aka lalatar da su yana da hali mai laushi tare da matsakaicin canji na kusan 0.119 V (Fig. 6a, b).Wannan yuwuwar rarrabawa yana da alaƙa da alaƙa da yanayin ƙasa (Fig. 6a).Babu wasu canje-canje masu dogara da matsayi a cikin laminar da ke cikin ciki da aka lura (Fig. 6b).Akasin haka, don haɗin oxides masu banƙyama tare da abun ciki daban-daban na Fe2 + da Fe3 + a cikin SDSS mai sanyi, wanda zai iya lura da yanayin rashin daidaituwa na pseudopotential (Fig. 6c, d).Fe3+ oxides da/ko (oxy)hydroxides sune manyan abubuwan da ke tattare da tsatsa a cikin karfe kuma suna iya shiga cikin iskar oxygen da ruwa50.A wannan yanayin, tsibiran da ke da arzikin Fe3 + ana ɗaukar su ana rarraba su a cikin gida kuma ana iya ɗaukar su azaman gurɓatattun wurare.A lokaci guda, gradient a cikin yuwuwar filin, maimakon madaidaicin ƙimar yuwuwar, ana iya amfani da shi azaman mai nuni don gano wuraren lalata masu aiki.Wannan m rarraba Fe2 + da Fe3 + a saman sanyi birgima SDSS iya canza gida sunadarai da kuma samar da wani karin m aiki surface yanki a lokacin oxide film rushewa da kuma lalata halayen, kyale matrix karfe matrix ya ci gaba da lalata, haifar da ciki iri-iri.Properties da rage m Properties na passivating Layer.
K-yana nufin gungu da madaidaitan XAS centroids a cikin yankin Fe L2.3 na gefen X-PEEM ac mai zafi mai zafi da df na SDSS mai sanyi.a, d K-yana nufin gungun makircin da aka lullube akan hotunan X-PEEM.An ambaci yuwuwar pseudoelectrode da aka ƙididdige (Epseudo) tare da makircin gungu na K-ma'ana.Hasken hoton X-PEEM, kamar launi a cikin siffa 2 daidai yake da ƙarfin ɗaukar X-ray.
Ingantacciyar hanyar Cr amma yanayin sinadarai daban-daban na Fe yana haifar da lalacewar fim ɗin oxide daban-daban da tsarin lalata a cikin aikin zafi da sanyi mai birgima Ce-2507.An yi nazarin wannan kadara ta C-2507 mai sanyi sosai.Game da samuwar oxides da hydroxides na Fe a cikin iska na yanayi a cikin wannan kusan aikin tsaka tsaki, halayen sune kamar haka:
Abubuwan da ke sama suna faruwa a cikin yanayi masu zuwa bisa nazarin X-PEEM.Ƙaramar kafada mai dacewa da Fe0 tana da alaƙa da ƙarfe na ƙarfe.Halin Fe na ƙarfe tare da yanayin yana haifar da samuwar Fe(OH) 2 Layer (equation (5)), wanda ke haɓaka siginar Fe2+ a cikin Fe L-gefen XAS.Tsawon tsawaitawa zuwa iska na iya haifar da samuwar Fe3O4 da/ko Fe2O3 oxides bayan Fe(OH)252,53.Siffofin barga guda biyu na Fe, Fe3O4 da Fe2O3, suma suna iya samuwa a cikin Cr3+ mai wadataccen kariya mai kariya, wanda Fe3O4 ya fi son tsarin uniform da m.Kasancewar duka sakamakon biyu a cikin jihohin hadawan abu da iskar shaka (XAS-1 bakan).Bakan XAS-2 yafi dacewa da Fe3O4.Yayin da kallon kallon XAS-3 a wurare da yawa ya nuna cikakkiyar juyi zuwa γ-Fe2O3.Tunda zurfin shigar da hasken X-ray ɗin da aka buɗe yana kusan 50 nm, siginar daga ƙaramin Layer yana haifar da mafi girman ƙarfi na kololuwar A.
