Name: methods of ex situ and in situ investigations of structural transformations: the case of crystallization of metallic glasses
Uploaded: 2018-06-07T14:00:00
Description: Watch this Scientific Journal Video about Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses at JoVE.com

Dette arbejde blev støttet af den slovakiske forskning og udvikling agentur under kontrakter nr. APVV-16-0079, og APVV-15-0621, tilskud VEGA 1/0182/16 og VEGA 2/0082/17 og de interne IGA grant Palacky Universitet (IGA_PrF_2018_002). Vi er taknemmelige for R. Rüffer (ESRF, Grenoble) bistand med synkrotron eksperimenter.

1. forberedelse af en MG
Bemærk: For at vise en bred vifte af diagnosticeringsmuligheder af NFS i kombination med Mössbauer massespektrometri, en passende MG sammensætning var designet, nemlig (Fe3Co1)76Mo8Cu1B15 (at.%). Dette system viser magnetiske overgangen fra den ferromagnetiske til Paramagnetiske tilstand under udbruddet af krystallisering. Desuden crystallites, der opstår under trinnet første krystallisering danne bcc...

<ol>
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Ex situ Mössbauer effekten eksperimenter beskrive en stabil situation, som er stødt på i de undersøgte MG efter den anvendte varmebehandling. Hvert spektrum blev indsamlet i en periode på flere timer ved stuetemperatur. Således, udviklingen af den oprindeligt amorfe struktur blev efterfulgt som en funktion af udglødning betingelser. Fordi Mössbauer massespektrometri er følsomme over for hyperfine interaktioner handler på resonant atomkerner, kan svag detaljer af strukturelle og/eller magnetiske ændrin...

