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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 yashwar ƙarfe galibi ana danganta su da lalata waɗannan yadudduka, amma da wuya tare da bayyanar inhomogeneities na saman, ya danganta da matakin ƙananan. A cikin wannan aikin, nanoscale chemical surface heterogeneity, gano ta spectroscopic microscopy da chemometric analysis, bazata mamaye karaya da kuma lalatawar sanyi birgima cerium modified super duplex bakin karfe 2507 (SDSS) a lokacin da zafi nakasawa. Ko da yake X-ray photoelectron microscopy ya nuna in mun gwada da uniform ɗaukar hoto na halitta Cr2O3 Layer, passivation yi na sanyi birgima SDSS ya matalauta saboda gida rarraba Fe3+ arziki nanoislands a kan Fe/Cr oxide Layer. Wannan ilimin sikelin atomic yana ba da zurfin fahimtar lalata bakin karfe kuma ana sa ran zai taimaka wajen magance lalata na manyan karafa masu kama da juna.
Tun da aka ƙirƙira bakin ƙarfe, abubuwan da ke hana lalata ferrochrome an danganta su zuwa chromium, wanda ke samar da oxides mai ƙarfi / oxyhydroxides kuma yana nuna halayen wucewa a yawancin mahalli. Idan aka kwatanta da na al'ada (austenitic da ferritic) bakin karfe 1, 2, 3, super duplex bakin karfe (SDSS) suna da mafi kyawun juriyar lalata da kyawawan kaddarorin inji. 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, ta haka yana faɗaɗa aikace-aikacensa zuwa sarrafa gurɓata, kwantenan sinadarai, da masana'antar mai da iskar gas4. Koyaya, kunkuntar kewayon yanayin yanayin zafi da ƙarancin tsari na hana aikace-aikacen su mai fa'ida. Don haka, an gyara SDSS don inganta aikin da ke sama. Misali, an gabatar da gyare-gyaren Ce a cikin SDSS 2507 (Ce-2507) tare da babban abun ciki na nitrogen6,7,8. Abun da ba kasafai ake samu ba (Ce) a matakin da ya dace na 0.08 wt.% yana da tasiri mai fa'ida akan kaddarorin injinan DSS, tunda yana inganta gyaran hatsi da karfin iyakan hatsi. Juriya da sawa da lalata, ƙarfin juriya da ƙarfin yawan amfanin ƙasa, 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 an lalatar da su ta filastik a yanayin zafi daban-daban (cryogenic, sanyi da zafi) don cimma kyawawan kaddarorin inji6,7,8. Duk da haka, kyakkyawan juriya na lalatawar SDSS saboda kasancewar fim ɗin oxide na bakin ciki a saman yana shafar abubuwa da yawa kamar nau'in halitta na halitta saboda kasancewar nau'i-nau'i daban-daban tare da iyakokin hatsi daban-daban, abubuwan da ba a so da kuma amsa daban-daban. nakasar austenitic da ferritic matakai7. Sabili da haka, nazarin ƙananan yanki na irin waɗannan fina-finai har zuwa matakin tsarin lantarki ya zama mahimmanci don fahimtar lalata SDSS kuma yana buƙatar dabarun gwaji masu rikitarwa. Ya zuwa yanzu, hanyoyin da ke da hankali kamar Auger electron spectroscopy11 da X-ray photoelectron spectroscopy12,13,14,15 da hard X-ray photoemission microscopy (HAX-PEEM)16 gabaɗaya sun kasa gano bambance-bambancen sinadarai a cikin saman yadudduka. jihohin sunadarai iri ɗaya a wurare daban-daban na sararin samaniya na nanoscale. Yawancin karatu na baya-bayan nan sun danganta oxidation na chromium tare da halayen lalatawar austenitic bakin karfe17, martensitic steels18 da SDSS19,20. Koyaya, waɗannan karatun sun fi mayar da hankali kan tasirin Cr heterogeneity (misali, yanayin Cr3+ oxidation) 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, wadanda suka gaji karamin girman sakamakon maganin thermomechanical, suna cikin kusanci da juna, amma sun bambanta a cikin abun da ke ciki da yanayin oxidation16,21. Sabili da haka, don gano fashewar fina-finai na oxide da pitting na gaba, ya zama dole a fahimci yanayin yanayin ƙasa a matakin ƙananan ƙananan. Duk da waɗannan buƙatun, ƙididdiga masu ƙididdigewa kamar nau'in nau'in nau'i na gefe a cikin hadawan abu da iskar shaka, musamman ga Fe a sikelin nano- da atomic, har yanzu ba a gano su ba, kuma dangantakarsa da juriya na lalata ya kasance ba a gano ba. Har zuwa kwanan nan, yanayin sinadarai na abubuwa daban-daban, irin su Fe da Ca22, akan samfuran ƙarfe an ƙididdige su ta hanyar amfani da microscopy na X-ray mai laushi (X-PEEM) a cikin nanoscale synchrotron radiation wurare. Haɗe tare da sinadarai mai mahimmancin X-ray absorption spectroscopy (XAS), X-PEEM yana ba da damar ma'aunin XAS tare da babban ƙuduri na sararin samaniya da na gani, yana ba da bayanan sinadarai game da abun da ke cikin abubuwan da yanayin sinadaran su tare da ƙudurin sararin samaniya zuwa sikelin nanometer ashirin da uku. . Wannan kallo na spectromicroscopic na farkon yana sauƙaƙe duban sinadarai na gida kuma yana iya nuna canje-canjen sinadarai a cikin sararin saman ƙarfen da ba a bincika ba a baya.
