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ʻO ke kila kila i hoʻohana nui ʻia a me kāna mau mana i hana ʻia he kūpaʻa i ka pala i nā kūlana ambient ma muli o ka papa passivation i hana ʻia me ka chromium oxide. ʻO ka pala a me ka erosion o ke kila e pili mau ana me ka luku ʻia ʻana o kēia mau papa, akā kākaʻikahi ma ka pae microscopic, ma muli o ke kumu o ka inhomogeneity o ka ʻili. Ma kēia hana, ʻo ka heterogeneity kemika nanoscale surface i ʻike ʻia e ka microscopy spectroscopic a me ka nānā ʻana chemometric e hoʻomalu koke i ka decomposition a me ka pala o ke kila kila super duplex i hoʻololi anu ʻia ʻo cerium 2507 (SDSS) i ka wā o kona ʻano deformation wela. ʻO kekahi ʻaoʻao. ʻOiai ua hōʻike ka microscopy photoelectron X-ray i ka uhi like ʻana o ka papa Cr2O3 kūlohelohe, ua hōʻike ka SDSS i hoʻopili anu i nā hopena passivation maikaʻi ʻole ma muli o ka hoʻolaha kūloko o nā nanoislands waiwai Fe3+ ma ka papa oxide Fe/Cr. Hāʻawi kēia ʻike ma ka pae atomika i kahi ʻike hohonu o ka pala kila kila a manaʻo ʻia e kōkua i ka hakakā ʻana i ka pala o nā metala alloy kiʻekiʻe like.
Mai ka wā i hana ʻia ai ke kila kila kila, ua pili ka pale ʻana o ka corrosion o nā ferrochromium alloys i ka chromium, kahi e hana ai i kahi oxide/oxyhydroxide ikaika e hōʻike ana i ke ʻano passivating ma ka hapa nui o nā wahi. Ke hoʻohālikelike ʻia me nā kila kila maʻamau (austenitic a me ferritic), ʻo nā kila kila super duplex (SDSS) me ka pale ʻana i ka corrosion ʻoi aku ka maikaʻi o nā waiwai mechanical kiʻekiʻe1,2,3. ʻO ka hoʻonui ʻana i ka ikaika mechanical e ʻae ai i nā hoʻolālā māmā a ʻoi aku ka liʻiliʻi. I ka hoʻohālikelike ʻana, ʻo ka SDSS waiwai he kūʻē kiʻekiʻe i ka pitting a me ka crevice corrosion, e hopena ana i kahi ola lawelawe lōʻihi a me nā noi ākea i ka kaohi haumia, nā pahu kemika, a me ka ʻoihana aila a me ke kinoea ma waho o ke kai4. Eia nō naʻe, ʻo ka laulā haiki o nā mahana mālama wela a me ka formability maikaʻi ʻole e pale aku i kāna noi ākea. No laila, ua hoʻololi ʻia ka SDSS e hoʻomaikaʻi i nā waiwai i luna. No ka laʻana, ua hoʻolauna ʻia ka hoʻololi ʻana o Ce a me nā hoʻohui kiʻekiʻe o N 6, 7, 8 ma 2507 SDSS (Ce-2507). ʻO kahi ʻano kūpono o 0.08 wt.% ka mea honua laha ʻole (Ce) he hopena maikaʻi ia i nā waiwai mechanical o ka DSS, ʻoiai e hoʻomaikaʻi ana i ka hoʻomaʻemaʻe ʻana o ka palaoa a me ka ikaika o ka palena palaoa. Ua hoʻomaikaʻi ʻia hoʻi ke kūpaʻa ʻana i ka ʻaʻahu a me ka palaho, ka ikaika tensile a me ka ikaika hua, a me ka hana wela. Hiki i ka nui o ka naikokene ke pani i ka nui o ka nickel pipiʻi, e hoʻolilo ana i ka SDSS i mea kūpono i ke kumukūʻai.
I kēia manawa, ua hoʻololi ʻia ka SDSS i ka plastically ma nā mahana like ʻole (haʻahaʻa haʻahaʻa, anu a me ka wela) e hoʻokō i nā waiwai mechanical maikaʻi loa6,7,8. Eia nō naʻe, ʻo ke kūpaʻa maikaʻi loa o ka SDSS ma muli o ke alo o kahi kiʻiʻoniʻoni oxide lahilahi ma luna o ka ʻili, kahi i hoʻopilikia ʻia e nā kumu he nui, e like me ke alo o nā pae he nui me nā palena palaoa like ʻole, nā precipitates makemake ʻole ʻia a me nā hopena like ʻole. ua hoʻololi ʻia ka microstructure inhomogeneous kūloko o nā ʻano austenitic a me ferritic like ʻole 7. No laila, ʻo ke aʻo ʻana i nā waiwai microdomain o ia mau kiʻiʻoniʻoni ma ka pae o ka hoʻonohonoho uila he mea nui loa ia no ka hoʻomaopopo ʻana i ka palaho SDSS a koi i nā ʻano hana hoʻokolohua paʻakikī. I kēia manawa, ʻo nā ʻano hana ʻili-sensitive e like me Auger electron spectroscopy11 a me X-ray photoelectron spectroscopy12,13,14,15 a me ka ʻōnaehana paʻakikī X-ray photoelectron photoelectron e hoʻokaʻawale, akā pinepine ʻaʻole hiki ke hoʻokaʻawale, i nā kūlana kemika o ka mea like ma nā wahi like ʻole ma ka hakahaka ma ka nanoscale. Ua hoʻopili kekahi mau noiʻi hou i ka oxidation kūloko o ka chromium i ke ʻano corrosion i ʻike ʻia o 17 mau kila kila austenitic, 18 mau kila kila martensitic, a me SDSS 19, 20. Eia nō naʻe, ua kālele nui kēia mau noiʻi i ka hopena o ka heterogeneity Cr (e laʻa, Cr3+ oxidation state) ma ke kūpaʻa ʻana i ka corrosion. Hiki ke hana ʻia ka heterogeneity lateral i nā mokuʻāina oxidation o nā mea e nā hui like ʻole me nā mea like, e like me nā oxides hao. Hoʻoilina kēia mau hui i kahi nui liʻiliʻi i hana ʻia me ka thermomechanically e pili kokoke ana kekahi i kekahi, akā ʻokoʻa i ka haku mele a me ke kūlana oxidation16,21. No laila, ʻo ka hōʻike ʻana i ka luku ʻia ʻana o nā kiʻiʻoniʻoni oxide a laila pitting e pono ai ka hoʻomaopopo ʻana i ka inhomogeneity o ka ʻili ma ka pae microscopic. ʻOiai kēia mau koi, ʻo nā loiloi quantitative e like me ka heterogeneity oxidation lateral, ʻoi aku ka hao ma ka nano/atomic scale, ʻaʻole i ʻimi ʻia a ʻo ko lākou koʻikoʻi no ke kūpaʻa ʻana i ka corrosion. A hiki i kēia manawa koke nei, ua wehewehe ʻia ke ʻano kemika o nā mea like ʻole, e like me Fe a me Ca, ma nā laʻana kila me ka hoʻohana ʻana i ka microscopy photoelectron X-ray palupalu (X-PEEM) i loko o nā hale hana radiation synchrotron nanoscale. I hui pū ʻia me nā ʻenehana spectroscopy absorption X-ray (XAS) chemically sensitive, hiki iā X-PEEM ke ana ʻana iā XAS me ka hoʻonā spatial a me spectral kiʻekiʻe, e hāʻawi ana i ka ʻike kemika e pili ana i ka haku mele elemental a me kona kūlana kemika me ka hoʻonā spatial a hiki i ka nanometer scale 23. ʻO kēia nānā spectroscopic o ke kahua o ka hoʻomaka ʻana ma lalo o kahi microscope e hoʻomaʻamaʻa i nā hoʻokolohua kemika kūloko a hiki ke hōʻike spatial i nā loli kemika i ʻimi ʻole ʻia ma ka papa Fe.
Hoʻonui kēia haʻawina i nā pono o PEEM i ka ʻike ʻana i nā ʻokoʻa kemika ma ka nanoscale a hōʻike i kahi ʻano loiloi ʻili atomika intuitive no ka hoʻomaopopo ʻana i ke ʻano corrosion o Ce-2507. Hoʻohana ia i ka K-means cluster chemometric data24 e palapala i ka haku mele kemika honua (heterogeneity) o nā mea i pili, me ko lākou mau kūlana kemika i hōʻike ʻia ma kahi hōʻike helu. ʻAʻole like me ka hihia kuʻuna o ka corrosion i hoʻokumu ʻia e ka haki ʻana o ka chromium oxide film, ʻo ka passivation maikaʻi ʻole o kēia manawa a me ke kūpaʻa ʻole o ka corrosion e pili ana i nā nanoislands waiwai Fe3+ kūloko kokoke i ka papa oxide Fe/Cr, ʻo ia paha ka hopena o nā oxides pale. Ma kahi o ka haki ʻana, ua hoʻokumu ʻia kahi kiʻiʻoniʻoni e hoʻoulu ai i ka corrosion.