Jern-baserede MGs udarbejdet af hurtige quenching af en smelte repræsenterer industrielt attraktive materialer med mange praktiske anvendelser1. Især da deres magnetiske egenskaber er ofte bedre end konventionelle (poly) krystallinsk legeringer2,3. Til bedre udbytte af deres fordelagtige parametre, skal deres svar på forhøjede temperaturer være kendt. Med stigende temperatur, den amorfe struktur slapper, og endelig krystalliseringen starter. I nogle typer af MGs, kan dette føre til en forringelse af deres magnetiske parametre og dermed dårligere performance. Der er dog flere familier af jern-baserede MGs med særlige kompositioner4,5,6,7 , hvor de nydannede krystallinske korn er meget fine, typisk under omkring 30 nm i størrelse. Nanokrystaller stabilisere strukturen og således bevare acceptable magnetiske parametre over et bredt temperatur interval8,9. Disse er de såkaldte nanocrystalline legeringer (NCA).
Langsigtede ydeevne pålidelighed MGs, især under høje temperaturer og/eller hårde betingelser (ioniserende stråling, korrosion, osv.) kræver indgående kendskab til deres adfærd og individuelle fysiske parametre. Fordi MGs er amorf, er sortiment af analytiske teknikker, der er egnet til deres karakterisering ret begrænset. For eksempel, giver diffraktion metoder bred og konturløse refleksioner, der kan bruges kun til verifikation af amorphicity.
Det er bemærkelsesværdigt, at flere, normalt findes indirekte metoder som giver hurtig og ikke-destruktiv karakterisering af MGs (fx, magnetostrictive forsinkelse linje sensing princippet). Denne metode giver hurtig karakterisering af strukturelle og stress stater herunder tilstedeværelsen af inhomogeneities. Det var med fordel anvendes til hurtig og ikke-destruktiv karakterisering langs hele længden af MG bånd10,11.
Mere detaljeret indsigt i uordnede strukturelle arrangement kan opnås via hyperfine interaktioner, der nænsomt afspejler de lokale atomare arrangement af resonant atomer. Derudover kan variationer i topologisk og kemiske kortrækkende bestilling afsløres. I denne forbindelse, metoderne som Kernemagnetisk resonans (NMR) massespektrometri og/eller Mössbauer massespektrometri, begge udført på 57Fe kerner, bør betragtes som12,13. Mens den tidligere metode giver svar udelukkende til magnetisk dipol hyperfine interaktioner, er sidstnævnte også opmærksom på de elektriske Quadrupol interaktioner. Således gør Mössbauer massespektrometri samtidigt tilgængelige oplysninger på både strukturelle arrangement og magnetiske stater resonant jern kerner14.
Ikke desto mindre, for at opnå rimelig statistik, erhvervelse af en Mössbauer spektrum normalt tager flere timer. Denne begrænsning bør overvejes især når temperaturen-afhængige eksperimenter er planlagt. Forhøjede temperatur, der er anvendt under eksperimentet medfører strukturelle ændringer i de undersøgte MGs15. Derfor giver kun ex situ eksperimenter udført ved stuetemperatur på prøver, der var først udglødet ved visse temperatur og vendte derefter tilbage til omgivelsesbetingelserne pålidelige resultater.
Udviklingen i MG strukturer ved varmebehandlingen er rutinemæssigt undersøgt af analytiske teknikker, som aktiverer hurtig datafangst som f.eks X-ray diffraktion af synkrotron stråling (DSR), differential scanning kalorimetri (DSC), eller magnetiske målinger. Selvom i situ eksperimenter er muligt, vedrører de fremkomne oplysninger enten strukturelle (DSR, DSC) eller magnetisk (magnetiske) datafunktioner. DSC (og magnetiske målinger) er identifikation af typen (nano) kerner, der opstår under krystalliseringen ikke muligt. På den anden side angiver DSR data ikke de magnetiske stater af den undersøgte ordning. En løsning på denne situation er en teknik, der gør brug af hyperfine interaktioner: NFS synkrotron stråling16. Det tilhører en gruppe af metoder, der udnytter nukleare resonant spredning processer17. På grund af ekstremt høj glans af stråling stammer fra den tredje generation af synchrotrons, temperatur NFS blev eksperimenter under i situ betingelser muligt18,19,20,21 ,22,23.
Både Mössbauer massespektrometri og NFS er underlagt de samme fysiske principper relateret til nukleare resonans blandt energi niveauer af 57Fe kerner. Ikke desto mindre, mens de tidligere scanninger hyperfine interaktioner i domænet energi, sidstnævnte giver interferograms i domænet tid. På denne måde er resultaterne fra begge metoder tilsvarende og komplementære. For at evaluere data, NFS, skal være etableret en rimelig fysisk model. Denne udfordrende opgave kan udføres ved hjælp af Mössbauer SPEKTROMETRI, der giver den første skøn. Komplementaritet mellem disse to metoder betyder, at i situ NFS inspicerer flygtige stater og Mössbauer massespektrometri afspejler de stabile stater, nemlig oprindelige og/eller den endelige tilstand af et materiale studerede ex situ.
Denne artikel beskriver i detaljer udvalgte anvendelser af disse to mindre almindelige metoder til nukleare resonanser: her, vi anvender dem til undersøgelse af strukturelle ændringer, der opstår i en (Fe2,85Co1)77Mo8Cu1 B14 MG udsat for varmebehandling. Vi håber, at denne artikel tiltrækker interesse af forskere til at anvende disse metoder til undersøgelse af lignende fænomener og til sidst med forskellige typer af materialer.