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 tsarin chemometric mai tari na K-means24 don taswirar sinadari na duniya (hetero) kamannin abubuwan da abin ya shafa, waɗanda aka gabatar da jihohin sinadarai a cikin wakilcin ƙididdiga. Ya bambanta da lalata da aka fara ta hanyar lalata fim din chromium oxide a cikin al'ada na al'ada, ƙarancin wucewa da ƙananan juriya a halin yanzu ana danganta su zuwa ƙananan nanoislands masu arziki na Fe3 + kusa da Fe/Cr oxide Layer, wanda zai iya zama kayan kariya. Oxide yana lalata fim ɗin dige 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) bayani mai ruwa na FeCl3 a 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 tsayayyiyar rami ba a cikin ɗaki, bincike ya ba da haske game da yiwuwar gazawar abubuwan da suka faru da kuma lalata. An yi amfani da ma'auni mai dacewa (Fig. 1d) don dacewa da nau'in nau'in nau'i na electrochemical impedance spectroscopy (EIS), kuma an nuna sakamakon da ya dace a cikin Table 1. Ƙimar da ba ta cika ba ta bayyana a cikin maganin da aka magance da zafi da zafi, yayin da ƙananan ƙananan ƙwayoyin cuta suna bayyana a cikin takwarorinsu masu sanyi (Fig. .1b). A cikin EIS spectroscopy, radius na semicircle za a iya la'akari da juriya na polarization (Rp) 25,26. Rp na titin jirgin sama da aka magance a cikin Teburin 1 yana kusan 135 kΩ cm-2, duk da haka, ƙimar titin titin jirgin sama mai zafi da sanyi yana da ƙasa sosai, 34.7 da 2.1 kΩ cm-2, bi da bi. Wannan raguwa mai mahimmanci a cikin Rp yana nuna mummunan tasirin nakasar filastik akan wucewa da juriya na lalata, kamar yadda aka nuna a cikin rahotannin da suka gabata27,28,29,30.
a Nyquist, b, c Bode impedance da zane-zane na zamani, da d daidaitattun samfuran kewaye, inda RS shine juriya na electrolyte, Rp shine juriya na polarization, kuma QCPE shine oxide na madaidaicin kashi na yau da kullun da ake amfani da shi don ƙirar ƙarfin da ba daidai ba (n). Ana yin ma'aunin EIS a buɗaɗɗen kewayawa.
Ana nuna madaukai na lokaci ɗaya a cikin makircin Bode, tare da faranti a cikin kewayon mitar mai girma wanda ke wakiltar juriya na 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 matsakaicin matsakaicin matsakaicin mitar mitar, sannan ya ragu (Fig. 1c). Koyaya, a cikin duka lokuta uku, wannan matsakaicin har yanzu bai wuce 90 ° ba, yana nuna halayen ƙarfin ƙarfin da ba daidai ba saboda tarwatsewar capacitive. Don haka, ana amfani da kashi na QCPE akai-akai (CPE) don wakiltar rarrabawar iyawar tsaka-tsakin tsaka-tsaki wanda ya taso daga rashin daidaituwa ko rashin daidaituwa, musamman ma a sikelin atomic, joometry fractal, porosity electrode, yuwuwar rashin daidaituwa, da lissafi tare da sifar electrodes31,32. CPE impedance:
inda j shine lambar hasashe kuma ω shine mitar angular. QCPE mita ce mai zaman kanta wanda yayi daidai da ingantaccen wurin buɗewa na electrolyte. n lambar wutar lantarki ce marar girma wacce ke kwatanta karkacewar capacitor daga madaidaicin capacitance, watau mafi kusancin n shine 1, mafi kusancin CPE shine capacitive zalla, yayin da n yana kusa da sifili, yana bayyana tsayayya. Ƙananan ƙetare na n, kusa da 1, suna nuna halayen da ba su dace ba na saman bayan gwaje-gwajen polarization. QCPE na SDSS mai sanyi yana da girma fiye da takwarorinsa, ma'ana cewa ingancin saman ba shi da daidaituwa.
Daidaita da mafi yawan kaddarorin juriyar lalata na bakin karfe, babban abun ciki na Cr na SDSS gabaɗaya yana haifar da kyakkyawan juriya na lalatawar SDSS saboda kasancewar fim ɗin kariya na oxide mai wucewa akan saman17. Irin waɗannan fina-finai masu wucewa yawanci suna da wadatar Cr3+ oxides da/ko hydroxides, galibi a haɗe da Fe2+, Fe3+ oxides da/ko (oxy)hydroxides33. Duk da daidaitattun yanayi iri ɗaya, Layer oxide mai wucewa, kuma ba a lura da fashewar ƙasa bisa ga ma'auni na microscopic 6,7, halayen lalata na SDSS masu zafi da sanyi sun bambanta, don haka zurfafa nazarin sifofin microstructural wajibi ne don nakasar ƙarfe.
An yi nazarin ƙananan ƙananan ƙarfe na gurɓataccen ƙarfe ta ƙididdigewa ta amfani da haskoki na ciki da na synchrotron masu ƙarfi (Ƙarin Figures 1, 2). Ana ba da cikakken bincike a cikin Ƙarin Bayani. Kodayake akwai yarjejeniya gaba ɗaya akan nau'in babban lokaci, an sami bambance-bambance a cikin ɓangarorin ɓangarori masu yawa, waɗanda aka jera a cikin Ƙarin Teburin 1. Waɗannan bambance-bambancen na iya zama saboda ɓangarorin lokaci marasa daidaituwa a saman da kuma a cikin ƙarar, waɗanda ke shafar zurfin ganowar X-ray (XRD) daban-daban. ) tare da hanyoyin makamashi daban-daban na abubuwan da suka faru photons34. Ingantattun ɓangarorin austenite a cikin samfuran birgima mai sanyi wanda XRD ya ƙaddara daga tushen dakin gwaje-gwaje yana nuna mafi kyawun wucewa sannan kuma mafi kyawun juriya na lalata35, yayin da ƙarin ingantattun sakamako na ƙididdiga suna ba da shawarar saɓanin yanayin ɓangarorin 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. Samfuran da aka yi wa aiki mai zafi-da aka yi sun nuna yanayi mafi kyau, kwatankwacin hatsi Micron-sized, karin zoben Fig. 3) sun kasance alama ce ta mahimmin gyaran hatsi don aiki a cikin aikin da ya gabata. Wannan ya kamata ya fifita fim ɗin m. 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 yanayin sinadarai na microdomains na manyan abubuwa an yi nazari akai-akai ta amfani da X-PEEM. Ko da yake akwai ƙarin abubuwan haɗakarwa, Cr, Fe, Ni da Ce39 an zaɓi su a nan, tunda Cr shine maɓalli don ƙirƙirar fim ɗin m, Fe shine babban kashi na ƙarfe, kuma Ni yana haɓaka haɓakawa da daidaita yanayin ferrite-austenitic. Tsari da gyare-gyare shine manufar Ce. Ta hanyar daidaita makamashin katako na synchrotron, XAS ya kama manyan halayen Cr (L2.3 gefen), Fe (L2.3 gefen), Ni (L2.3), da Ce (M4.5 gefen) daga saman. -2507 SDSS. An yi nazarin bayanan da suka dace ta haɗa da daidaitawar makamashi tare da bayanan da aka buga (misali XAS akan Fe L2, 3 ribs40,41).
