Name: quantification of hydrogen concentrations in surface and interface layers and bulk materials through depth profiling with nuclear reaction analysis
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Description: Watch this Scientific Journal Video about Quantification of Hydrogen Concentrations in Surface and Interface Layers and Bulk Materials through Depth Profiling with Nuclear Reaction Analysis at JoVE.co

Vi sætter stor pris M. Matsumoto til gennemførelse af software, der gør det muligt at automatisk måling af NRA H dybde profiler ved fjernkontrol af MALT accelerator parametre fra datafangst PC. Vi takker K. Namba for dygtigt udfører Pd (110) prøve præparater og NRA og TDS målinger på BL-1E UHV-system, og C. Nakano til teknisk bistand i acceleratoren drift. Den SiO 2 / Si (100) prøven taknemmeligt modtaget som en høflighed af Z. Liu af NEC Corporation, Japan. Dette arbejde er delvist støttet af Grants-in-Støtte til videnskabelig forskning (Grant numre 24246013 og 26108705) af Japan Society for fremme af Science (JSP&#39;er), samt gennem en Grant-in-Aid for Videnskabelige Undersøgelser i Innovative områder &#39;Material design gennem Computics: Complex Korrelation og ikke-Equilibrium Dynamics&#39; fra Ministeriet for Undervisning, Kultur, Sport, Videnskab og Teknologi i Japan.

1. Planlægning af forsøg <ol><li> Identificer MALT accelerator stråle linje af interesse afhængigt af målingen opgave (BL-1E til overfladen brint, BL-2C for bulk eller grænsefladepolymerisering brint). Kontakt den assisterende videnskabsmand (aktuelt MW eller KF) for at drøfte detaljerne i den nationale tilsynsmyndighed målinger og deres nødvendige forberedelser. </li><li> Download en stråle tid ansøgningsskema og observere afleveringsfristen på MALT hjemmeside 31. Bemærk: MALT facilitet...

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Figur 4 viser den effektive skelnen og kvantificering overfladeaktivt adsorberes fra hovedparten-absorberet hydrogen gennem 15N NRA på eksemplet med en Pd (110) enkelt krystal i BL-1E UHV system. Den høje reproducerbarhed af overfladen H top i de tre profiler vidner om pålideligheden af in situ-fremstilling UHV prøven og til den ikke-destruktive karakter af NRA måling. Den kvantitative aftale af det fastslåede H dækning med den forventede atomare mætning tæthed yderligere vi...