Siffar XPA ta nuna cewa bangaren Fe a cikin fim ɗin oxide yana da tsarin da aka haɗa tare da Layer oxide Layer.Ya bambanta da alamun wucewa saboda rashin daidaituwa na gida na Cr2O3 a lokacin lalata, duk da nau'in nau'in nau'in Cr2O3 a cikin wannan aikin, ana lura da ƙananan juriya a cikin wannan yanayin, musamman ga samfurori masu sanyi.Halin da aka lura ana iya fahimtar shi azaman nau'in nau'in sinadarai na oxidation a cikin babban Layer (Fe), wanda ke shafar aikin lalata.Saboda wannan stoichiometry na babba Layer (baƙin ƙarfe oxide) da ƙananan Layer (chromium oxide) 52,53 mafi kyawun hulɗar (mannewa) a tsakanin su yana haifar da jinkirin sufuri na karfe ko ions oxygen a cikin lattice, wanda, bi da bi, yana haifar da karuwa a cikin juriya na lalata.Saboda haka, ci gaba da stoichiometric rabo, watau daya hadawan abu da iskar shaka jihar Fe, ya fi so ga stoichiometric canje-canje kwatsam.SSS ɗin da aka lalatar da zafi yana da mafi daidaiton saman ƙasa, Layer na kariya mai yawa, da mafi kyawun juriya na lalata.Ganin cewa SDSS mai sanyi-birgima, kasancewar Fe3 + - tsibiran masu wadata a ƙarƙashin rufin kariya yana keta mutuncin saman kuma yana haifar da lalata galvanic tare da madaidaicin wurin da ke kusa, wanda ke haifar da digo mai kaifi a cikin Rp (Table 1).An rage bakan EIS da juriyar lalatarsa.Ana iya ganin cewa rarraba cikin gida na Fe3 + tsibiran arziki saboda lalacewar filastik ya fi shafar juriya na lalata, wanda shine ci gaba a cikin wannan aikin.Don haka, wannan binciken yana gabatar da Hotunan ƙayyadaddun ƙayyadaddun ƙayyadaddun abubuwa na raguwar juriya na lalata samfuran SDSS da aka yi nazari ta hanyar nakasar filastik.
Bugu da kari, ko da yake kasa da kasa alloying a cikin dual lokaci karafa yana nuna mafi kyawun aiki, hulɗar wannan ƙari tare da matrix ɗin ƙarfe ɗaya cikin sharuddan halayen lalata bisa ga ƙayyadaddun ƙayyadaddun ƙayyadaddun ƙayyadaddun ƙayyadaddun gani.Bayyanar siginonin Ce (ta hanyar XAS M-gefuna) yana bayyana a ƴan wurare ne kawai yayin jujjuyawar sanyi, amma yana ɓacewa a lokacin zafi mai zafi na SDSS, yana nuna hazo na gida na Ce a cikin matrix ɗin ƙarfe, maimakon haɗaɗɗen haɗin gwiwa.Duk da yake ba a inganta kayan aikin injiniya na SDSS6,7 sosai ba, kasancewar abubuwan da ba kasafai ba na duniya suna rage girman abubuwan da aka haɗa kuma ana tunanin hana rami a yankin farko54.
A ƙarshe, wannan aikin yana bayyana tasirin yanayin yanayin ƙasa akan lalatar 2507 SDSS da aka gyara tare da cerium ta ƙididdige abubuwan sinadaran nanoscale.Mun amsa tambayar dalilin da ya sa bakin karfe lalata ko da a karkashin wani m Layer oxide ta hanyar ƙididdige microstructure, saman chemistry, da kuma sarrafa sigina ta amfani da K- nufin clustering.An kafa cewa tsibiran da ke da wadata a Fe3+, gami da haɗin gwiwar su na octahedral da tetrahedral tare da dukkan fasalin gaurayewar Fe2 +/Fe3 +, sune tushen lalacewa da lalata fim ɗin oxide mai sanyi-birgima na SDSS.Nanoislands wanda Fe3+ ya mamaye yana haifar da rashin juriya mara kyau ko da a gaban isassun stoichiometric Cr2O3 mai wucewa.Baya ga ci gaban dabara wajen tantance tasirin nau'ikan nau'ikan sinadarai na nanoscale akan lalata, ana sa ran aikin da ke gudana zai zaburar da hanyoyin injiniya don inganta juriyar gurɓataccen ƙarfe yayin yin ƙarfe.