Ua loiloi mua ʻia ke ʻano corrosive o ka SDSS 2507 i hoʻololi ʻia me ka hoʻohana ʻana i nā ana electrochemical. Ma ke kiʻi. Hōʻike ka Kiʻi 1 i nā piʻo Nyquist a me Bode no nā laʻana i koho ʻia i loko o nā hopena wai acidic (pH = 1) o FeCl3 ma ka mahana o ka lumi. Hana ka electrolyte i koho ʻia ma ke ʻano he mea oxidizing ikaika, e hōʻike ana i ke ʻano o ka ʻili passivation e haki. ʻOiai ʻaʻole i loaʻa ka mea i ka pitting mahana o ka lumi paʻa, ua hāʻawi kēia mau loiloi i ka ʻike i nā hanana hāʻule hiki a me nā kaʻina hana ma hope o ka corrosion. Ua hoʻohana ʻia ke kaapuni like (Kiʻi 1d) e hoʻokomo i nā spectra impedance spectroscopy electrochemical (EIS), a ua hōʻike ʻia nā hopena kūpono e pili ana ma ka Papa 1. Ua ʻike ʻia nā hapalua pōʻai piha ʻole i ka wā e hoʻāʻo ai i nā laʻana i mālama ʻia a hana wela ʻia, ʻoiai ua ʻōwili anu ʻia nā hapalua pōʻai i hoʻopaʻa ʻia (Kiʻi 1b). I ka spectrum EIS, hiki ke noʻonoʻo ʻia ka radius semicircle ʻo ia ke kū'ē polarization (Rp)25,26. ʻO ka Rp o ka SDSS i mālama ʻia i ka hopena ma ka Papa 1 ma kahi o 135 kΩ cm-2, akā naʻe no ka SDSS i hana wela ʻia a me ka SDSS i ʻōwili anu ʻia hiki iā mākou ke ʻike i nā waiwai haʻahaʻa loa o 34.7 a me 2.1 kΩ cm–2. ʻO kēia emi nui ʻana o Rp e hōʻike ana i kahi hopena maikaʻi ʻole o ka deformation plastic i ka passivation a me ke kūpaʻa ʻana i ka corrosion, e like me ka mea i hōʻike ʻia ma nā hōʻike mua 27, 28, 29, 30.
a ʻO Nyquist, b, c Bode impedance a me nā kiʻikuhi pae, a me kahi kumu hoʻohālike kaapuni like no d, kahi ʻo RS ke kū'ē electrolyte, ʻo Rp ke kū'ē polarization, a ʻo QCPE ka oxide element pae mau i hoʻohana ʻia e hoʻohālike i ka capacitance kūpono ʻole (n). Ua hoʻokō ʻia nā ana EIS ma ka hiki ke hoʻouka ʻole.
Hōʻike ʻia nā kūpaʻa kauoha mua ma ka kiʻikuhi Bode a hōʻike ka plateau alapine kiʻekiʻe i ke kū'ē electrolyte RS26. I ka emi ʻana o ke alapine, piʻi ka impedance a loaʻa kahi kihi pae maikaʻi ʻole, e hōʻike ana i ka capacitance dominance. Piʻi ka kihi pae, e mālama ana i kona waiwai kiʻekiʻe loa ma kahi ākea alapine ākea, a laila emi iho (Kiʻi 1c). Eia naʻe, i nā hihia ʻekolu a pau, ʻoi aku ka liʻiliʻi o kēia waiwai kiʻekiʻe ma mua o 90°, e hōʻike ana i kahi ʻano capacitive maikaʻi ʻole ma muli o ka hoʻolaha capacitive. No laila, hoʻohana ʻia ka QCPE constant phase element (CPE) e hōʻike i ka hoʻolaha capacitance interfacial i loaʻa mai ka ʻili o ka ʻili a i ʻole ka inhomogeneity, ʻoi aku hoʻi ma ke ʻano o ka unahi atomika, ka geometry fractal, ka porosity electrode, ka hiki ʻole ke like, a me ka hoʻolaha ʻana o ke au e pili ana i ka ʻili. Geometry electrode 31,32. CPE impedance:
kahi ʻo j ka helu hoʻokalakupua a ʻo ω ka alapine angular. ʻO QCPE kahi alapine kūʻokoʻa mau e pili ana i ka wahi hāmama hana o ka electrolyte. ʻO n kahi helu mana dimensionless e wehewehe ana i ka ʻokoʻa mai ke ʻano capacitive kūpono o kahi capacitor, ʻo ia hoʻi, ʻo ka kokoke o n i ka 1, ʻo ka kokoke o CPE i ka capacitance maʻemaʻe, a inā kokoke ʻo n i ka ʻole, he kūʻē ia. ʻO kahi ʻokoʻa liʻiliʻi o n, kokoke i ka 1, e hōʻike ana i ke ʻano capacitive kūpono ʻole o ka ʻili ma hope o ka hoʻāʻo polarization. ʻOi aku ke kiʻekiʻe o ka QCPE o ka SDSS i ʻōwili anu ʻia ma mua o nā huahana like, ʻo ia hoʻi, ʻaʻole like ka maikaʻi o ka ʻili.
E kūlike me ka hapa nui o nā waiwai kūpaʻa i ka palaho o nā kila kila kila, ʻo ka nui o ka Cr o SDSS e hopena i ka kūpaʻa maikaʻi loa o SDSS ma muli o ke alo o kahi kiʻiʻoniʻoni oxide pale passive ma luna o ka ʻili17. ʻO kēia kiʻiʻoniʻoni passivating he waiwai nui ia i nā oxides Cr3+ a/a i ʻole hydroxides, e hoʻohui nui ana i ka Fe2+, Fe3+ oxides a/a i ʻole (oxy)hydroxides 33. ʻOiai ke ʻano like o ka ʻili, ka papa oxide passivating, a ʻaʻohe haki i ʻike ʻia ma ka ʻili, e like me ka mea i hoʻoholo ʻia e nā kiʻi microscopic,6,7 ʻokoʻa ke ʻano palaho o ka SDSS i hana wela ʻia a me ke anu-wili ʻia a no laila pono e noiʻi hohonu i ka microstructure deformation a me ke ʻano hoʻonohonoho o ke kila.
Ua noiʻi ʻia ka microstructure o ke kila kila deformed me ka hoʻohana ʻana i nā kukuna X-energy kiʻekiʻe o loko a me synchrotron (Nā Kiʻi Hoʻohui 1, 2). Hāʻawi ʻia kahi loiloi kikoʻī ma ka ʻIke Hoʻohui. ʻOiai pili kēia i ke ʻano o ka pae nui, ua ʻike ʻia nā ʻokoʻa i nā ʻāpana nui o nā pae, i helu ʻia ma ka Papa Hoʻohui 1. Hiki ke ʻokoʻa ma muli o ka ʻāpana pae heterogeneous ma ka ʻili a me ka ʻāpana nui (XRD) i kau ʻia i ka hohonu ʻokoʻa o ka ʻike ʻana me ka hoʻohana ʻana i ka diffraction X-ray me nā kumu ikehu like ʻole o nā photons hanana. ʻO ka hapa kiʻekiʻe o ka austenite i nā specimens i ʻōwili anu ʻia, i hoʻoholo ʻia e XRD mai kahi kumu hale hana, e hōʻike ana i ka passivation maikaʻi a ma hope o ka pale ʻana i ka corrosion35, ʻoiai ʻoi aku ka pololei a me nā hopena helu e hōʻike ana i nā ʻano kūʻē i nā ʻāpana pae. Eia kekahi, pili pū ka pale ʻana i ka corrosion o ke kila i ke kiʻekiʻe o ka hoʻomaʻemaʻe ʻana i ka palaoa, ka hōʻemi ʻana o ka nui o ka palaoa, ka hoʻonui ʻana i nā microdeformations a me ka dislocation density e hana ʻia i ka wā o ka mālama thermomechanical36,37,38. Hōʻike nā ʻano hana wela i kahi ʻano ʻoi aku ka nui o nā hua, e hōʻike ana i nā hua micron-sized, ʻoiai ʻo nā apo laumania i ʻike ʻia i nā ʻano hana i ʻōwili anu ʻia (Kiʻi Hoʻohui 3) e hōʻike ana i ka hoʻomaʻemaʻe nui ʻana o ka hua i ka nanoscale i ka hana ma mua6, kahi e kōkua ai i ka passivation film. a me ka hoʻonui ʻana o ke kū'ē ʻana i ka corrosion. ʻO ke kiʻekiʻe o ka dislocation density e pili pinepine ʻia me ka haʻahaʻa o ke kū'ē ʻana i ka pitting, kahi e kūlike maikaʻi me nā ana electrochemical.