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 Cr da Fe L2,3 gefuna a kowane matsayi mai alama. Ƙashin L2,3 XAS yana bincika jihohin 3d na electrons da ba a cika su ba bayan photoexcitation a 2p3 / 2 (L3 gefen) da 2p1 / 2 (L2 gefen) matakan rarraba-orbit. An samo bayani game da yanayin valence na Cr daga nazarin diffraction X-ray na gefen L2,3 a cikin siffa 2b,d. Kwatancen mahaɗin. 42, 43 ya nuna cewa an lura da kololuwa hudu A (578.3 eV), B (579.5 eV), C (580.4 eV), da D (582.2 eV) kusa da gefen L3, yana nuna octahedral Cr3+ ions, daidai Cr2O3. Siffofin gwaji sun yarda da ƙididdige ƙididdiga, kamar yadda aka nuna a cikin bangarori b da e, waɗanda aka samo daga lissafin filin kristal da yawa a cikin 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 mai zafi-samar da SDSS daidai da gefen b Cr L2.3 da gefen c Fe L2.3, d Hoton Thermal X-PEEM na SDSS mai sanyi wanda ya dace da gefen e Cr L2.3 da f Fe L2.3 na gefe (e) . Siffar XAS da aka yi ƙulla a wurare daban-daban waɗanda aka yiwa alama akan hotuna masu zafi (a, d) ta layukan masu dige-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, ana amfani da palette na thermal don inganta karatun 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 sinadari na abubuwan da aka haɗa Ni da Ce ga samfuran duka sun kasance iri ɗaya. Ƙarin zane. A kan fig. 5-9 yana nuna hotuna na X-PEEM da madaidaicin sifofin XAS don Ni da Ce a wurare daban-daban a saman kayan aikin zafi da sanyi. Ni XAS yana nuna yanayin oxidation na Ni2+ a kan dukkan ma'aunin da aka auna na samfuran zafi da aka yi birgima (Ƙarin Tattaunawa). Yana da kyau a lura cewa a cikin yanayin da aka yi da zafi mai zafi, ba a lura da siginar XAS na Ce ba, yayin da bakan na Ce3 + na samfurori masu sanyi a wani lokaci. Duban alamun Ce a cikin samfuran sanyi-birgima ya nuna cewa Ce galibi yana wanzuwa ta hanyar hazo.
A cikin SDSS nakasar zafi, ba a sami canjin tsarin gida a cikin XAS ba a gefen Fe L2.3 (Fig. 2c). Duk da haka, kamar yadda aka nuna a cikin fig. 2f, Fe matrix a microscopically yana canza yanayin sinadarai a wurare bakwai da aka zaɓa a cikin sanyi mai birgima SSS. 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 amfani da ƙididdigar 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 haɗe-haɗe na 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 bayyana shi azaman 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 aikin da ya gabata, ko da yake ma'auni mai tsanani na biyu sun 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 yana nuna yiwuwar kawai Fe3 + kasancewa a cikin wannan yanayin. Idan akai la'akari da yanayin Fe3O4 tare da haɗuwa da Fe2 + da Fe3 +, an san cewa mafi raunin (ƙarfi) na farko a cikin L3 gefen Fe yana nuna ƙarami (mafi girma) rashin zama a cikin t2g jihar. Wannan ya shafi Fe2+ (Fe3+), wanda ke nuna karuwa a alamar farko da ke nuna karuwa a cikin Fe2+47. Waɗannan sakamakon sun nuna cewa Fe2+ da γ-Fe2O3, α-Fe2O3 da/ko Fe3O4 sun fi rinjaye akan saman da aka yi birgima mai sanyi na abubuwan da aka haɗa.
Girman hotunan zafi na (a, c) da (b, d) XAS bakan Fe L2,3 a wurare daban-daban na sarari tsakanin yankuna 2 da E a cikin figs. 2d.
Bayanan gwaji da aka samo (Fig. 4A da ƙarin Fig. 11) An lura da nau'ikan tsarkakakkun fe L-Es-1, Xas-2 da Xas-3, XAS-3: Fig.) An lura da su a wurare daban-daban wurare. Musamman ma, wani nau'i mai kama da 2-a (wanda aka nuna a matsayin XAS-1) a cikin siffa 3b an lura da shi a kan dukan yanki na sha'awa, sannan kuma 2-b bakan (lakabi XAS-2), yayin da aka lura da nau'i mai kama da E-3 a cikin fig. 3d (wanda ake kira XAS-3) an lura dashi a wasu wuraren da aka keɓe. Yawancin lokaci, ana amfani da sigogi guda huɗu don gano jihohin valence da ke cikin samfurin bincike: (1) L3 da L2 siffofi na ban mamaki, (2) matsayi na makamashi na L3 da L2 fasali, (3) L3-L2 bambancin makamashi, (4) L2 ƙarfin rabo / L3. Dangane da abubuwan gani na gani (Fig. 4a), duk abubuwan da aka gyara guda uku na Fe, wato Fe0, Fe2+, da Fe3+, suna nan a saman SDSS da aka yi nazari. Ƙididdigar ƙarfin ƙididdigewa L2/L3 kuma ya nuna kasancewar dukkan abubuwa uku.