<table border="0" cellpadding="0" cellspacing="0" width="728">
	<tbody>
		<tr height="30">
			<td height="30" style="height:30px;width:216px;">stable isotope, 57Fe</td>
			<td style="width:147px;">Isoflex USA</td>
			<td style="width:119px;">iron-57</td>
			<td style="width:247px;">metallic form</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">standard eletrolytic Fe, 99.95 %</td>
			<td style="width:147px;">Sigma Aldrich (Merck)</td>
			<td style="width:119px;">1.03819</td>
			<td>fine powder</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">electrolytic Co, 99.85 %</td>
			<td style="width:147px;">Sigma Aldrich (Merck)</td>
			<td style="width:119px;">1.12211</td>
			<td>fine powder</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">electrolytic Cu, 99.8 %</td>
			<td style="width:147px;">Sigma Aldrich (Merck)</td>
			<td style="width:119px;">1.02703</td>
			<td>fine powder</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">electrolytic Mo, 99.95 %</td>
			<td style="width:147px;">Sigma Aldrich (Merck)</td>
			<td style="width:119px;">1.12254</td>
			<td>fine powder</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">crystalline B, 99.95 %</td>
			<td style="width:147px;">Sigma Aldrich (Merck)</td>
			<td style="width:119px;">266620</td>
			<td>crystalline</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">calibration foil for M&#246;ssbauer spectrometry, bcc-Fe</td>
			<td style="width:147px;">GoodFellow</td>
			<td style="width:119px;">564-385-23</td>
			<td>foil 0.0125 mm, purity 99.85 %</td>
		</tr>
		<tr height="44">
			<td height="44" style="height:44px;width:216px;">HNO3 acid, ANALPURE Ultra</td>
			<td style="width:147px;">Analytika Praha, Czech Republic</td>
			<td style="width:119px;">UAc0061a</td>
			<td>concentration 67 %, volume 500 mL</td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">spectrometer for atomic absorption spectrometry</td>
			<td style="width:147px;">Perkin Elmer 1100, Germany</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="63">
			<td height="63" style="height:63px;width:216px;">spectrometer for optical emmission spectrometry with inductively coupled plasma</td>
			<td style="width:147px;">Jobin Yvon 70 Plus, France</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">X-ray diffractometer</td>
			<td style="width:147px;">Bruker D8 Advance, USA</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
		<tr height="42">
			<td height="42" style="height:42px;width:216px;">differential scanning calorimeter</td>
			<td style="width:147px;">Perkin Elmer DSC 7, Germany</td>
			<td style="width:119px;"></td>
			<td></td>
		</tr>
	</tbody>
</table>

methods of ex situ and in situ investigations of structural transformations: the case of crystallization of metallic glasses

Vi demonstrere brugen af to nukleare-baserede analytiske metoder, der kan følge ændringerne af mikrostrukturanalyse arrangement af jern-baserede metalliske briller (MGs). Trods deres amorfe art afslører identifikation af hyperfine interaktioner svage strukturelle ændringer. Til dette formål, har vi ansat to teknikker, der anvender nuklear resonans blandt nukleare niveauer af en stabil 57Fe isotop, nemlig Mössbauer massespektrometri og nukleare fremad spredning (NFS) af synkrotron stråling. Virkningerne af varmebehandling ved (Fe2,85Co1)77Mo8Cu1B14 MG diskuteres ved hjælp af resultaterne af ex situ og i situ eksperimenter, henholdsvis. Som begge metoder er følsomme over for hyperfine interaktioner, er oplysninger om strukturelle arrangement samt magnetiske mikrostruktur let tilgængelige. Mössbauer massespektrometri udført ex situ beskriver hvordan strukturelle arrangement og magnetiske mikrostruktur vises ved stuetemperatur efter udglødning under visse omstændigheder (temperatur, tid), og dermed denne teknik inspicerer støt Stater. På den anden side NFS data er indspillet i situ under dynamisk skiftende temperatur og NFS undersøger forbigående stater. Brugen af begge teknikker giver supplerende oplysninger. Generelt, kan de anvendes på enhver egnet system, hvor det er vigtigt at kende sin steady state men også forbigående stater.

XRD mønster i figur 2 udstiller bred konturløse diffraktion toppe. Den observerede refleksioner viser, at de producerede bånd (Fe2,85Co1)77Mo8Cu1B14 MG XRD amorfe.
På grund af dens følsomhed har XRD nogle begrænsninger i afsløringen overflade krystallisering. Tilstedeværelsen af crystallites beløber sig til mindre end omkring...

Watch this Scientific Journal Video about Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses at JoVE.com

Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

Vi præsenterer her, en protokol til at beskrive ex situ og i situ undersøgelser af strukturelle forandringer i metalliske briller. Vi ansat nukleare-baserede analytiske metoder, som inspicerer hyperfine interaktioner. Vi påvise anvendeligheden af Mössbauer massespektrometri og nukleare fremad spredning af synkrotron stråling under temperatur-drevet eksperimenter.

Metoder til Ex Situ og In Situ undersøgelser af strukturelle forandringer: sagen om krystallisering af metalliske briller

We demonstrate the use of two nuclear-based analytical methods that can follow the modifications of microstructural arrangement of iron-based metallic ...

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Methods of Ex Situ and In Situ Investigations of Structural Transformations: The Case of Crystallization of Metallic Glasses

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