Ua aʻo ʻia nā loli i nā kūlana kemika o nā microdomains o nā mea mua me ka hoʻohana ʻana iā X-PEEM. ʻOiai ka nui o nā mea hoʻohuihui, ua koho ʻia ʻo Cr, Fe, Ni, a me Ce39 ma ʻaneʻi no ka mea ʻo Cr ke kumu nui no ka hoʻokumu ʻana o ke kiʻi passivation, ʻo Fe ke kumu nui i ke kila, a hoʻonui ʻo Ni i ka passivation a kaulike i ka ʻano ferrite-austenitic a me ke kumu o ka hoʻololi ʻana iā Ce. Ma ka hoʻoponopono ʻana i ka ikehu o ka radiation synchrotron, ua uhi ʻia ka RAS mai ka ʻili me nā hiʻohiʻona nui o Cr (kaʻe L2.3), Fe (kaʻe L2.3), Ni (kaʻe L2.3) a me Ce (kaʻe M4.5). ka hoʻokumu wela a me ka ʻōwili anu Ce-2507 SDSS. Ua hana ʻia ka loiloi ʻikepili kūpono ma ka hoʻohui ʻana i ka calibration ikehu me ka ʻikepili i paʻi ʻia (e laʻa me XAS 40, 41 ma Fe L2, 3 mau ʻaoʻao).
Ma ke kiʻi. Hōʻike ka Kiʻi 2 i nā kiʻi X-PEEM o ka hana wela (Kiʻi 2a) a me ka ʻōwili anu (Kiʻi 2d) Ce-2507 SDSS a me nā lihi XAS e pili ana o Cr a me Fe L2,3 ma nā wahi i hōʻailona ʻia. ʻO ka lihi L2,3 o ka XAS e nānā i nā kūlana 3d i noho ʻole ʻia ma hope o ka photoexcitation electron ma nā pae hoʻokaʻawale spin-orbit 2p3/2 (lihi L3) a me 2p1/2 (lihi L2). Ua loaʻa ka ʻike e pili ana i ke kūlana valence o Cr mai XAS ma ka lihi L2,3 ma ke Kiʻi 2b, e. Hoʻohālikelike me nā luna kānāwai. Ua hōʻike ʻia ʻehā mau piko i ʻike ʻia ma kahi kokoke i ka lihi L3, i kapa ʻia ʻo A (578.3 eV), B (579.5 eV), C (580.4 eV) a me D (582.2 eV), e hōʻike ana i ka octahedral Cr3+, e pili ana i ka ion Cr2O3. Ua kūlike nā spectra hoʻokolohua me nā helu kumumanaʻo i hōʻike ʻia ma nā panela b a me e, i loaʻa mai nā helu he nui o ke kahua kristal ma ka interface Cr L2.3 me ka hoʻohana ʻana i kahi kahua kristal o 2.0 eV44. Ua uhi ʻia nā ʻili ʻelua o ka SDSS i hana wela ʻia a me ka SDSS i ʻōwili anu ʻia me kahi papa like o Cr2O3.
he kiʻi wela X-PEEM o ka SDSS i hoʻololi ʻia i ke ʻano wela e pili ana i ka lihi b Cr L2.3 a me ka lihi c Fe L2.3, d kiʻi wela X-PEEM o ka SDSS i ʻōwili anu ʻia e pili ana i ka lihi e Cr L2.3 a me ka ʻaoʻao lihi f Fe L2.3 ( f). Ua hoʻolālā ʻia nā spectra XAS ma nā kūlana spatial like ʻole i hōʻailona ʻia ma nā kiʻi wela (a, d), ʻo nā laina kiko ʻalani ma (b) a me (e) e hōʻike ana i nā spectra XAS i hoʻohālikelike ʻia o Cr3+ me ka waiwai kahua kristal o 2.0 eV. No nā kiʻi X-PEEM, e hoʻohana i kahi palette wela e hoʻomaikaʻi i ka heluhelu ʻana o ke kiʻi, kahi e kūlike ai nā kala mai ka uliuli a i ka ʻulaʻula me ka ikaika o ka omo ʻana o ka X-ray (mai ka haʻahaʻa a i ke kiʻekiʻe).
Me ka nānā ʻole i ke kaiapuni kemika o kēia mau mea metala, ua mau ke ʻano kemika o nā hoʻohui ʻana o nā mea hoʻohuihui Ni a me Ce no nā laʻana ʻelua. Kiʻi hou aʻe. Hōʻike nā Kiʻi 5-9 i nā kiʻi X-PEEM a me nā spectra XAS e pili ana no Ni a me Ce ma nā kūlana like ʻole ma ka ʻili o nā laʻana i hana wela ʻia a me nā laʻana i ʻōwili anu ʻia. Hōʻike ʻo Ni XAS i nā kūlana oxidation o Ni2+ ma luna o ka ʻili holoʻokoʻa i ana ʻia o nā laʻana i hana wela ʻia a me nā laʻana i ʻōwili anu ʻia (Kūkākūkā Hoʻohui). Pono e hoʻomaopopo ʻia, i ke ʻano o nā laʻana i hana wela ʻia, ʻaʻole i ʻike ʻia ka hōʻailona XAS o Ce, ʻoiai i ke ʻano o nā laʻana i ʻōwili anu ʻia, ua ʻike ʻia ka spectrum o Ce3+. ʻO ka nānā ʻana o nā kiko Ce i nā laʻana i ʻōwili anu ʻia ua hōʻike nui ʻia ʻo Ce ma ke ʻano o nā precipitates.
I loko o ka SDSS i hoʻololi ʻia i ka wela, ʻaʻohe loli kūkulu kūloko ma XAS ma ka lihi Fe L2,3 i ʻike ʻia (Kiʻi 2c). Eia nō naʻe, hoʻololi ka matrix Fe micro-regional i kona kūlana kemika ma ʻehiku mau wahi i koho ʻia ma ke ʻano random o ka SDSS i ʻōwili anu ʻia, e like me ka mea i hōʻike ʻia ma ke Kiʻi 2f. Eia kekahi, i mea e loaʻa ai kahi manaʻo pololei o nā loli i ke kūlana o Fe ma nā wahi i koho ʻia ma ke Kiʻi 2f, ua hana ʻia nā haʻawina ʻili kūloko (Kiʻi 3 a me ke Kiʻi Hoʻohui 10) kahi i koho ʻia ai nā ʻāpana pōʻai liʻiliʻi. Ua hoʻohālikelike ʻia nā spectra XAS o ka lihi Fe L2,3 o nā ʻōnaehana α-Fe2O3 a me nā oxides octahedral Fe2+ e nā helu ʻana o ke kahua kristal he nui e hoʻohana ana i nā kahua kristal o 1.0 (Fe2+) a me 1.0 (Fe3+)44. Hoʻomaopopo mākou he ʻokoʻa nā symmetries kūloko o α-Fe2O3 a me γ-Fe2O345,46, loaʻa iā Fe3O4 ka hui pū ʻana o Fe2+ & Fe3+,47, a me FeO45 ma ke ʻano he Fe2+ oxide divalent formally (3d6). Hoʻomaopopo mākou he ʻokoʻa nā symmetries kūloko o α-Fe2O3 a me γ-Fe2O345,46, loaʻa iā Fe3O4 ka hui pū ʻana o Fe2+ & Fe3+,47, a me FeO45 ma ke ʻano he Fe2+ oxide divalent formally (3d6).E hoʻomaopopo he ʻokoʻa nā symmetries kūloko o α-Fe2O3 a me γ-Fe2O345,46, hoʻohui ʻo Fe3O4 iā Fe2+ a me Fe3+,47 a me FeO45 ma ke ʻano o ka oxide divalent formally Fe2+ (3d6).E hoʻomaopopo he ʻokoʻa nā symmetries kūloko o α-Fe2O3 a me γ-Fe2O345,46, loaʻa iā Fe3O4 ka hui pū ʻana o Fe2+ a me Fe3+,47 a hana ʻo FeO45 ma ke ʻano he oxide divalent formal Fe2+ (3d6). Loaʻa i nā ion Fe3+ āpau i loko o α-Fe2O3 nā kūlana Oh wale nō, ʻoiai ʻo γ-Fe2O3 e hōʻike pinepine ʻia e Fe3+ t2g [Fe3+5/3V1/3]eg O4 spinel me nā hakahaka i nā kūlana eg. No laila, loaʻa i nā ion Fe3+ i loko o γ-Fe2O3 nā kūlana Td a me Oh. E like me ka mea i ʻōlelo ʻia ma kahi pepa ma mua,45 ʻoiai he ʻokoʻa ka lakio ikaika o nā mea ʻelua, ʻo kā lākou lakio ikaika eg/t2g he ≈1, ʻoiai ma kēia hihia ʻo ka lakio ikaika i ʻike ʻia eg/t2g ma kahi o 1. Hoʻopau kēia i ka hiki ke loaʻa wale ʻo Fe3+ i ke kūlana o kēia manawa. Ke noʻonoʻo nei i ka hihia o Fe3O4 me Fe2+ a me Fe3+, ʻo ka hiʻohiʻona mua, ka mea i ʻike ʻia he nāwaliwali (ikaika) ka lihi L3 no Fe, e hōʻike ana i kahi helu liʻiliʻi (nui) o nā kūlana t2g i noho ʻole ʻia. Pili kēia iā Fe2+ (Fe3+), e hōʻike ana ʻo ka hiʻohiʻona mua o ka hoʻonui ʻana e hōʻike ana i ka hoʻonui ʻana i ka ʻike o Fe2+47. Hōʻike kēia mau hopena i ka noho pū ʻana o Fe2+ a me γ-Fe2O3, α-Fe2O3 a/a i ʻole Fe3O4 e noho aliʻi ana ma luna o ka ʻili i ʻōwili anu ʻia o nā composites.