Don shirya ingot Ce-2507 SDSS da aka yi amfani da ita a cikin wannan binciken, an narkar da wani abun da ya haɗa da Fe-Ce master alloy wanda aka hatimce da bututun ƙarfe mai tsafta a cikin tanderun shigar da matsakaicin kilogiram 150 don samar da narkakkar karfe kuma a zuba a cikin wani mold.Abubuwan da aka auna sinadarai (wt%) an jera su a cikin Ƙarin Tebura 2. Ingots an fara ƙirƙira su cikin tubalan.Sa'an nan kuma an shafe shi a 1050 ° C na minti 60 don samun karfe a cikin yanayin ingantaccen bayani, sa'an nan kuma a kashe shi cikin ruwa zuwa zafin jiki.An yi nazarin samfuran da aka yi nazari dalla-dalla ta amfani da TEM da DOE don nazarin matakai, girman hatsi da ilimin halittar jiki.Ana iya samun ƙarin cikakkun bayanai game da samfurori da tsarin samarwa a wasu kafofin6,7.
Samfurori na Silindrical (φ10 mm × 15 mm) don matsawa mai zafi an sarrafa su don haka axis na Silinda ya kasance daidai da nakasar shugabanci na toshe.An gudanar da matsananciyar zafi a yanayin zafi daban-daban a cikin kewayon 1000-1150 ° C ta amfani da na'urar kwaikwayo ta thermal Gleeble-3800 a matsakaicin matsakaici a cikin kewayon 0.01-10 s-1.Kafin nakasawa, samfuran sun yi zafi a cikin adadin 10 ° C s-1 na 2 min a zaɓaɓɓen zafin jiki don kawar da gradient zafin jiki.Bayan cimma daidaiton yanayin zafin jiki, samfurin ya zama naƙasasshe zuwa ƙimar ƙimar gaske na 0.7.Bayan nakasawa, ana kashe samfuran nan da nan da ruwa don adana gurɓataccen tsarin.Sa'an nan kuma za a yanke samfurin mai tauri daidai da alkiblar matsawa.Don wannan binciken na musamman, mun zaɓi samfurin tare da yanayin zafi mai zafi na 1050 ° C, 10 s-1 saboda microhardness da aka lura ya fi sauran samfuran7.
An yi amfani da samfura masu ƙarfi (80 × 10 × 17 mm3) na ingantaccen maganin Ce-2507 a cikin injina na LG-300 asynchronous guda biyu na mirgine tare da ingantattun kaddarorin injina tsakanin duk sauran matakan nakasa.Matsakaicin ƙima da raguwar kauri ga kowane hanya sune 0.2 m·s-1 da 5%, bi da bi.