Den allestedsnærværende af brint som en urenhed eller som bestanddel af et stort udvalg af materialer og det væld af brint-induceret interaktion fænomener gør afslører distribution af brint i nær-overflade-regionen og på nedgravede grænseflader faste stoffer en vigtig opgave i mange områder af teknik og grundlæggende materiale videnskab. Fremtrædende sammenhænge omfatter undersøgelser af brint absorption i lagring og rensning materialer til brint energi applikationer, brændselscelle, foto-, og hydrogenering katalyse, brint fastholdelse og sprødhed i nukleare og fusionsreaktor engineering, brint-induceret overfladeaktive effekter i epitaksial vækst fabrikation og hydrogen- relaterede elektrisk pålidelighed spørgsmål i halvleder-enhed teknologi. Trods sin allestedsnærværelse og enkel atomare struktur, kvantitativ påvisning af hydrogen udgør analytiske udfordringer. Da brint indeholder kun en enkelt elektron, ellers alsidige elementært analyser ved elektron spektroskopi gøres ineffektiv. Fælles brint påvisningsmetoder gennem masse analytiske, optiske, eller nukleare resonans teknikker såsom metallurgiske fusion, termisk desorption, infrarød absorption eller NMR-spektroskopi er hovedsagelig ufølsomme over for dybden placeringen af ​​brint. Dette udelukker fx skelne mellem overflade-adsorberet og bulk-absorberet brint som afviger væsentligt i deres fysiske og kemiske materielle vekselvirkninger, og deres skelnen bliver derfor stadig vigtigere for analysen af nanostrukturerede materialer, der omfatter små volumener og store flader. Hydrogen profilering af sekundær ion massespektroskopi, selv om at give dybde-løst kvantitative H koncentrationer, er lige så ødelæggende for det analyserede mål som metallurgiske fusion, og sputtering virkninger kan gøre information dybde opnået nær overfladen upålidelige. Kernereaktion analyse med den smalleenergi resonans (E res) af 1H (15 N, αγ) 12 C reaktionstemperatur på 6.385 MeV 1-3, på den anden side, kombinerer fordelene ved ikke-destruktiv hydrogen kvantificering med høj dybde opløsning i størrelsesordenen et par nanometer nær overfladen. Ved denne metode bestemmes overflade H dækningsområder med en følsomhed af størrelsesordenen 10 13 cm -2 (~ 1% af en typisk atomar monolag densitet). Hydrogenkoncentrationen i det indre af materialer kan vurderes med en detektionsgrænse på adskillige 10 18 cm -3 (~ 100 på. Ppm) og en pochedybde området fra ca. 2 um. Den nær overfladen dybde opløsning er rutinemæssigt 2-5 nm i overfladen-normal forekomst af de 15 N ion stråle på analyserede mål. I overfladeaktive græsning incidens geometrier, kan opløsningen blive yderligere forstærket til værdier under 1 nm. Se ref. 3 for en detaljeret redegørelse. Disse funktioner har vist 1 H ( <sop&gt; 15 N, αγ) 12 C NRA som en kraftfuld teknik til at belyse den statiske og dynamiske opførsel af hydrogen ved overflader og grænseflader i en lang række forskellige processer og materialer 3. Etableret af Lanford 4 i 1976, blev 15 N NRA først brugt overvejende kvantitativt bestemme volumen H koncentrationer i bulk materialer og tynde film. Blandt andre formål, har de absolutte brint koncentrationer opnået gennem 15N NRA blevet brugt til at kalibrere andre, som ikke er direkte kvantitative, brint detektionsteknikker 5,6. Også 15 N NRA brint profilering i mål med veldefinerede grænseflader i lagdelte tyndfilmstrukturer er blevet beskrevet 7-10. For nylig er der gjort store fremskridt i at studere brint i nær-overflade region af kemisk rene og strukturelt veldefinerede mål ved at kombinere 15N NRA med overfladen analytisk ultrahøj vakuum (UHV) instrumentering til prepare atomisk kontrollerede overflader i stedet for H-analyse 3. Ved at kvantificere brint dækning på enkelt krystal overflader, har NRA bidraget betydeligt til den aktuelle mikroskopiske forståelse af brint adsorption faser på mange materialer. 1H (15 N, αγ) 12 C NRA er endvidere den eneste eksperimentelle teknik til direkte at måle nul punkt vibrationsenergi af overfladeaktive adsorberet H-atomer 11, dvs., kan det afsløre kvantemekaniske vibrationsbevægelse af adsorberede H-atomer i retning af den indfaldende ionstrålen. Gennem evnen til diskrimination nanometer-skala mellem overflade-adsorberet og bulk-absorberede H, kan 15N NRA give værdifuld indsigt i brint indtrængen gennem materielle overflader, såsom relevante for mineralske hydrering dating 12 eller for at observere hydrid kernedannelse under overflader af H -absorberende metaller 13-15. High-resolution 15 N NTM applikationer har vist potentialet til at detektere sub-monolag variationer af adlayers 16 tykkelse og til at skelne overfladen adsorberes fra volumen-absorberet hydrogen i Pd nanokrystaller 17. Kombinationen med termisk desorption spektroskopi (TDS) giver mulighed for en entydig identifikation af H 2 termisk desorption funktioner og for dybden-løst vurdering af den termiske stabilitet af adsorberet og absorberet hydrogen stater mod desorption og diffusion 13,15,18. På grund af dets ikke-destruktive og høj dybdeopløsning 1H (15 N, αγ) 12 C NRA er også den ideelle metode til at detektere hydrogen begravet på intakte grænseflader, som giver mulighed for at studere hydrogen trapping på metal / metal 19-22 og metal / halvleder grænseflader 16,23-25 ​​og til sporing af brint diffusion i stablet tynd film systemer 9. Ved direkte at visualisere brint omfordeling fænomenen mellem grænseflader SiO 2 / Si-baserede metal-oxid-halvleder (MOS) strukturer, der vedrører elektriske nedbrydning enhed, har NRA gjort særligt værdifulde bidrag til enhedens pålidelighed forskning 26. Princippet hydrogenet detektion i NRA er at bestråle det analyserede mål med en 15 N ionstråle på mindst E res = 6.385 MeV at inducere resonant 1H (15 N, αγ) 12 C kernereaktion mellem 15 N og 1 H i materiale. Denne reaktion frigiver karakteristiske y-stråler af 4,43 MeV, der måles med en scintillationsdetektor i nærheden prøven. Den γ Yield er proportional med koncentrationen af ​​H i en vis dybde af målet. Normalisere dette signal med antallet af indfaldende 15 N ioner konverterer det til absolut H tæthed efter γ-detection system er kalibreret med en standard mål med kendt H-koncentration. 