Nā kiʻi kiʻi wela photoelectron i hoʻonui ʻia o nā spectra XAS (a, c) a me (b, d) e hele ana i ka lihi Fe L2,3 ma nā kūlana ākea like ʻole i loko o nā ʻāpana i koho ʻia 2 a me E ma nā Kiʻi 2d.
Ua hoʻolālā ʻia nā ʻikepili hoʻokolohua i loaʻa (Kiʻi 4a a me ke Kiʻi Hoʻohui 11) a ua hoʻohālikelike ʻia me ka ʻikepili no nā hui maʻemaʻe 40, 41, 48. ʻEkolu mau ʻano like ʻole o nā spectra Fe L-edge XAS i nānā ʻia ma ka hoʻokolohua (XAS- 1, XAS-2 a me XAS-3: Kiʻi 4a). Ma ke ʻano kūikawā, ua ʻike ʻia ka spectrum 2-a (i hōʻike ʻia ʻo XAS-1) ma ke Kiʻi 3b i ukali ʻia e ka spectrum 2-b (i kapa ʻia ʻo XAS-2) ma luna o ka wahi ʻike holoʻokoʻa, ʻoiai ua ʻike ʻia nā spectra e like me E-3 ma ke kiʻi 3d (i kapa ʻia ʻo XAS-3) ma nā wahi kikoʻī. Ma ke ʻano he kānāwai, ua hoʻohana ʻia ʻehā mau palena e ʻike i nā kūlana valence e kū nei i loko o ka laʻana ma lalo o ke aʻo ʻana: (1) nā ʻano spectral L3 a me L2, (2) nā kūlana ikehu o nā ʻano L3 a me L2, (3) ka ʻokoʻa ikehu L3-L2. , ( 4) ka lakio ikaika L2/L3. Wahi a nā nānā ʻike maka (Kiʻi 4a), aia nā ʻāpana Fe ʻekolu, ʻo ia hoʻi ʻo Fe0, Fe2+, a me Fe3+, ma ka ʻili SDSS e aʻo ʻia nei. Ua hōʻike pū ka lakio ikaika i helu ʻia ʻo L2/L3 i ke alo o nā ʻāpana ʻekolu.
ʻO kahi spectra XAS i hoʻohālikelike ʻia o Fe me ʻekolu ʻikepili hoʻokolohua like ʻole i ʻike ʻia (nā laina paʻa XAS-1, XAS-2 a me XAS-3 e pili ana iā 2-a, 2-b a me E-3 ma ke Kiʻi 2 a me 3) Hoʻohālikelike, Octahedrons Fe2+, Fe3+ me nā waiwai kahua kristal o 1.0 eV a me 1.5 eV, kēlā me kēia, nā ʻikepili hoʻokolohua i ana ʻia me bd (XAS-1, XAS-2, XAS-3) a me ka ʻikepili LCF i hoʻonui ʻia e pili ana (laina ʻeleʻele paʻa), a ma ke ʻano hoʻi o nā spectra XAS-3 me nā kūlana Fe3O4 (kūlana hui o Fe) a me Fe2O3 (Fe3+ maʻemaʻe).
Ua hoʻohana ʻia kahi hui kūpono linear (LCF) o nā kūlana ʻekolu 40, 41, 48 e helu i ka haku mele ʻana o ka hao oxide. Ua hoʻokō ʻia ʻo LCF no ʻekolu mau spectra Fe L-edge XAS i koho ʻia e hōʻike ana i ke ʻano ʻokoʻa kiʻekiʻe loa, ʻo ia hoʻi ʻo XAS-1, XAS-2 a me XAS-3, e like me ka mea i hōʻike ʻia ma ke Kiʻi 4b–d. No nā mea hoʻopili LCF, ua noʻonoʻo ʻia he 10% Fe0 i nā hihia āpau ma muli o ka ʻike ʻana i kahi lihi liʻiliʻi i nā ʻikepili āpau, a ma muli hoʻi o ka hao metala ka ʻāpana nui o ke kila. ʻOiaʻiʻo, ʻoi aku ka nui o ka hohonu o ka hoʻāʻo ʻana o X-PEEM no Fe (~ 6 nm) 49 ma mua o ka mānoanoa o ka papa oxidation i manaʻo ʻia (ʻoi aku ka nui ma mua o 4 nm), e ʻae ana i ka ʻike ʻana i ka hōʻailona mai ka matrix hao (Fe0) ma lalo o ka papa passivation. ʻOiaʻiʻo, ʻoi aku ka nui o ka hohonu o ka hoʻāʻo ʻana o X-PEEM no Fe (~ 6 nm) 49 ma mua o ka mānoanoa o ka papa oxidation i manaʻo ʻia (ʻoi aku ka nui ma mua o 4 nm), e ʻae ana i ka ʻike ʻana i ka hōʻailona mai ka matrix hao (Fe0) ma lalo o ka papa passivation. Действительно, пробная глубина X-PEEM для Fe (~ 6 нм)49 больше, чем предполагаемая толщина слоя окисленияго, > 4 ночпол обнаружить сигнал от железной матрицы (Fe0) под пассивирующим слоем. ʻOiaʻiʻo, ʻoi aku ka hohonu o ka probe X-PEEM no Fe (~6 nm)49 ma mua o ka mānoanoa i manaʻo ʻia o ka papa oxidation (ʻoi aku ka nui ma mua o 4 nm), e hiki ai ke ʻike i ka hōʻailona mai ka matrix hao (Fe0) ma lalo o ka papa passivation.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），允许检测来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） 允记钝化层 下方 铁基体 （fe0） 的。 信号 信号 信号 信号 信号 信号 信号 信号 信号 信号 信号信号Фактически, глубина обнаружения Fe (~ 6 нм) 49 с помощью X-PEEM больше, чем предполагаемая толщина оксиного (меного >сидного) что позволяет обнаруживать сигнал от железной матрицы (Fe0) ниже пассивирующего слоя. ʻO ka ʻoiaʻiʻo, ʻoi aku ka hohonu o ka ʻike ʻana o Fe (~6 nm) 49 e X-PEEM ma mua o ka mānoanoa i manaʻo ʻia o ka papa oxide (ʻoi aku ka nui ma mua o 4 nm), e hiki ai ke ʻike i ka hōʻailona mai ka matrix hao (Fe0) ma lalo o ka papa passivation. .Ua hana ʻia nā hui like ʻole o Fe2+ a me Fe3+ e ʻimi i ka hopena maikaʻi loa no ka ʻikepili hoʻokolohua i ʻike ʻia. Ma ke kiʻi 4b e hōʻike ana i ka XAS-1 spectrum no ka hui pū ʻana o Fe2+ a me Fe3+, kahi i like ai nā ʻāpana o Fe2+ a me Fe3+ ma kahi o 45%, e hōʻike ana i nā kūlana oxidation hui ʻia o Fe. ʻOiai no ka XAS-2 spectrum, lilo ka pakeneka o Fe2+ a me Fe3+ i ~30% a me 60%, kēlā me kēia. ʻOi aku ka liʻiliʻi o Fe2+ ma mua o Fe3+. ʻO ka lakio o Fe2+ i Fe3, like me 1:2, ʻo ia hoʻi hiki ke hoʻokumu ʻia ʻo Fe3O4 ma ka lakio like ma waena o nā ion Fe. Eia kekahi, no ka XAS-3 spectrum, lilo ka pakeneka o Fe2+ a me Fe3+ i ~10% a me 80%, e hōʻike ana i ka hoʻololi kiʻekiʻe o Fe2+ i Fe3+. E like me ka mea i ʻōlelo ʻia ma luna, hiki iā Fe3+ ke hele mai mai α-Fe2O3, γ-Fe2O3 a i ʻole Fe3O4. No ka hoʻomaopopo ʻana i ke kumu kūpono loa o Fe3+, ua hoʻolālā ʻia ka spectrum XAS-3 me nā kūlana Fe3+ like ʻole ma ke Kiʻi 4e, e hōʻike ana i ka like me nā kūlana ʻelua i ka wā e noʻonoʻo ai i ka piko B. Eia nō naʻe, ʻo ka ikaika o nā piko poʻohiwi (A: mai Fe2+) a me ka lakio ikaika B/A e hōʻike ana ua kokoke ka spectrum o XAS-3, akā ʻaʻole kūlike me ka spectrum o γ-Fe2O3. Ke hoʻohālikelike ʻia me ka γ-Fe2O3 nui, ʻoi aku ka ikaika o ka piko Fe 2p XAS o A SDSS (Kiʻi 4e), e hōʻike ana i ka ikaika kiʻekiʻe o Fe2+. ʻOiai ua like ka spectrum o XAS-3 me ko γ-Fe2O3, kahi i loaʻa ai ʻo Fe3+ ma nā kūlana Oh a me Td, ʻo ka ʻike ʻana i nā kūlana valence like ʻole a me ka hoʻonohonoho ʻana ma ka lihi L2,3 a i ʻole ka lakio ikaika L2/L3 e mau ana he pilikia. he kumuhana o ke kūkākūkā mau ʻana ma muli o ka paʻakikī o nā mea like ʻole e hoʻopilikia ai i ka spectrum hope loa41.