Bayanan gwaji guda uku da aka lura daban-daban (layi masu ƙarfi XAS-1, XAS-2 da XAS-3 sun dace da 2-a, 2-b da E-3 a cikin siffa 2 da siffa 3) idan aka kwatanta da simulated XAS Comparison spectra, octahedrons Fe2+, Fe3+, darajar filin crystal na 1.0 eV, da gwaji na 1.0 eV, da gwaji (XAS-1, XAS-2, XAS-3) da daidaitattun bayanan LCF (layin baki mai ƙarfi), da kwatankwacin sifofin XAS-3 tare da Fe3O4 (haɗewar yanayin Fe) da Fe2O3 (tsarki Fe3+).
An yi amfani da haɗin kai tsaye (LCF) dacewa na ma'auni uku40,41,48 don ƙididdige abun da ke tattare da 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 ƙaramin leji da muka lura a cikin duk bayanan da gaskiyar cewa ƙarfe mai 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) 49 больше, чем предполагаемая толщина слоя окислоя окислоя позволяет обнаружить сигнал от железной матрицы (Fe0) под пассивирующим слоем. Lallai, zurfin binciken X-PEEM na Fe (~ 6 nm) 49 ya fi girman girman da aka ɗauka na Layer oxidation (dan kadan> 4 nm), wanda ke sa ya yiwu a gano siginar daga matrix baƙin ƙarfe (Fe0) a ƙarƙashin Layer passivation.A gaskiya ma, X-PEEM yana gano Fe (~ 6 nm) 49 zurfi fiye da kauri da ake tsammani na Layer oxide (kawai a kan 4 nm), yana ba da damar gano sigina 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. Hoto 4b yana nuna haɗin Fe2 + da Fe3 + a cikin XAS-1 bakan, inda ma'auni na Fe2 + da Fe3 + suna kusa, game da 45%, wanda ke nuna yanayin yanayin oxidation na Fe. Ganin cewa bakan XAS-2, yawan Fe2+ da Fe3+ ya zama ~ 30% da 60%, bi da bi. Abin da ke cikin Fe2+ ya yi ƙasa da na Fe3+. Rabon Fe2+ zuwa Fe3 na 1:2 yana nufin cewa Fe3O4 za a iya samu a daidai wannan rabo na Fe ions. Bugu da kari, don bakan XAS-3, yawan Fe2+ da Fe3+ sun canza zuwa ~ 10% da 80%, yana 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 mafi kusantar tushen Fe3 +, XAS-3 spectra an tsara su tare da ma'auni daban-daban na Fe3 + a cikin siffa 4e suna nuna kamance tare da duk ma'auni guda biyu lokacin da aka yi la'akari da Peak B. Koyaya, ƙarfin kafada (A: daga Fe2+) da ƙimar ƙarfin B/A suna nuna cewa bakan XAS-3 yana kusa da amma ba iri ɗaya da na γ-Fe2O3 ba. Idan aka kwatanta da girma γ-Fe2O3, ƙarfin Fe 2p XAS na ƙwanƙolin A SDSS ya ɗan fi girma (Fig. 4e), wanda ke nuna girman Fe2+ mafi girma. Kodayake bakan XAS-3 yayi kama da na γ-Fe2O3, inda Fe3 + ke kasancewa a cikin matsayi na Oh da Td, gano jihohin valence daban-daban da daidaitawa kawai ta gefen L2,3 ko girman girman L2 / L3 har yanzu yana da matsala. batun tattaunawa mai maimaitawa saboda sarkar abubuwa daban-daban da ke cikin bakan na ƙarshe41.
Baya ga wariyar launin fata na jihohin sinadarai na yankuna da aka zaɓa na sha'awar da aka bayyana a sama, an kimanta 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 martaba na gefen Cr L an saita su ta hanyar da za a samar da ingantattun gungu guda biyu da aka rarraba su a sararin aiki mai zafi da sanyi da aka nuna a cikin Figs. 5. A bayyane yake cewa ba a sami canje-canje na tsarin gida ba, tun da centroids 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 an rarraba iri ɗaya akan SDSS.
gungu na K-yana nufin L-gefen Cr yankuna, b daidai da XAS centroids. Sakamako na K-yana nufin X-PEEM kwatankwacin SDSS mai sanyi: c tari na yankunan K-ma'anar gefen Cr L2,3 da d madaidaitan XAS centroids.
Don kwatanta taswirar gefen FeL mafi hadaddun, ingantattun gungu huɗu da biyar ana amfani da su masu alaƙa (rabin rabe-raben rabe-rabe) don samfurori masu zafi da birgima, bi da bi. Saboda haka, ana iya samun kashi (%) na Fe2 + da Fe3 + ta hanyar daidaita 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 \(\rm{Fe} + 2e^ - \to\rm {Fe}^{2 + (3 + )}\), wanda shine 0.440 da 0.036 V, bi da bi. Wuraren da ke da ƙananan yuwuwar suna da babban abun ciki na mahadi Fe3+. Rarraba yuwuwar rarrabawa a cikin samfurin nakasasshen thermal 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). Ba a sami wasu canje-canje masu alaƙa da matsayi ba a cikin ƙananan lamellar ciki (Fig. 6b). Akasin haka, don haɗuwa da nau'o'in oxides daban-daban tare da abun ciki daban-daban na Fe2 + da Fe3 + a cikin SDSS mai sanyi, ana iya lura da yanayin rashin daidaituwa na pseudopotential (Fig. 6c, d). Fe3+ oxides da/ko (oxy)hydroxides sune manyan abubuwan lalata a cikin ƙarfe kuma suna iya jujjuyawa zuwa iskar oxygen da ruwa50. A wannan yanayin, ana iya ganin cewa tsibiran da ke cikin Fe3 + ana rarraba su a cikin gida kuma ana iya ɗaukar su azaman wuraren lalata. A wannan yanayin, gradient a cikin yuwuwar filin, maimakon madaidaicin ƙimar yuwuwar, ana iya la'akari da shi azaman mai nuni ga ƙayyadaddun yankuna masu lalata aiki51. Wannan inhomogeneous rarraba Fe2 + da Fe3 + a saman da sanyi birgima SDSS iya canza gida sinadaran Properties da kuma samar da wani mafi tasiri surface yankin a oxide fim fatattaka da lalata halayen, game da shi kyale matrix karfe matrix zuwa ci gaba da lalata, haifar da ciki inhomogeneity. da kuma rage halayen kariya na Layer passivating.