15 </sup&gt; N ioner hændelse på E res kan reagere med brint på målet overflade. Koncentrationen af begravede brint er målt med 15 N ioner hændelse ved energier (E i) over E res. Inde i målet materiale, lider de 15 N ioner energi tab på grund af elektronisk stop. Denne effekt giver den høje dybde opløsning, fordi 1H (15 N, αγ) 12 C kernereaktion resonans har en meget smal bredde (Lorentz bredde parameter Γ = 1,8 keV) og stoppeevne af materialer til 6,4 MeV 15 N intervaller mellem 1-4 keV / nm, således at passagen af 15N ion gennem kun nogle få atomare lag er tilstrækkelig til at forskyde sin energi uden for resonans vinduet. , Den resonante reaktion registrerer således begravet H ved E i&gt; E res i en sonderende dybde d = (E i - E res) / S, hvor S er den elektroniskestandse strømmen af det analyserede materiale 3. Ved at måle γ-udbytte under scanning hændelsen 15N ionenergi i små trin, opnår man en kernereaktion excitationskurve der indeholder tætheden dybtgående fordeling af hydrogen i målet. I denne excitation kurve (γ-udbytte vs. 15N energi), er det faktiske H dybde fordeling foldet med NRA instrumental funktion, der tilføjer en overvejende Gauss udvidelse og er den vigtigste begrænsning for dybden resolution 3. Ved overfladen (dvs. ved E i = E res) den gaussiske bredde er domineret af en Doppler-effekten på grund af nul-punkt vibration af H-atomer mod måloverfladen. 11,27,28 Kurven af begravede hydrogen udbytte detekteret ved E i&gt; E res påvirkes af en ekstra Gauss udvidelse komponent på grund af tilfældige 15 N ion energi straggling inde i målet. De tjavset bredde øges proportionalt med kvadratroden af den ion bane længde i materialet 29,30 og bliver den dominerende resolution begrænsende faktor over sondering dybder på 10-20 nm. For at demonstrere et par meget typiske brint profilering applikationer med 15 N NRA, vi her eksemplarisk beskrive (1) den kvantitative evaluering af overfladen H dækning og af bulk-absorberet koncentrationen af hydrogen i et H2 udsat palladium (Pd) enkeltkrystal, og (2) evaluering af dybde placering og brint lag tætheder på begravede grænseflader SiO 2 / Si (100) stakke. NRA Målingerne udføres ved MALT 5 MV van-de-Graaf tandem accelerator 31 fra University of Tokyo, der leverer en meget stabil og godt monochromatized (AE i ≥ 2 keV) 15 N ion stråle af 6-13 MeV. Forfatterne har udviklet en computer kontrol system til accelerateller for at gøre det muligt for automatiseret energi scanning og datafangst for brint profilering. Afspejler de to forskellige nationale tilsynsmyndigheder måleopgaver præsenteret af de ovennævnte H profilering applikationer, den MALT facilitet giver to ion stråle linjer med specialiserede eksperimentelle stationer: (1) en UHV overflade analytisk system med en enkelt bismuth germanate (BGO, Bi 4 Ge 3 O 12 ) γ-scintillationsdetektor dedikeret til NRA kvantificering af brint overflade dækningsområder, til nul-punkt vibrationer spektroskopi, og til H dybde profilering på atomisk kontrollerede enkelt krystal mål i en unik kombination med TDS; og (2) en høj vakuumkammer udstyret med to BGO detektorer placeret meget tæt på målet for øget γ-detektion effektivitet, hvilket giver en lavere H detektionsgrænse og erhvervelse hurtigere data. Denne opsætning har ingen prøveforberedelse faciliteter, men giver mulighed for hurtig prøve udveksling (~ 30 min) og dermed en højere overførselshastighed på mål for, hvor et godt controlled overfladelag ikke er en væsentlig del af den analytiske opgave, såsom H profilering på nedgravede grænseflader eller kvantificering af bulk-H koncentrationer. På begge beam linjer er de BGO detektorer placeres bekvemt uden for vakuumsystemer fordi y-stråler trænger de tynde kammervægge med ubetydelig dæmpning. <img alt="figur 1" src="/files/ftp_upload/53452/53452fig1.jpg" /> Figur 1. NRA setup i BL-1E UHV-system. (A) Skematisk ovenfra ind i BL-1E UHV-system udstyret med sputter ion pistol, lav energi elektron diffraktion (LEED), og Auger elektron spektroskopi (AES) til i -situ udarbejdelse af atomisk bestilt og kemisk rene enkelt krystal overflade mål og kombineret NRA og TDS målinger med en kvadrupolmassespektrometer (QMS) monteret på en lineær oversættelse scene. (B) Pd monokrystallinske model vedlagt på than prøve indehaver af den kryogene manipulator. <a href="https://www.jove.com/files/ftp_upload/53452/53452fig1large.jpg" target="_blank">Klik her for at se en større version af dette tal.</a> Figur 1 (A) illustrerer UHV systemet på strålelinie (BL) -1e, som er fuldt udstyret til in-situ-fremstilling af atomisk bestilt monokrystallinske overflader og har en basis tryk &lt;10 -8 Pa at opretholde overflade renlighed. At tilvejebringe prøve adgang for overfladeaktive analytiske værktøjer, er 4 &quot;BGO scintillator placeret på 15 N ion beam akse ~ 30 mm bag målet. Prøven er monteret på en 4-akset manipulation fase til præcis (x, y, z, Θ) positionering og kan køles med flydende nitrogen til ~ 80 K eller med komprimeret Han til ~ 20 K. Figur 1 (B) viser et Pd enkelt krystal target monteret ved punktsvejset Ta support ledninger til en He komprimering kryostat. Quartz ark afstandsstykker isolere Sampl<html> e Holdeplade elektrisk fra kryostat krop. Dette gør det muligt hændelsen 15N ionstrålestrøm måling nødvendig for kvantitativ NRA og giver mulighed for elektron bombardement opvarmning fra glødetråd wolfram på bagsiden af holderen prøven. En type K termoelement er punktsvejset til kanten af ​​Pd prøven. En kvartsplade fastgjort på manipulatoren akse over prøven anvendes til at overvåge ionstrålen profil og for prøve-lyshøjden. Figur 2 (A) viser opsætningen på BL-2C med to 4 &quot;BGO detektorer anbragt ved 90 ° i forhold til 15 N stråle med deres forflade ikke videre end 19,5 mm fra stråleaksen. Prøveholderen (Figur 2 (B)) giver en enkel klemmemekanisme til hurtig prøve udveksling og muliggør drejning af prøven omkring den vertikale akse at justere 15N indfaldsvinklen. Iles / ftp_upload / 53.452 / 53452fig2.jpg &quot;/&gt; Figur 2. NRA setup på BL-2C. (A) Skematisk ovenfra ind i højvakuum kammeret ved BL-2C udstyret med to BGO y-detektorer tæt til målpositionen. (B) Prøve holder med en stor chip mål på SiO 2 / Si (100) fastspændt på. Dug op denne prøvetype med vanddamp efter NRA analyse visualiserer de pletter, der blev bestrålet med den 15 N ion stråle. <a href="https://www.jove.com/files/ftp_upload/53452/53452fig2large.jpg" target="_blank">Klik her for at se en større version af dette tal.</a>