Ma waho aʻe o nā ʻokoʻa spectral i ke kūlana kemika o nā wahi hoihoi i koho ʻia i wehewehe ʻia ma luna, ua loiloi ʻia hoʻi ka heterogeneity kemika honua o nā mea nui ʻo Cr a me Fe ma ka hoʻokaʻawale ʻana i nā spectra XAS āpau i loaʻa ma ka ʻili laʻana me ka hoʻohana ʻana i ke ʻano clustering K-means. . Hoʻonohonoho ʻia nā ʻaoʻao lihi Cr L e hana i ʻelua mau hui kūpono i hoʻolaha ʻia ma kahi ākea i nā spectrums i hana wela ʻia a me nā ʻōwili anu i hōʻike ʻia ma nā Kiʻi 5. Ua maopopo ʻaʻole i ʻike ʻia nā loli kūkulu kūloko he like, ʻoiai ua like nā centroids ʻelua o nā spectra XAS Cr. ʻAneʻane like kēia mau ʻano spectral o nā hui ʻelua me nā mea e pili ana iā Cr2O342, ʻo ia hoʻi, ua like like nā papa Cr2O3 ma ka SDSS.
ʻO Cr L K-ʻo ia hoʻi nā hui ʻāpana lihi, a ʻo b nā kikowaena XAS pili. Nā hopena o ka hoʻohālikelike ʻana o K-means X-PEEM o ka SDSS i ʻōwili anu ʻia: c Cr L2.3 ʻāpana lihi o nā hui K-means a me d nā kikowaena XAS pili.
No ka hoʻākāka ʻana i nā palapala ʻāina lihi FeL paʻakikī, ua hoʻohana ʻia ʻehā a me ʻelima mau hui i hoʻomaikaʻi ʻia a me kā lākou mau centroids pili (nā ʻikepili spectral) no nā specimens i hana wela ʻia a me nā ʻōwili anu. No laila, hiki ke loaʻa ka pakeneka (%) o Fe2+ a me Fe3+ ma ke kau ʻana i ka LCF i hōʻike ʻia ma ke Kiʻi 4. Ua hoʻohana ʻia ka pseudoelectrode potential Epsudo ma ke ʻano he hana o Fe0 e hōʻike i ka microchemical inhomogeneity o ka ʻili oxide film. Ua manaʻo ʻia ʻo Epsudo e ka lula hui ʻana,
kahi \(\rm{E}_{\rm{Fe}/\rm{Fe}^{2 + (3 + )}}\) e like me \(\rm{Fe} + 2e^ – \ a i \rm { Fe}^{2 + (3 + )}\), 0.440 a me 0.036 V, kēlā me kēia. ʻO nā ʻāpana me ka hiki ke haʻahaʻa he ʻoi aku ka nui o ka hui Fe3+. ʻO ka hoʻolaha hiki i nā laʻana i hoʻololi ʻia i ka thermally he ʻano papa me ka loli nui loa ma kahi o 0.119 V (Kiʻi 6a, b). Pili loa kēia hoʻolaha hiki i ka topography ʻili (Kiʻi 6a). ʻAʻohe loli ʻē aʻe e pili ana i ke kūlana ma loko o ka laminar ma lalo i ʻike ʻia (Kiʻi 6b). Ma ke ʻano ʻē aʻe, no ka pilina o nā oxides like ʻole me nā ʻike like ʻole o Fe2+ a me Fe3+ i ka SDSS i ʻōwili anu ʻia, hiki i kekahi ke ʻike i kahi ʻano like ʻole o ka pseudopotential (Kiʻi 6c, d). ʻO nā oxides Fe3+ a/a i ʻole (oxy)hydroxides nā ʻāpana nui o ka popo i loko o ke kila a he permeable i ka oxygen a me ka wai50. I kēia hihia, ua manaʻo ʻia nā mokupuni waiwai i ka Fe3+ ua hoʻolaha ʻia ma kahi kūloko a hiki ke manaʻo ʻia he mau wahi i ʻino ʻia. I ka manawa like, hiki ke hoʻohana ʻia ka gradient i ke kahua hiki, ma mua o ka waiwai paʻa o ka hiki, ma ke ʻano he hōʻailona no ka localization o nā wahi ʻino hana. Hiki i kēia hoʻolaha like ʻole o Fe2+ a me Fe3+ ma ka ʻili o ka SDSS i ʻōwili anu ke hoʻololi i ka kemika kūloko a hāʻawi i kahi ʻili hana ʻoi aku ka pono i ka haki ʻana o ka ʻili oxide a me nā hopena corrosion, no laila e ʻae ana i ka corrosion mau o ka matrix metala ma lalo, e hopena ana i ka corrosion kūloko. heterogeneity o nā waiwai a me ka emi ʻana o nā waiwai pale o ka papa passivating.
ʻO nā hui K-means a me nā kikowaena XAS e pili ana ma ka ʻāpana lihi Fe L2.3 o ka X-PEEM ac wela-deformed a me df o ka SDSS i ʻōwili anu ʻia. a, d Nā kiʻi hui K-means i uhi ʻia ma nā kiʻi X-PEEM. Ua ʻōlelo ʻia ka pseudoelectrode potential i helu ʻia (Epseudo) me ka kiʻi hui K-means. ʻO ka ʻōlinolino o ke kiʻi X-PEEM, e like me ke kala ma ke Kiʻi 2, ua kūlike ia me ka ikaika o ka omo ʻana o ka X-ray.