K-ma'anar gungu na yankuna na Fe L2,3 da madaidaitan XAS centroids don a-c mai zafi-aiki X-PEEM da d-f SDSS mai sanyi. a, d K-yana nufin gungun makircin da aka lullube akan hoton X-PEEM. Ƙimar pseudoelectrode yuwuwar (epseudo) an ambaci su tare da zane-zane na K-ma'ana. Hasken hoton X-PEEM kamar launi a cikin siffa 2 yana daidai da ƙarfin ɗaukar X-ray kai tsaye.
Ingantacciyar hanyar Cr amma yanayin sinadarai daban-daban na Fe yana haifar da asali daban-daban na fashewar fim ɗin oxide da tsarin lalata a cikin birgima mai zafi da sanyi mai birgima Ce-2507. Wannan kadarar ta sanyi ce-2507 sananne ne. Game da samuwar oxides da hydroxides na Fe a cikin iska mai iska, ana rufe halayen masu zuwa a cikin wannan aikin azaman halayen tsaka tsaki:
Dangane da ma'aunin X-PEEM, abin da ke sama ya faru a cikin waɗannan lokuta. 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 XAS na L gefen Fe. Tsawaitawa zuwa iska zai haifar da samuwar Fe3O4 da/ko Fe2O3 oxides bayan Fe (OH) 252,53. Nau'o'i biyu na barga Fe, Fe3O4 da Fe2O3, kuma suna iya samuwa a cikin wani Layer na kariya mai wadata na Cr3 +, inda Fe3O4 ya fi son tsari da haɗin kai. Kasancewar duka sakamakon biyu a cikin jihohin hadawan abu da iskar shaka (XAS-1 bakan). Bakan XAS-2 yafi dacewa da Fe3O4. Ganin cewa bakan XAS-3 da aka lura a wurare da yawa sun nuna cikakkiyar juyi zuwa γ-Fe2O3. Tun da na'urorin X-ray da ba a nannade suna da zurfin shigar kusan 50 nm, siginar da ke ƙasa yana haifar da ƙarin ƙarfi na kololuwar A.
Siffar XRD ta nuna cewa sashin Fe a cikin fim ɗin oxide yana da tsari mai laushi, wanda aka haɗa tare da Layer na Cr oxide. Ya bambanta da halayyar wucewar lalata saboda rashin daidaituwa na gida na Cr2O317, duk da nau'in nau'in nau'in Cr2O3 a cikin wannan binciken, an lura da ƙananan juriya a cikin wannan yanayin, musamman ga samfurori masu sanyi. Halin da aka lura ana iya fahimtar shi azaman nau'in yanayin yanayin iskar oxygenation na saman Layer (Fe) yana shafar aikin lalata. Jinkirin canja wurin ƙarfe ko ions oxygen a cikin lattice saboda stoichiometry ɗaya na babba (Fe oxide) da ƙananan yadudduka (Cr oxide) 52,53 yana haifar da mafi kyawun hulɗa (mannewa) a tsakanin su. Wannan, bi da bi, yana inganta juriya na lalata. Saboda haka, ci gaba da stoichiometry, watau yanayin oxidation ɗaya na Fe, ya fi dacewa da canje-canjen stoichiometric kwatsam. SDSS maras ƙarfi ta thermally yana da ƙarin daidaitaccen saman ƙasa da Layer na kariya mai yawa, wanda ke ba da mafi kyawun juriya na lalata. Duk da haka, don SDSS mai sanyi, kasancewar Fe3 + - tsibiran masu wadata a ƙarƙashin tsarin kariya yana lalata mutuncin saman kuma yana haifar da lalata galvanic na substrate na kusa, wanda ke haifar da raguwa a cikin Rp (Table 1) a cikin EIS bakan da lalata. juriya. Sabili da haka, tsibiran da aka rarraba a cikin gida masu wadata a Fe3+ saboda nakasar filastik galibi suna tasiri aikin juriya na lalata, wanda shine ci gaba a cikin wannan aikin. Don haka, wannan binciken yana gabatar da spectromicrographs na raguwar juriya na lalata saboda nakasar filastik na samfuran SDSS da aka yi karatu.
Bugu da ƙari kuma, yayin da ƙarancin ƙasa a cikin karafa na lokaci biyu yana aiki mafi kyau, hulɗar wannan ƙarin kashi tare da matrix ɗin ƙarfe ɗaya cikin sharuddan halayen lalata ya kasance mai wuyar gaske dangane da abubuwan gani na gani na gani. Siginar Ce (tare da XAS M-gefen) yana bayyana ne kawai a ƴan wurare yayin jujjuyawar sanyi, amma yana ɓacewa a lokacin zafi mai zafi na SDSS, yana nuna alamar gida na Ce a cikin matrix ɗin ƙarfe maimakon haɗaɗɗen allo. Ko da yake ba a inganta kayan aikin injiniya na SDSS6,7, kasancewar REE yana rage girman abubuwan da aka haɗa kuma ana tunanin zai hana rami a asalin54.
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 lokacin da aka mai rufi da wani m Layer oxide ta quantitatively nazarin microstructure, sinadarai yanayin saman fasali da kuma sarrafa sigina ta amfani da K- nufin tari. An kafa cewa Fe3 + - tsibiran masu wadata, gami da haɗin gwiwar su na octahedral da tetrahedral a duk faɗin tsarin gauraya Fe2+/Fe3+, tushen lalata fim ɗin oxide ne kuma tushen lalatawar SDSS mai sanyi. 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 dabarar da aka samu wajen tantance tasirin nau'ikan nau'ikan sinadarai na nanoscale akan lalata, ana sa ran aikin na yanzu zai zaburar da hanyoyin injiniya don haɓaka juriya na lalata karafa yayin yin ƙarfe.