<table>
	<tbody>
		<tr>
			<td>Pd single crystal&#160;</td>
			<td>SPL (Surface Preparation Laboratory), http://www.spl.eu/products.html, or any other suitable supplier</td>
			<td>Order made to specification</td>
			<td>Disk, 9 mm diam., (110) oriented, aligned to &#60; 0.5 degree or less, one side polished to &#60; 0.3 mm roughness, self-prepared specimen&#160;</td>
		</tr>
		<tr>
			<td>H2 gas</td>
			<td>Joutou Gas Corporation, Ltd., Japan, http://www.jyotougas.co.jp/item/gas.html</td>
			<td></td>
			<td>(99.9995%), or any other suitable supplier</td>
		</tr>
		<tr>
			<td>O2 gas</td>
			<td>Joutou Gas Corporation, Ltd., Japan, http://www.jyotougas.co.jp/item/gas.html</td>
			<td></td>
			<td>(99.99%), or any other suitable supplier</td>
		</tr>
		<tr>
			<td>Ar gas</td>
			<td>Joutou Gas Corporation, Ltd., Japan, http://www.jyotougas.co.jp/item/gas.html</td>
			<td></td>
			<td>(99.99995%), or any other suitable supplier</td>
		</tr>
		<tr>
			<td>Tantalum / Wire</td>
			<td>The Nilaco Corporation, http://nilaco.jp/en/order.php</td>
			<td>TA-411325</td>
			<td>(99.95%), 0.3 mm diam., or any other suitable supplier</td>
		</tr>
		<tr>
			<td>Alumel / Wire&#160;</td>
			<td>The Nilaco Corporation, http://nilaco.jp/en/order.php</td>
			<td>851266</td>
			<td>0.2 mm diam., or any other suitable supplier</td>
		</tr>
		<tr>
			<td>Chromel / Wire (Chromel)</td>
			<td>The Nilaco Corporation, http://nilaco.jp/en/order.php</td>
			<td>861266</td>
			<td>0.2 mm diam., or any other suitable supplier</td>
		</tr>
	</tbody>
</table>