An yi amfani da wurin aiki na lantarki na Autolab PGSTAT128N don ma'aunin lantarki na SDSS bayan sanyin juyi zuwa raguwar 90% a cikin kauri (1.0 daidai da nau'in gaskiya) kuma bayan danna zafi a 1050 ° C don 10 s-1 zuwa nau'in gaske na 0.7.Wurin aiki yana da tantanin halitta-electrode uku tare da madaidaicin calomel electrode azaman lantarki mai tunani, graphite counter electrode, da samfurin SDSS azaman lantarki mai aiki.An yanke samfuran a cikin silinda tare da diamita na 11.3 mm, zuwa sassan da aka sayar da wayoyi na jan karfe.An gyara samfuran tare da epoxy, suna barin yanki mai aiki na 1 cm2 azaman lantarki mai aiki (gefen ƙasa na samfurin cylindrical).Yi hankali yayin gyaran epoxy da yashi da gogewa na gaba don guje wa fashewa.Abubuwan da ke aiki sun kasance ƙasa kuma an goge su tare da dakatarwar goge lu'u-lu'u tare da girman barbashi na 1 μm, an wanke su da ruwa mai tsafta da ethanol, kuma an bushe su cikin iska mai sanyi.Kafin ma'auni na electrochemical, samfurori masu gogewa sun kasance suna nunawa zuwa iska na kwanaki da yawa don samar da fim din oxide na halitta.Maganin ruwa mai ruwa na FeCl3 (6.0 wt%), daidaitawa zuwa pH = 1.0 ± 0.01 tare da HCl bisa ga shawarwarin ASTM, ana amfani da shi don haɓaka lalata na bakin karfe55 saboda yana da lalata a gaban ions chloride tare da ƙarfin oxidizing da ƙananan pH Environmental da kuma G24.8 G24.Zuba samfurin a cikin maganin gwajin na awa 1 don isa kusa da daidaito kafin yin kowane ma'auni.Don ingantacciyar mafita, samfura masu zafi, da samfuran birgima mai sanyi, an aiwatar da ma'aunin impedance a buɗaɗɗen kewayawa (OPC) na 0.39, 0.33, da 0.25 V, bi da bi, a cikin kewayon mitar daga 1 105 zuwa 0.1 Hz tare da girman 5 mV.An maimaita duk gwaje-gwajen sinadarai aƙalla sau 3 a ƙarƙashin yanayi guda don tabbatar da sake fasalin bayanai.
Don ma'aunin HE-SXRD, tubalan karfe na rectangular duplex mai auna 1 × 1 × 1.5 mm3 an auna su don ƙididdige tsarin tsarin katako na babban wiggler mai ƙarfi na Brockhouse a CLS, Kanada56.An gudanar da tarin bayanai a cikin Geometry na Debye-Scherrer ko jigon watsawa a cikin ɗaki.Tsawon tsayin raƙuman X-ray wanda aka daidaita tare da madaidaicin LaB6 shine 0.212561 Å, wanda yayi daidai da 58 keV, wanda ya fi na Cu Kα (8 keV) wanda aka saba amfani dashi azaman tushen X-ray na dakin gwaje-gwaje.An samo samfurin a nesa na 740 mm daga mai ganowa.Girman ganowa na kowane samfurin shine 0.2 × 0.3 × 1.5 mm3, wanda aka ƙaddara ta girman katako da kauri samfurin.An tattara duk bayanan ta amfani da na'urar gano wuri Perkin Elmer, lebur panel X-ray detector, 200 µm pixels, 40×40 cm2 ta amfani da lokacin fallasa na 0.3 s da 120 firam.