Don shirya ingots na Ce-2507 SDSS da aka yi amfani da su a cikin wannan binciken, gauraye abubuwan da suka haɗa da Fe-Ce master alloy da aka hatimce da bututun ƙarfe mai tsafta, an narkar da su a cikin tanderun shigar da matsakaicin mitar kilogiram 150 don samar da narkakken ƙarfe kuma a zuba a cikin simintin gyare-gyare. Abubuwan da aka auna sinadarai (wt%) an jera su a cikin ƙarin Tebura 2. Ingot ɗin yana da zafi na farko da ya zama tubalan. Sa'an nan kuma an shafe karfe a 1050 ° C na minti 60 zuwa wani bayani mai mahimmanci, sa'an nan kuma a kashe shi a 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.
Tsari samfurori na silindi (φ10 mm × 15 mm) don matsi mai zafi tare da axis na Silinda a layi daya zuwa nakasar shugabanci na toshe. An yi matsananciyar zafin jiki a matsakaicin matsakaici a cikin kewayon 0.01-10 s-1 a yanayi daban-daban a cikin kewayon 1000-1150 ° C ta amfani da na'urar kwaikwayo ta thermal Gleeble-3800. Kafin nakasawa, samfurori sun yi zafi a zafin jiki da aka zaɓa a cikin adadin 10 ° C s-1 na 2 min don kawar da gradient zafin jiki. Bayan cimma daidaiton yanayin zafin jiki, samfuran sun lalace zuwa ƙimar ƙimar gaske na 0.7. Bayan nakasawa, nan da nan an kashe shi da ruwa don kula da gurɓataccen tsari. Sa'an nan kuma an yanke samfurori masu tauri a layi daya zuwa alkiblar matsawa. Don wannan binciken na musamman, mun zaɓi wani samfurin da ya lalace a 1050 ° C, 10 s-1 saboda mafi girma da aka lura da microhardness fiye da sauran samfuran7.
Girma (80 × 10 × 17 mm3) samfurori na ingantaccen bayani na Ce-2507 an gwada su akan na'urar lalata mai juzu'i mai nau'i-nau'i guda uku LG-300, wanda ya ba da mafi kyawun kaddarorin injina a tsakanin duk sauran nau'ikan gurɓataccen yanayi6. Matsakaicin ƙima da raguwar kauri sun kasance 0.2 m·s-1 da 5% ga kowace hanya, bi da bi.
An yi amfani da wurin aiki na lantarki na lantarki na Autolab PGSTAT128N don auna SDSS ta hanyar lantarki bayan mirgina sanyi zuwa 90% rage kauri (1.0 daidai nau'in gaskiya) da matsawa mai zafi zuwa 0.7 na gaskiya a 1050 oC da 10 s-1. 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. Sa'an nan samfurin da aka zuba tare da epoxy guduro, barin wani aiki bude yanki na 1 cm2 a matsayin mai aiki electrode (ƙananan saman na cylindrical samfurin). Yi amfani da kulawa yayin gyaran epoxy da kuma lokacin yashi da gogewa na gaba don guje wa fashewa. Wurin aiki yana lapped kuma an goge shi tare da dakatarwar goge lu'u-lu'u tare da girman barbashi na 1 micron, an tsabtace shi da ruwa mai tsafta da ethanol kuma an bushe a 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. Wani bayani mai ruwa na FeCl3 (6.0 wt.%), daidaitawa tare da HCl zuwa pH = 1.0 ± 0.01, an yi amfani da shi don haɓaka lalata na bakin karfe55, tun da yake an samo shi a cikin yanayi mai tsanani inda ions chloride ke kasancewa tare da ƙarfin oxidizing da ƙananan pH kamar yadda ASTM ta ƙayyade. Matsayin da aka tsara shine G48 da A923. An nutsar da samfuran a cikin maganin gwajin na sa'a 1 kafin a ɗauki kowane ma'auni don isa ga yanayin da ke kusa da tsayawa. Don ingantaccen bayani, samfuran zafi da aka yi birgima da sanyi, kewayon ma'aunin impedance shine 1 × 105 ~ 0.1 Hz, kuma yuwuwar buɗewa (OPS) shine 5 mV, wanda shine 0.39, 0.33, da 0.25 VSCE, bi da bi. Kowane gwajin lantarki na kowane samfurin an maimaita shi aƙalla sau uku a ƙarƙashin yanayi guda don tabbatar da sake fasalin bayanai.
Don ma'aunin HE-SXRD, 1 × 1 × 1.5 mm3 tubalan ƙarfe na duplex na rectangular an auna su akan babban layin wiggler na Brockhouse mai ƙarfi a CLS, Kanada don ƙididdige fasalin fasalin56. An gudanar da tattara bayanai a cikin zafin ɗaki a cikin Geometry na Debye-Scherrer ko jigilar kaya. Tsawon tsayin radiyon da aka daidaita zuwa ga LaB6 calibrant 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. Ana sanya 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. Kowane ɗayan waɗannan bayanan an tattara su ta amfani da mai gano yanki na Perkin Elmer, na'urar ganowa ta X-ray, 200 µm pixels, 40 × 40 cm2, ta amfani da lokacin fallasa na daƙiƙa 0.3 da firam 120.