quantification of hydrogen concentrations in surface and interface layers and bulk materials through depth profiling with nuclear reaction analysis

Kernereaktion analyse (NRA) via resonant 1H (15 N, αγ) 12 C reaktion er en meget effektiv metode til dybde profilering, der kvantitativt og ikke-destruktivt afslører hydrogen massefylde fordelingen ved overflader, ved grænseflader, og i mængden af faste materialer med høj dybde opløsning. Teknikken anvendes en 15 N ionstråle af 6.385 MeV leveret af en elektrostatisk accelerator og specifikt detekterer 1H isotop i dybder på op til ca. 2 um fra måloverfladen. Overflade H dækningsområder måles med en følsomhed af størrelsesordenen ~ 10 13 cm -2 (~ 1% af en typisk atomar monolag densitet) og H volumen fusioner af detektionsgrænse på ~ 10 18 cm -3 (~ 100 ved. Ppm ). Den nær overfladen dybde opløsning er 2-5 nm for overfladen-normal 15 N ion forekomst på målet og kan forbedres til værdier under 1 nm for meget flade mål ved vedtaTing en overflade-græsning forekomst geometri. Fremgangsmåden er alsidig og let anvendes på enhver højvakuum kompatibel homogent materiale med en glat overflade (ingen porer). Elektrisk ledende mål sædvanligvis tolerere ionstrålen bestråling med ubetydelig nedbrydning. Hydrogen kvantificering og korrekte dybde analyse kræver kendskab til den elementære sammensætning (udover brint) og masse densiteten af ​​målmaterialet. Især i kombination med ultra-høje vakuum metoder til in-situ target forberedelse og karakterisering, 1H (15 N, αγ) 12 C NRA er ideel til brint analyse på atomisk styrede overflader og nanostrukturerede grænseflader. Vi eksemplarisk demonstrerer her anvendelse af 15N NRA på MALT Tandem accelerator facilitet fra University of Tokyo til (1) kvantitativt måle overfladen dækning og hovedparten koncentration af brint i nær-overflade region af en H2 udsat Pd(110) enkeltkrystal, og (2) at bestemme dybden placering og lag tæthed af hydrogen nær grænseflader tynde SiO2 film på Si (100).

Figur 4 viser nær overfladen NRA H profiler af H2 -exposed Pd (110) målt i BL-1E UHV system på en stikprøve på 90 K under en H2 baggrund tryk på 1,33 x 10 -6 Pa. De 15 N ion forekomst energi er blevet omdannet til pochedybde hjælp af bremseevne Pd (S = 3,90 keV / nm). Den åbne symbol profil blev opnået efter præ-udsætte Pd (110) prøve til 2.000 LH 2 ved 145 K til at inducere absorptionen af hydro...

Watch this Scientific Journal Video about Quantification of Hydrogen Concentrations in Surface and Interface Layers and Bulk Materials through Depth Profiling with Nuclear Reaction Analysis at JoVE.co

Quantification of Hydrogen Concentrations in Surface and Interface Layers and Bulk Materials through Depth Profiling with Nuclear Reaction Analysis

Vi illustrere anvendelsen af 1H (15 N, αγ) 12 C resonant kernereaktion analyse (NRA) for kvantitativt at evaluere densiteten af hydrogenatomer på overfladen, i volumenet, og ved en grænsefladelag af faste materialer. Den nær overfladen brint dybde profilering af en Pd (110) enkelt krystal og SiO 2 / Si (100) stakke beskrives.