ʻO ke ʻano like ʻole o ka Cr akā ʻokoʻa ke kūlana kemika o Fe e alakaʻi ai i nā ʻano hōʻino ʻili oxide like ʻole a me nā ʻano pala i ka Ce-2507 i hana wela ʻia a me ka Ce-2507 i ʻōwili anu ʻia. Ua aʻo maikaʻi ʻia kēia ʻano o ka Ce-2507 i ʻōwili anu ʻia. E pili ana i ka hoʻokumu ʻia ʻana o nā oxides a me nā hydroxides o Fe i ka lewa ambient i kēia hana kokoke i ke kūlike ʻole, penei nā hopena:
ʻO nā hopena ma luna aʻe e hana ʻia ma nā hiʻohiʻona ma lalo nei e pili ana i ka loiloi X-PEEM. Hoʻopili ʻia kahi poʻohiwi liʻiliʻi e pili ana iā Fe0 me ka hao metala ma lalo. ʻO ka hopena o ka metala Fe me ke kaiapuni e hopena i ka hoʻokumu ʻia ʻana o kahi papa Fe(OH)2 (equation (5)), kahi e hoʻonui ai i ka hōʻailona Fe2+ ma ka Fe L-edge XAS. ʻO ka lōʻihi o ka hoʻopili ʻana i ka ea e hopena i ka hoʻokumu ʻia ʻana o Fe3O4 a/a i ʻole Fe2O3 oxides ma hope o Fe(OH)252,53. ʻElua mau ʻano paʻa o Fe, ʻo Fe3O4 a me Fe2O3, hiki ke hana ʻia i loko o ka papa pale waiwai Cr3+, kahi e makemake ai ʻo Fe3O4 i kahi ʻano like a paʻa. ʻO ke alo o nā mea ʻelua e hopena i nā kūlana oxidation hui ʻia (XAS-1 spectrum). ʻO ka XAS-2 spectrum e pili nui ana iā Fe3O4. ʻOiai ʻo ka nānā ʻana o nā spectra XAS-3 ma kekahi mau wahi i hōʻike i ka hoʻololi piha ʻana i γ-Fe2O3. ʻOiai ʻo ka hohonu o ke komo ʻana o nā kukuna X i wehe ʻia ma kahi o 50 nm, ʻo ka hōʻailona mai ka papa haʻahaʻa e hopena i ka ikaika kiʻekiʻe o ka piko A.
Hōʻike ka spectrum XPA he ʻano papa ka ʻāpana Fe i loko o ka ʻili oxide i hui pū ʻia me kahi papa Cr oxide. I ka hoʻohālikelike ʻana i nā hōʻailona o ka passivation ma muli o ka inhomogeneity kūloko o Cr2O3 i ka wā o ka corrosion, ʻoiai ke ʻano like o ka papa o Cr2O3 i kēia hana, ʻike ʻia ka pale ʻana i ka corrosion haʻahaʻa ma kēia hihia, ʻoi aku hoʻi no nā specimens i ʻōwili anu ʻia. Hiki ke hoʻomaopopo ʻia ke ʻano i ʻike ʻia ʻo ia ka heterogeneity o ke kūlana oxidation kemika ma ka papa o luna (Fe), ka mea e hoʻopilikia ai i ka hana corrosion. Ma muli o ka stoichiometry like o ka papa o luna (iron oxide) a me ka papa o lalo (chromium oxide)52,53 ʻoi aku ka maikaʻi o ka launa pū ʻana (adhesion) ma waena o lākou e alakaʻi ai i ka lawe lohi ʻana o nā ion metala a i ʻole oxygen i loko o ka lattice, ʻo ia hoʻi, e alakaʻi ai i ka hoʻonui ʻana i ke kūpaʻa corrosion. No laila, ʻoi aku ka maikaʻi o ka ratio stoichiometric hoʻomau, ʻo ia hoʻi hoʻokahi kūlana oxidation o Fe, ma mua o nā loli stoichiometric koke. ʻOi aku ka like o ka ʻili o ka SDSS i hoʻololi ʻia i ka wela, kahi papa pale ʻoi aku ka paʻa, a ʻoi aku ka maikaʻi o ke kūpaʻa corrosion. ʻOiai no ka SDSS i ʻōwili anu ʻia, ʻo ke alo o nā mokupuni waiwai Fe3+ ma lalo o ka papa pale e hōʻino i ka pono o ka ʻili a hoʻoulu i ka pala galvanic me ka substrate kokoke, kahi e alakaʻi ai i ka hāʻule nui ʻana o Rp (Papa 1). Ua hoʻemi ʻia ka spectrum EIS a me kona kūpaʻa ʻana i ka pala. Hiki ke ʻike ʻia ʻo ka hoʻolaha kūloko o nā mokupuni waiwai Fe3+ ma muli o ka deformation plastic e hoʻopilikia nui i ke kūpaʻa ʻana i ka pala, he holomua ia i kēia hana. No laila, hōʻike kēia haʻawina i nā kiʻi microscopic spectroscopic o ka hōʻemi ʻana i ke kūpaʻa ʻana i ka pala o nā laʻana SDSS i aʻo ʻia e ke ʻano deformation plastic.
Eia kekahi, ʻoiai ʻo ka hoʻohui ʻana me nā mea honua laha ʻole i nā kila ʻelua-pae e hōʻike ana i ka hana maikaʻi aʻe, ʻo ka launa pū ʻana o kēia mea hoʻohui me kahi matrix kila pākahi ma ke ʻano o ke ʻano corrosion e like me ka ʻikepili microscopy spectroscopic e mau ana ka paʻakikī. ʻIke ʻia ka ʻike ʻia ʻana o nā hōʻailona Ce (ma o XAS M-edges) ma kekahi mau wahi i ka wā o ka ʻōwili anu, akā nalo i ka wā o ka deformation wela o ka SDSS, e hōʻike ana i ka ua kūloko o Ce i loko o ka matrix kila, ma mua o ka homogeneous alloying. ʻOiai ʻaʻole i hoʻomaikaʻi nui i nā waiwai mechanical o SDSS6,7, ʻo ka loaʻa ʻana o nā mea honua laha ʻole e hōʻemi i ka nui o nā inclusions a manaʻo ʻia e kāohi i ka pitting ma ka ʻāpana mua54.
I ka hopena, hōʻike kēia hana i ka hopena o ka heterogeneity o ka ʻili ma ka corrosion o 2507 SDSS i hoʻololi ʻia me ka cerium ma ka helu ʻana i ka ʻike kemika o nā ʻāpana nanoscale. Pane mākou i ka nīnau no ke aha e corrodes ai ke kila kila ʻoiai ma lalo o kahi papa oxide pale ma ka helu ʻana i kāna microstructure, ke kemika ʻili, a me ka hana hōʻailona me ka hoʻohana ʻana i ka K-means clustering. Ua hoʻokumu ʻia ʻo nā mokupuni waiwai i Fe3+, me kā lākou octahedral a me ka tetrahedral coordination ma ke ʻano holoʻokoʻa o Fe2+/Fe3+ i hui pū ʻia, ke kumu o ka hōʻino a me ka corrosion o ka kiʻiʻoniʻoni oxide SDSS i ʻōwili anu ʻia. ʻO nā Nanoislands i hoʻomalu ʻia e Fe3+ e alakaʻi i ka pale ʻino maikaʻi ʻole ʻoiai i ke alo o kahi papa passivating Cr2O3 stoichiometric lawa. Ma waho aʻe o nā holomua methodological i ka hoʻoholo ʻana i ka hopena o ka heterogeneity kemika nanoscale ma ka corrosion, manaʻo ʻia ka hana e hoʻomau nei e hoʻoulu i nā kaʻina hana ʻenekinia e hoʻomaikaʻi i ke kūpaʻa corrosion o nā kila kila i ka wā o ka hana kila.
No ka hoʻomākaukau ʻana i ka ingot Ce-2507 SDSS i hoʻohana ʻia ma kēia haʻawina, ua hoʻoheheʻe ʻia kahi hui like ʻana me ka Fe-Ce master alloy i hoʻopaʻa ʻia me kahi paipu hao maʻemaʻe i loko o ka umu hoʻokomo alapine waena 150 kg e hana i ke kila i hoʻoheheʻe ʻia a ninini ʻia i loko o kahi ʻōmole. Ua helu ʻia nā hui kemika i ana ʻia (wt%) ma ka Papa Hoʻohui 2. Hoʻoheheʻe mua ʻia nā Ingots i loko o nā poloka. A laila ua hoʻomehana ʻia ma 1050°C no 60 min e loaʻa ai ke kila i ke ʻano o kahi hopena paʻa, a laila hoʻopau ʻia i ka wai a hiki i ka mahana o ka lumi. Ua aʻo kikoʻī ʻia nā laʻana i aʻo ʻia me ka hoʻohana ʻana iā TEM a me DOE e aʻo i nā pae, ka nui o ka palaoa a me ke ʻano. Hiki ke loaʻa ka ʻike kikoʻī e pili ana i nā laʻana a me ke kaʻina hana ma nā kumu ʻē aʻe6,7.