An gudanar da ma'aunin X-PEEM na tsarin ƙirar ƙira guda biyu a tashar ƙarshen PEEM na layin Beamline MAXPEEM 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. Ana samun ƙudurin makamashi na katako ta hanyar auna ma'aunin fitarwa na ion daga N 1 s zuwa 1 \ (\pi _g^ \ ast \) na yankin tashin hankali tare da hv = 401 eV a cikin N2 da kuma dogara da makamashin photon akan E3 / 2.57. Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwararren Ƙwaƙwalwa na Ƙaƙwalwa na Ƙaƙwalwa ) ya yi a kan iyakar ƙarfin da aka auna. 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 L2,2p , L2, C, C, C, C, C, C, C, C, C2, 3, 2P, 2P, 2P, L2P, C2P, 2P, C2P, 2P, 2P, 2P, 2P, 2P, C2P, 2P, C2P, L2P, 2p, 2p, 2p da 2p Ce M4,5. Saboda haka, an kiyasta ƙudurin makamashi na beamline don zama E / ∆E = 700 eV / 0.3 eV> 2000 da kuma 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 gefe, L2.3 gefen, C.2p, C.2, C.3, C.2, C.3 da SX-2p. Ce M4.5. Таkym obrazom, эnergеtycheskoe razrешение knala chuchka bыlo otseneno kak E/∆E = 700 эВ/0,3 эВ> 2000 и 2000 и 2000 при использовании модифицированного монохроматора SX-700 с решеткой Si 1200 штрихов/мм для Fe кромать, L2,3, кромка Ni 2p L2,3 da кромка 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 ga Fe gefen 2p L2 ,3, Cr.2 gefen 3 L2p.2p.2p.3, Cr.3, L2, SX-2p. M4.5.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 通过使用0单色器和Si 1200 线mm−1 光栅用于 Fe 2p L2,3 边缘、Cr 2p L2,3 边缘、Ni 2p L2,3 边缘咘因此单色器 和 SI 1200 线 mm-1 光栅 于 Fe 2P 2P 2P L2.3 边缘、Cr 2p L2.3Don haka, lokacin amfani da gyare-gyaren SX-700 monochromator da layin 1200 Si grating. 3, Cr baki 2p L2.3, Ni gefen 2p L2.3 da Ce baki M4.5.Fadada makamashin photon a cikin matakan 0.2 eV. A kowane makamashi, an yi rikodin hotunan PEEM ta amfani da mai gano TVIPS F-216 CMOS tare da haɗin fiber optic na 2 x 2 yana samar da 1024 × 1024 pixels a cikin filin kallo na 20 µm. Lokacin bayyanar hotunan shine 0.2 seconds, matsakaicin firam 16. Ana zaɓar makamashin hoton hoto ta yadda za a samar da matsakaicin siginar lantarki na biyu. Ana yin duk ma'aunai a al'ada ta al'ada na katakon hoton hoto na layi. Don ƙarin bayani kan ma'auni, duba binciken da ya gabata58. Bayan nazarin jimlar yawan amfanin lantarki (TEY) yanayin ganowa 59 da aikace-aikacen sa a cikin X-PEEM, an kiyasta zurfin gano wannan hanyar a ~ 4-5 nm don siginar Cr da ~ 6 nm don siginar Fe. Zurfin Cr yana kusa da kauri na fim ɗin oxide (~ 4 nm) 60,61 yayin da zurfin Fe ya fi girma fiye da kauri na fim ɗin oxide. XAS ɗin da aka tattara a kusa da gefen Fe L shine cakuda baƙin ƙarfe oxide XAS da FeO daga matrix. A cikin yanayin farko, ƙarfin wutar lantarki da ake fitarwa yana faruwa ne saboda kowane nau'in electrons da ke iya ba da gudummawa ga TEY. Koyaya, siginar ƙarfe mai tsafta yana buƙatar ƙarin ƙarfin motsi don electrons su wuce ta Layer oxide, isa saman, kuma mai tantancewa ya tattara su. A wannan yanayin, siginar Fe0 ya fi girma saboda LVV Auger electrons da sakandaren lantarki da suke fitarwa. Bugu da ƙari, ƙarfin TEY da waɗannan electrons ke bayarwa ya lalace yayin hanyar tserewa ta hanyar lantarki49 yana ƙara rage sa hannun Fe0 a cikin taswirar XAS baƙin ƙarfe.
Haɗa haƙar ma'adinan bayanai a cikin cubes data (bayanan X-PEEM) muhimmin mataki ne na fitar da bayanan da suka dace (kayan sinadarai ko na zahiri) ta hanyoyi da yawa. K-ma'anar tari ana amfani dashi ko'ina a wurare da yawa, gami da hangen nesa na inji, sarrafa hoto, ƙirar ƙirar da ba a kula da shi ba, hankali na wucin gadi, da ƙididdigar ƙima24. Misali, K-ma'anar tari yana da amfani sosai ga tarin bayanan hoto na hyperspectral62. A ka'ida, don bayanan abubuwa da yawa, K-ma'anar algorithm na iya haɗa su cikin sauƙi gwargwadon bayanin halayensu (halayen makamashin hoto). K-ma'anar tari shine algorithm na jujjuya don rarraba bayanai zuwa ƙungiyoyin K waɗanda ba su zo ba (gungu), inda kowane pixel ya kasance ga takamaiman gungu wanda ya danganta da rarrabuwar yanayin rashin daidaituwar sinadarai a cikin ƙirar ƙananan ƙarfe. Algorithm na K-ma'anar ya ƙunshi matakai biyu: mataki na farko yana ƙididdige K centroids, kuma mataki na biyu yana sanya kowane batu zuwa gungu tare da centroid makwabta. An ayyana tsakiyar nauyi na gungu a matsayin ma'anar lissafin ma'aunin bayanai (XAS spectra) na wannan tari. Akwai nisa daban-daban don ayyana centroids makwabta azaman nisan Euclidean. Don hoton shigarwa na px, y (x da y ƙuduri ne a cikin pixels), CK shine cibiyar nauyi na 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. Yi ƙididdige ƙimar memba na 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 sosai tare da mafi kyawun zaɓi na farkon centroids63. Don tsarin bayanan PEEM na hotunan karfe, yawanci X (x × y × λ) cube ne na bayanan tsararru na 3D, yayin da x da y axes ke wakiltar bayanan sararin samaniya ( ƙudurin pixel) kuma λ axis ya yi daidai da yanayin yanayin makamashi na photons. An yi amfani da algorithm na K-ma'anar don gano yankuna masu sha'awar bayanan X-PEEM ta hanyar raba pixels (gungu ko ƙananan tubalan) bisa ga halayen su da kuma fitar da mafi kyawun centroid (XAS spectral curve) ga kowane mai nazari (cluster). Ana amfani da shi don nazarin rarraba sararin samaniya, sauye-sauye na yanayi na gida, halin oxidation da yanayin 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 daban-daban na K-clusters (yankunan ƙayyadaddun tsarin) don nemo mafi kyawun gungu da centroids. Lokacin da aka nuna jadawali, ana canza pixels zuwa madaidaitan centroids gungu. 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 daga marubucin WC bisa ga buƙatu mai ma'ana.