An gudanar da ma'aunin X-PEEM na tsarin ƙira guda biyu da aka zaɓa a tashar ƙarshen Beamline MAXPEEM PEEM a cikin dakin gwaje-gwaje na MAX IV (Lund, Sweden).An shirya samfurori daidai da ma'auni na lantarki.An ajiye samfuran da aka shirya a cikin iska na kwanaki da yawa kuma an watsar da su a cikin ɗaki mai ɗorewa kafin a haskaka su da synchrotron photons.Tsarin makamashi na layin katako ya samu ta hanyar ion yana samar da bakan gizo a cikin Yaren Phenton daga E3 / 2, 57. Faɗin Layi na 11.3 Saboda haka, an kiyasta ƙudurin makamashi na beamline don zama E / ∆E = 700 eV / 0.3 eV> 2000 da juyi ≈1012 ph / s ta hanyar amfani da SX-700 monochromator da aka gyara tare da Si 1200-line mm-1 grating ga Fe 2p L2,2,2p, C2, C2, C2, C2, C2, C2, C2, 3, C2, C2, 3, 3, 2p, da Fe 2p. baki. Sabili da haka, an kiyasta ƙudurin makamashi na beamline don zama E / ∆E = 700 eV / 0.3 eV> 2000 da juzu'i ≈1012 ph / s ta hanyar amfani da SX-700 monochromator da aka gyara tare da Si 1200-line mm-1 grating ga Fe 2p L2.2.2 gefen, C.2p.5, C.2, C.2, C.2, C.3, C.3, C.2, C.3 da Fe 2p. baki. Таkym obrazom, эnergetycheskoe razreshennыe kanala chuchka bыlo otseneno kak E/∆E = 700 эВ/0,3 эВ > 2000 и 2000 ользовании модифицированного монохроматора SX-700 с решеткой Si 1200 штрихов/мм для Fe кромка 2p L2, 2p L23 2p L2,3 da kuma Ce M4,5. Don haka, an kiyasta ƙudurin makamashi na tashar katako kamar yadda E / ∆E = 700 eV / 0.3 eV> 2000 da juzu'i ≈1012 f / s ta amfani da SX-700 monochromator da aka gyara tare da Si grating na 1200 Lines / mm don Fe gefen 2p L2 ,3, Cr.5 Edge 2p L.3, Cr.5, L.2p & 2p.因此,光束线能量分辨率估计为E/ΔE = 700 eV/0.3 eV > 2000 和通量≈1012 ph/s栅的改进的SX-700 单色器用于 Fe 2p L2,3 边缘,因此线 mm-1 光栅 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.Don haka, lokacin amfani da gyare-gyaren SX-700 monochromator tare da layin 1200 Si grating.3, Cr baki 2p L2.3, Ni gefen 2p L2.3 da Ce baki M4.5.Duba makamashin photon a cikin matakan 0.2 eV.A kowane makamashi, an yi rikodin hotunan PEEM ta amfani da TVIPS F-216 fiber-coupled CMOS detector tare da 2 x 2 bins, wanda ke ba da ƙuduri na 1024 × 1024 pixels a cikin filin kallo na 20 µm.Lokacin bayyanar hotunan shine 0.2 s, matsakaicin firam 16.Ana zaɓar makamashin hoton hoto ta yadda za a samar da matsakaicin siginar lantarki na biyu.An gudanar da duk ma'aunai a al'ada ta al'ada ta amfani da katako na photon mai layi.Ana iya samun ƙarin bayani game da ma'auni a cikin binciken da ya gabata.Bayan nazarin yanayin gano yawan amfanin lantarki (TEY) da aikace-aikacen sa a cikin X-PEEM49, an kiyasta zurfin gwaji na wannan hanyar ya zama kusan 4-5 nm don siginar Cr da kusan 6 nm na Fe.Zurfin Cr yana kusa da kauri na fim din oxide (~ 4 nm) 60,61 yayin da zurfin Fe ya fi girma fiye da kauri.XRD da aka tattara a gefen Fe L shine cakuda XRD na baƙin ƙarfe oxides da Fe0 daga matrix.A cikin shari'ar farko, ƙarfin wutar lantarki da aka fitar ya fito ne daga kowane nau'in electrons da ke taimakawa ga TEY.Koyaya, siginar ƙarfe mai tsafta yana buƙatar ƙarin ƙarfin motsi don electrons su wuce ta Layer oxide zuwa saman kuma mai tantancewa ya tattara shi.A wannan yanayin, siginar Fe0 ya fi girma saboda LVV Auger electrons, da kuma na biyu electrons da suke fitarwa.Bugu da ƙari, ƙarfin TEY da waɗannan electrons suka ba da gudummawar sun lalace yayin hanyar tserewa ta lantarki, yana ƙara rage martanin Fe0 a cikin taswirar XAS na baƙin ƙarfe.