Ua hana ʻia nā hāpana cylindrical (φ10 mm × 15 mm) no ka hoʻopili wela i mea e kūlike ai ke axis o ka cylinder me ke kuhikuhi deformation o ka poloka. Ua hoʻokō ʻia ka hoʻopili wela kiʻekiʻe ma nā mahana like ʻole ma ka pae o 1000-1150 ° C me ka hoʻohana ʻana i kahi simulator thermal Gleeble-3800 ma kahi helu strain mau ma ka pae o 0.01-10 s-1. Ma mua o ka deformation, ua hoʻomehana ʻia nā hāpana ma ka helu o 10 ° C s-1 no 2 min ma kahi mahana i koho ʻia e hoʻopau i ka gradient mahana. Ma hope o ka hoʻokō ʻana i ke ʻano like o ka mahana, ua hoʻololi ʻia ka hāpana i kahi waiwai strain maoli o 0.7. Ma hope o ka deformation, ua hoʻopau koke ʻia nā hāpana me ka wai e mālama i ke ʻano deformed. A laila ʻoki ʻia ka hāpana paʻakikī e like me ke kuhikuhi compression. No kēia haʻawina kikoʻī, ua koho mākou i kahi hāpana me ke kūlana strain wela o 1050 ° C, 10 s-1 no ka mea ʻoi aku ka kiʻekiʻe o ka microhardness i ʻike ʻia ma mua o nā hāpana ʻē aʻe7.
Ua hoʻohana ʻia nā laʻana nui (80 × 10 × 17 mm3) o ka hopena paʻa Ce-2507 i loko o kahi wili ʻelua-ʻōwili asynchronous ʻekolu-pae LG-300 me nā waiwai mechanical maikaʻi loa ma waena o nā pae deformation ʻē aʻe āpau6. ʻO ka helu hoʻoluhi a me ka hoʻemi ʻana o ka mānoanoa no kēlā me kēia ala he 0.2 m·s-1 a me 5%, kēlā me kēia.
Ua hoʻohana ʻia kahi kahua hana electrochemical Autolab PGSTAT128N no nā ana electrochemical SDSS ma hope o ka ʻōwili anu ʻana i ka 90% o ka mānoanoa (1.0 like ʻoiaʻiʻo like) a ma hope o ke kaomi wela ʻana ma 1050°C no 10 s-1 i kahi ʻoiaʻiʻo o 0.7. Loaʻa i ka kahua hana kahi cell electrode ʻekolu me kahi electrode calomel saturated ma ke ʻano he electrode kuhikuhi, kahi electrode counter graphite, a me kahi laʻana SDSS ma ke ʻano he electrode hana. Ua ʻoki ʻia nā laʻana i loko o nā cylinders me ke anawaena o 11.3 mm, i nā ʻaoʻao i hoʻopaʻa ʻia ai nā uea keleawe. A laila ua hoʻopaʻa ʻia nā laʻana me ka epoxy, e waiho ana i kahi ākea hana o 1 cm2 ma ke ʻano he electrode hana (ʻaoʻao lalo o ka laʻana cylindrical). E makaʻala i ka wā e hoʻōla ai i ka epoxy a me ke one ʻana a me ka polishing ma hope e pale aku i ka haki ʻana. Ua wili ʻia nā ʻili hana a poli ʻia me kahi hoʻokuʻu poli daimana me ka nui o ka ʻāpana o 1 μm, holoi ʻia me ka wai distilled a me ka ethanol, a hoʻomaloʻo ʻia i ka ea anuanu. Ma mua o nā ana electrochemical, ua hōʻike ʻia nā laʻana poli i ka ea no kekahi mau lā e hana i kahi kiʻiʻoniʻoni oxide kūlohelohe. Hoʻohana ʻia kahi hopena wai o FeCl3 (6.0 wt%), i hoʻopaʻa ʻia i ka pH = 1.0 ± 0.01 me HCl e like me nā ʻōlelo aʻoaʻo a ASTM, e hoʻolalelale i ka pala o ke kila kila 55 no ka mea he pala ia i ke alo o nā ion chloride me ka mana oxidizing ikaika a me nā kūlana kaiapuni pH haʻahaʻa G48 a me A923. E hoʻokomo i ka laʻana i loko o ka hopena hoʻāʻo no 1 hola e hiki ai i kahi kokoke i ke kūlana paʻa ma mua o ka hana ʻana i kekahi ana. No nā laʻana paʻa-hoʻonā, hoʻokumu wela, a me nā laʻana ʻōwili anu, ua lawe ʻia nā ana impedance ma nā potentials kaapuni hāmama (OPC) o 0.39, 0.33, a me 0.25 V, kēlā me kēia, ma ka pae alapine mai 1 105 a 0.1 Hz me ka amplitude o 5 mV. Ua hana hou ʻia nā hoʻāʻo kemika āpau ma ka liʻiliʻi he 3 mau manawa ma lalo o nā kūlana like e hōʻoia i ka hana hou ʻana o ka ʻikepili.
No nā ana HE-SXRD, ua ana ʻia nā poloka kila duplex rectangular e ana ana i ka 1 × 1 × 1.5 mm3 e helu i ka haku mele ʻana o ka beam phase o kahi wiggler ikehu kiʻekiʻe Brockhouse ma CLS, Kanada56. Ua hana ʻia ka hōʻiliʻili ʻikepili ma ke geometry Debye-Scherrer a i ʻole ke geometry hoʻoili ma ka mahana o ka lumi. ʻO ka nalu X-ray i hoʻoponopono ʻia me ka calibrator LaB6 he 0.212561 Å, e kūlike ana me 58 keV, ʻoi aku ka kiʻekiʻe ma mua o Cu Kα (8 keV) i hoʻohana pinepine ʻia ma ke ʻano he kumu X-ray hale hana. Aia ka laʻana ma kahi mamao o 740 mm mai ka mea ʻike. ʻO ka nui o ka ʻike o kēlā me kēia laʻana he 0.2 × 0.3 × 1.5 mm3, i hoʻoholo ʻia e ka nui o ka beam a me ka mānoanoa o ka laʻana. Ua hōʻiliʻili ʻia nā ʻikepili āpau me ka hoʻohana ʻana i kahi mea ʻike wahi Perkin Elmer, kahi mea ʻike X-ray panel pālahalaha, 200 µm pixels, 40 × 40 cm2 me ka hoʻohana ʻana i ka manawa hōʻike o 0.3 s a me 120 mau kiʻi.
Ua hoʻokō ʻia nā ana ʻana o X-PEEM o ʻelua mau ʻōnaehana hoʻohālike i koho ʻia ma ke kahua hopena Beamline MAXPEEM PEEM ma ka hale hana MAX IV (Lund, Sweden). Ua hoʻomākaukau ʻia nā laʻana ma ke ʻano like me nā ana electrochemical. Ua mālama ʻia nā laʻana i hoʻomākaukau ʻia i ka lewa no kekahi mau lā a ua hoʻohemo ʻia ke kinoea i loko o kahi keʻena vacuum ultrahigh ma mua o ka hoʻomālamalama ʻia ʻana me nā photons synchrotron. Ua loaʻa ka hoʻonā ikehu o ka laina kukuna ma ke ana ʻana i ka spectrum ion yield ma ka ʻāpana hoʻonāukiuki mai N 1 s a i 1\(\pi _g^ \ast\) kokoke i hv = 401 eV ma N2 me ka hilinaʻi o ka ikehu photon ma E3/2, 57. Ua hāʻawi nā spectra hoʻokokoke i ka ΔE (ka laulā o ka laina spectral) ma kahi o 0.3 eV ma ka pae ikehu i ana ʻia. No laila, ua manaʻo ʻia ka hoʻonā ikehu beamline ʻo E/∆E = 700 eV/0.3 eV > 2000 a me ka flux ≈1012 ph/s ma ka hoʻohana ʻana i kahi monochromator SX-700 i hoʻololi ʻia me kahi grating Si 1200-line mm−1 no ka lihi Fe 2p L2,3, ka lihi Cr 2p L2,3, ka lihi Ni 2p L2,3, a me ka lihi Ce M4,5. No laila, ua manaʻo ʻia ka hoʻonā ikehu beamline ʻo E/∆E = 700 eV/0.3 eV > 2000 a me ka flux ≈1012 ph/s ma ka hoʻohana ʻana i kahi monochromator SX-700 i hoʻololi ʻia me kahi grating Si 1200-line mm−1 no ka lihi Fe 2p L2.3, ka lihi Cr 2p L2.3, ka lihi Ni 2p L2.3, a me ka lihi Ce M4.5. Таким образом, энергетическое разрешение канала пучка было оценено как E/∆E = 700 эВ/0,3 эВ > 2000 и/10ф ≤ LIKE LIKE LIKE LIKE кромка Ce M4,5. No laila, ua manaʻo ʻia ka hoʻonā ikehu o ke kahawai kukuna e like me E/∆E = 700 eV/0.3 eV > 2000 a me ka flux ≈1012 f/s me ka hoʻohana ʻana i kahi monochromator SX-700 i hoʻololi ʻia me kahi grating Si o 1200 laina/mm no ka lihi Fe 2p L2,3, ka lihi Cr 2p L2.3, ka lihi Ni 2p L2.3, a me ka lihi Ce 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，通过使甉 1mm 1 mm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边缘和因此 ， 光束线 能量 分辨率 为 为 为 为 δe = 700 EV/0.3 EV> 2000 和 ≈1012 PH/S ， 使禔 ， 使禔1200 线 mm-1 光栅 改进 的 SX-700 单色器 于 于 于 用 用 用Fe 2p L2.3 边缘、Cr 2p L2.3 边缘、Cr 2p L2.3 边缘、Cr 2p L2.3 边边缘和Ce M4.5 边缘。