Sieurin, H. & Sandström, R. Karfe tauri na welded duplex bakin karfe. Sieurin, H. & Sandström, R. Karfe tauri na welded duplex bakin karfe. Sieurin, H. & Sandström, R. Вязкость разрушения сварной дуплексной. Sieurin, H. & Sandström, R. Karfe tauri na welded duplex bakin karfe. Sieurin, H. & Sandström, R. 焊接双相不锈钢的断裂韧性。 Sieurin, H. & Sandstrom, R. 焊接双相不锈钢的断裂韧性。 Sieurin, H. & Sandström, R. Вязкость разрусения Sieurin, H. & Sandström, R. Karya tauri na welded duplex bakin karfe.aikin. fractal. fur. 73, 377-390 (2006).
Adams, FV, Olubambi, PA, Potgieter, JH & Van Der Merwe, J. Lalata juriya na duplex bakin karafa a cikin zaɓaɓɓen kwayoyin acid da kwayoyin acid/chloride muhalli. Adams, FV, Olubambi, PA, Potgieter, JH & Van Der Merwe, J. Lalata juriya na duplex bakin karafa a cikin zaɓaɓɓen kwayoyin acid da kwayoyin acid/chloride muhalli.Adams, FW, Olubambi, PA, Potgieter, J. Kh. da Van Der Merwe, J. Lalata juriya na duplex bakin karfe a cikin mahalli tare da wasu kwayoyin acid da Organic acid/chlorides. Adams, FV, Olubambi, PA, Potgieter, JH & Van Der Merwe, J. Adams, FV, Olubambi, PA, Potgieter, JH & Van Der Merwe, J.Adams, FW, Olubambi, PA, Potgieter, J. Kh. da Van Der Merwe, J. Lalata juriya na duplex bakin karfe a cikin mahalli tare da wasu kwayoyin acid da Organic acid/chlorides.anticorrosive. Hanyar Mater 57, 107-117 (2010).
Barella S. et al. Lalata-oxidizing Properties na Fe-Al-Mn-C Duplex Alloys. Abubuwan 12, 2572 (2019).
Levkov, L., Shurygin, D., Dub, V., Kosyrev, K. & Balikoev, A. Sabon ƙarni na super duplex karfe don kayan aiki gas da mai samar. Levkov, L., Shurygin, D., Dub, V., Kosyrev, K. & Balikoev, A. Sabon ƙarni na super duplex karfe don kayan aiki gas da mai samar.Levkov L., Shurygin D., Dub V., Kosyrev K., Balikoev A. Sabon ƙarni na super duplex karfe don man fetur da gas samar da kayan aiki.Levkov L., Shurygin D., Dub V., Kosyrev K., Balikoev A. Sabon ƙarni na super duplex steels don gas da kuma samar da kayan aikin mai. E3S Webinar. 121, 04007 (2019).
Kingklang, S. & Uthaisangsuk, V. Binciken zafi nakasawa hali na Duplex bakin karfe sa 2507. Metall. Kingklang, S. & Uthaisangsuk, V. Binciken zafi nakasawa hali na Duplex bakin karfe sa 2507. Metall. Kingklang, S. & Uthaisangsuk, V. Kingklang, S. & Uthaisangsuk, V. Nazarin Zafafan Lalacewar Halayen Nau'in 2507 Duplex Bakin Karfe. Karfe. Kingklang, S. & Uthaisangsuk, V. 2507 级双相不锈钢的热变形行为研究。 Kingklang, S. & Uthaisangsuk, V. 2507Kingklang, S. da Utaisansuk, V. Binciken Halayen Nakasar Zafi Na Nau'in 2507 Duplex Bakin Karfe. Karfe.almajiri. hayyacinta. A 48, 95-108 (2017).
Zhou, T. et al. Tasirin mirgina sanyi mai sarrafawa akan microstructure da kaddarorin inji na cerium-gyaran super-duplex SAF 2507 bakin karfe. almajiri. ilimin kimiyya. aikin. 766, 138352 (2019).
Zhou, T. et al. Tsarin nakasawa mai zafi da kaddarorin inji na cerium-gyaran super-duplex SAF 2507 bakin karfe. J. Alma Matar. tankin ajiya. fasaha. 9, 8379-8390 (2020).
Zheng, Z., Wang, S., Long, J., Wang, J. & Zheng, K. Tasirin rare duniya abubuwa a kan high zafin jiki hadawan abu da iskar shaka hali na austenitic karfe. Zheng, Z., Wang, S., Long, J., Wang, J. & Zheng, K. Tasirin rare duniya abubuwa a kan high zafin jiki hadawan abu da iskar shaka hali na austenitic karfe.Zheng Z., Wang S., Long J., Wang J. da Zheng K. Tasirin abubuwan da ba kasafai suke yi a duniya ba a kan halayen karfen austenitic a karkashin yanayin iska mai zafi. Zheng, Z., Wang, S., Long, J., Wang, J. & Zheng, K. 稀土元素对奥氏体钢高温氧化行为的影响。 Zheng, Z., Wang, S., Long, J., Wang, J. & Zheng, K.Zheng Z., Wang S., Long J., Wang J. da Zheng K. Tasirin abubuwan da ba kasafai suke yi a duniya ba a kan halayen karfen austenitic a yanayin zafi mai zafi.lalata. ilimin kimiyya. 164, 108359 (2020).