Haɗa ma'adinan bayanai a cikin cube data (X-PEEM data) wani muhimmin mataki ne na fitar da bayanan da suka dace (kayan sinadarai ko na jiki) a cikin hanyar da ta dace.K-ma'anar tari ana amfani dashi ko'ina a fagage da yawa, gami da hangen nesa na inji, sarrafa hoto, ƙirar ƙirar da ba a kula da shi ba, hankali na wucin gadi, da bincike na ƙima.Misali, gungu na K-ma'ana ya yi kyau sosai wajen tattara bayanan hoto na hyperspectral.A ka'ida, don bayanan fasali da yawa, K-ma'anar algorithm na iya haɗa su cikin sauƙi bisa bayanai game da halayensu (kaddarorin makamashi na hoto).K-ma'anar tari shine algorithm mai jujjuyawa don rarraba bayanai zuwa ƙungiyoyin K waɗanda ba su haɗa juna ba (gungu), inda kowane pixel ya kasance ga takamaiman gungu dangane da rarrabuwar rashin daidaituwar sinadarai a cikin ƙayyadaddun ƙirar ƙarfe.Algorithm na K-ma'anar ya ƙunshi matakai biyu: a matakin farko, K centroids ana ƙididdige su, kuma a mataki na biyu, kowane batu yana sanya gungu tare da centroid makwabta.An ayyana tsakiyar nauyi na tari azaman ma'anar lissafin ma'aunin bayanai (XAS spectrum) na wannan tari.Akwai nisa daban-daban don ayyana centroids makwabta azaman nisan Euclidean.Don hoton shigarwa na px, y (inda x da y suke ƙuduri a cikin pixels), CK shine tsakiyar tari;Ana iya raba wannan hoton zuwa gungu na K ta amfani da K-means63.Matakan ƙarshe na K-ma'anar tari algorithm sune:
Mataki 2. Lissafin membobin duk pixels bisa ga centroid na yanzu.Misali, ana lissafta shi daga nisan Euclidean d tsakanin tsakiya da kowane pixel:
Mataki 3 Sanya kowane pixel zuwa centroid mafi kusa.Sannan sake lissafin matsayin K centroid kamar haka:
Mataki na 4. Maimaita tsarin (equations (7) da (8)) har sai centroids sun haɗu.Sakamakon ingancin gungu na ƙarshe yana da alaƙa da ƙarfi tare da mafi kyawun zaɓi na centroids na farko.Don tsarin bayanan PEEM na hotunan karfe, yawanci X (x × y × λ) cube ne na bayanan tsararrun 3D, yayin da x da y axes ke wakiltar bayanan sarari ( ƙudurin pixel) kuma λ axis yayi daidai da photon.makamashi bakan hoto.Ana amfani da algorithm na K-ma'anar don bincika yankuna masu sha'awar bayanan X-PEEM ta hanyar raba pixels (gungu ko ƙananan tubalan) bisa ga fasalin fasalin su da kuma fitar da mafi kyawun centroids (XAS spectral profiles) ga kowane mai nazari.tari).Ana amfani da shi don nazarin rarraba sararin samaniya, sauye-sauyen yanayi na gida, halin oxidation, da jihohin sinadarai.Misali, K-ma'anar tari algorithm an yi amfani da shi don Fe L-gefen da Cr L-gefen yankuna a cikin aiki mai zafi da sanyi mai birgima X-PEEM.An gwada lambobi dabam-dabam na gungu na K (yankunan microstructure) don nemo mafi kyawun gungu da centroids.Lokacin da aka nuna waɗannan lambobi, ana canza pixels zuwa madaidaitan centroids cluster.Kowane rarraba launi yayi daidai da tsakiyar gungu, yana nuna tsarin sararin samaniya na sinadarai ko abubuwa na zahiri.Cire centroids haɗe-haɗe ne na layi na tsaftataccen bakan.
Ana samun bayanan da ke goyan bayan sakamakon wannan binciken bisa buƙatu mai ma'ana daga mawallafin WC.
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