No laila, i ka wā e hoʻohana ai i kahi monochromator SX-700 i hoʻololi ʻia me kahi grating Si laina 1200. 3, Cr edge 2p L2.3, Ni edge 2p L2.3 a me Ce edge M4.5.E scan i ka ikehu photon ma nā ʻanuʻu 0.2 eV. Ma kēlā me kēia ikehu, ua hoʻopaʻa ʻia nā kiʻi PEEM me ka hoʻohana ʻana i kahi mea ʻike TVIPS F-216 CMOS i hoʻopili ʻia me ka fiber me 2 x 2 bins, kahi e hāʻawi ai i kahi hoʻonā o 1024 x 1024 mau pikela ma kahi kahua ʻike 20 µm. ʻO ka manawa hōʻike o nā kiʻi he 0.2 s, me ka awelika o 16 mau kiʻi. Ua koho ʻia ka ikehu kiʻi photoelectron i ke ʻano e hāʻawi ai i ka hōʻailona electron lua kiʻekiʻe loa. Ua hana ʻia nā ana āpau ma ka hanana maʻamau me ka hoʻohana ʻana i kahi kukuna photon polarized linearly. Hiki ke loaʻa ka ʻike hou aku e pili ana i nā ana ma kahi noiʻi mua. Ma hope o ke aʻo ʻana i ke ʻano ʻike huina electron (TEY) a me kāna noi ma X-PEEM49, ua manaʻo ʻia ka hohonu hoʻāʻo o kēia ʻano ma kahi o 4-5 nm no ka hōʻailona Cr a ma kahi o 6 nm no Fe. Ua kokoke loa ka hohonu Cr i ka mānoanoa o ka ʻili oxide (~4 nm)60,61 ʻoiai ʻoi aku ka nui o ka hohonu Fe ma mua o ka mānoanoa. ʻO ka XRD i hōʻiliʻili ʻia ma ka lihi o FeL he hui ʻana ia o XRD o nā oxides hao a me Fe0 mai ka matrix. I ka hihia mua, ʻo ka ikaika o nā electrons i hoʻopuka ʻia mai nā ʻano electrons āpau e hāʻawi ana i ka TEY. Eia nō naʻe, pono ka hōʻailona hao maʻemaʻe i ka ikehu kinetic kiʻekiʻe no nā electrons e hele ma waena o ka papa oxide i ka ʻili a hōʻiliʻili ʻia e ka mea kālailai. I kēia hihia, ʻo ka hōʻailona Fe0 ma muli nui o nā electrons LVV Auger, a me nā electrons lua i hoʻopuka ʻia e lākou. Eia kekahi, ʻo ka ikaika TEY i hāʻawi ʻia e kēia mau electrons e palaho ana i ka wā o ke ala pakele electron, e hōʻemi hou ana i ka pane spectral Fe0 ma ka palapala ʻāina hao XAS.
ʻO ka hoʻohui ʻana i ka ʻeli ʻikepili i loko o kahi pahu ʻikepili (ʻikepili X-PEEM) kahi hana koʻikoʻi i ka unuhi ʻana i ka ʻike pili (nā waiwai kemika a kino paha) ma kahi ʻano multidimensional. Hoʻohana nui ʻia ka hui ʻana o K-means ma nā ʻano he nui, me ka ʻike mīkini, ka hana kiʻi, ka ʻike ʻano i nānā ʻole ʻia, ka naʻauao hana, a me ka nānā ʻana i ka hoʻokaʻawale ʻana. No ka laʻana, ua hana maikaʻi ka hui ʻana o K-means i ka hui ʻana i ka ʻikepili kiʻi hyperspectral. Ma ke kumumanaʻo, no ka ʻikepili multi-feature, hiki i ka algorithm K-means ke hoʻohui maʻalahi iā lākou ma muli o ka ʻike e pili ana i ko lākou mau ʻano (nā waiwai ikehu photon). ʻO ka hui ʻana o K-means kahi algorithm iterative no ka hoʻokaʻawale ʻana i ka ʻikepili i nā hui K non-overlapping (nā hui), kahi e pili ai kēlā me kēia pixel i kahi hui ma muli o ka hoʻolaha spatial o ka inhomogeneity kemika i loko o ka haku mele microstructural o ke kila. Loaʻa i ka algorithm K-means ʻelua mau pae: i ka pae mua, ua helu ʻia nā centroids K, a i ka pae ʻelua, ua hāʻawi ʻia kēlā me kēia kiko i kahi hui me nā centroids kokoke. Ua wehewehe ʻia ke kikowaena o ke koʻikoʻi o kahi hui ʻo ia ka awelika arithmetic o nā kiko ʻikepili (XAS spectrum) no kēlā hui. Aia nā mamao like ʻole e wehewehe i nā centroids kokoke e like me ka mamao Euclidean. No kahi kiʻi hoʻokomo o px,y (kahi ʻo x a me y ka hoʻonā ma nā pikela), ʻo CK ke kikowaena o ke koʻikoʻi o ka hui; a laila hiki ke hoʻokaʻawale ʻia kēia kiʻi (hui ʻia) i loko o nā hui K me ka hoʻohana ʻana iā K-means63. ʻO nā ʻanuʻu hope loa o ka algorithm clustering K-means:
KaʻAnuʻu Hana 2. E helu i ka lālā o nā pikela āpau e like me ke kikowaena o kēia manawa. No ka laʻana, ua helu ʻia mai ka mamao Euclidean d ma waena o ke kikowaena a me kēlā me kēia pikela:
KaʻAnuʻu Hana 3 E hāʻawi i kēlā me kēia pikela i ka centroid kokoke loa. A laila e helu hou i nā kūlana K centroid penei:
KaʻAnuʻu Hana 4. E hana hou i ke kaʻina hana (nā kaulike (7) a me (8)) a hiki i ka hui ʻana o nā centroids. Hoʻopili ikaika ʻia nā hopena maikaʻi o ka clustering hope loa me ke koho maikaʻi loa o nā centroids mua. No ka hoʻonohonoho ʻikepili PEEM o nā kiʻi kila, ʻo X (x × y × λ) ma ke ʻano maʻamau he cube o ka ʻikepili array 3D, ʻoiai ʻo nā axis x a me y e hōʻike ana i ka ʻike spatial (hoʻonā pixel) a ʻo ke axis λ e pili ana i kahi photon. kiʻi spectral ikehu. Hoʻohana ʻia ka algorithm K-means e ʻimi i nā wahi hoihoi i ka ʻikepili X-PEEM ma ka hoʻokaʻawale ʻana i nā pixels (nā hui a i ʻole nā ​​​​​​sub-blocks) e like me kā lākou mau hiʻohiʻona spectral a me ka unuhi ʻana i nā centroids maikaʻi loa (nā ʻikepili spectral XAS) no kēlā me kēia analyte. cluster). Hoʻohana ʻia ia e aʻo i ka hoʻolaha spatial, nā loli spectral kūloko, ke ʻano oxidation, a me nā kūlana kemika. No ka laʻana, ua hoʻohana ʻia ka algorithm clustering K-means no nā ʻāpana Fe L-edge a me Cr L-edge ma ka X-PEEM i hana wela ʻia a me ke anu. Ua hoʻāʻo ʻia nā helu like ʻole o nā hui K (nā ʻāpana o ka microstructure) e ʻike i nā hui kūpono a me nā centroids. Ke hōʻike ʻia kēia mau helu, ua hoʻololi hou ʻia nā pikela i nā centroids hui like. Pili kēlā me kēia hoʻolaha kala i ke kikowaena o ka hui, e hōʻike ana i ka hoʻonohonoho spatial o nā mea kemika a i ʻole nā ​​​​mea kino. ʻO nā centroids i unuhi ʻia he mau hui linear o nā spectra maʻemaʻe.
Loaʻa nā ʻikepili e kākoʻo ana i nā hopena o kēia haʻawina ma ke noi kūpono mai ka mea kākau WC pili.
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