Kvantificering af Hydrogen Koncentrationer i Surface og Interface-Lag og Bulk Materials gennem Dybde Profilering med kernereaktion Analysis

Nuclear reaction analysis (NRA) via the resonant 1H(15N,&#945;&#947;)12C reaction is a highly effective method of depth profiling that quantitatively and ...

The overall goal of nuclear reaction analysis with the resonant 15 nH nuclear reaction is to measure the density of absorbed hydrogen atoms on solid surfaces, and to determine the concentration versus depth distribution of absorbed hydrogen in the volume of materials. Clarifying the hydrogen content on surfaces, in the near surface region, and at shallow interfaces of solids is a key question in many fields of fundamental material science and engineering. The main advantage of nuclear reaction analysis is that it reveals the concentration and depth location of hydrogen quantitatively, nondestructively, and with nanometer depth resolution.Hydrogen profiling with NRA supports research of hydrogen storage and purification materials. Fuel cell and hydrogenation catalysts, hydrogen retention and embrittlement, device fabrication and hydrogen-related reliability concerns in semi-conducted technology. In this video, we demonstrate a unique combination of NRA with surface science instrumentation for the quantification of a hydrogen-layered densities on atomically-controlled target surfaces and at shallow interfaces.These nuclear reaction analysis experiments take place at the University of Tokyo's MALT accelerator facility. Measurements of surface hydrogen are done on beam line 1E in this ultra-high vacuum chamber. This chamber has been loaded with a palladium 110 single crystal sample and is held at less than 10 nanopascals at room temperature.This top view schematic of the sample chamber gives an overview of the equipment layout. The nitrogen ion beam line including a deflector and a Faraday cup comes in at the left. In addition, there is an ion gun for sputtering as well as an input for hydrogen.The chamber is equipped to perform low energy electron diffraction and Auger electron spectroscopy for INC2 preparation of targets. The final two instruments are quadrupole mass spectrometer shown at the bottom of the schematic and a scintillation detection system at the right. The sample is held by a sample holder on an XYZ stage near the center of the chamber and can be viewed through a viewport.This picture provides an example of the sample holder with a sample that is currently in the chamber. Tantalum wires support a single crystal specimen. The holder also facilitates electrical and thermal measurements.Begin with cleaning the target surface in the chamber through sputtering and annealing. Operate the XYZ stage to position the sample in the center of the chamber. In addition, rotate the sample to properly align it.The sample should face the gas doser between the ion gun and the viewport. To fine adjust the angle, turn on the ion gun power supply. Adjust emission control to 20 milliamps.Observe the sample through the viewport while fine adjusting its angle. The goal is to have the mirror image of the ion gun filament visible on the sample surface. Once fine adjustment is complete, change the ion gun power supply setting for the beam energy to 800 electron volts.Next, at the bottom of the chamber, close the NEG pump gate valve. Use a variable leak valve to introduce 9 millipascal argon gas into the chamber. For sputter ion current reading, consult the digital tester connected between the sample and ground.Confirm that the current is around two microamps for the 10-minute duration of the sputter. Stop the sputtering by closing the variable leak valve and turning off the ion gun power supply. Continue preparations by bringing liquid nitrogen to the manipulator and adding about 100 milliliters to the cryostat.Stay at the manipulator to make electrical connections for annealing. Connect the filament heater lids to the heater power supply. Also, connect the thermocouple feedthrough to a digital tester to monitor the temperature.Ground the filament by connecting it to the chamber body. Finally, connect the sample contact to the bias voltage power supply. At this point, set up the high voltage power supply.Apply a sample bias of one kilovolt. Proceed to anneal the sample at 1, 000 Kelvin and oxidize it at 750 Kelvin. After annealing and oxidation, prepare to do low energy electron diffraction on the sample.Observe the diffraction pattern and look for a clear structure with bright spots and low background noise as in this example. Be prepared to repeat the sputtering, annealing, oxidation, and reduction steps as necessary. The next step is to align the nitrogen ion beam to the single crystal target for nuclear reaction analysis.Center the sample in the XY plane and adjust the Z position to the height of the mass spectrometer front aperture. Rotate the sample back to face the beam line. Next, lower the sample holder to put the beam profile monitor into position for nuclear reaction analysis.Set a camera on the window flange to transmit beam profile images to the control room. Return to the manipulator and remove all electrical contacts to the sample. After this, attach the sample current line.Now, prepare for introducing the ion beam. Set the electrostatic deflector voltage on the beam line to 8, 500 volts. Enter the control room to continue.There, switch the current integrator from standby mode to operate. This schematic represents a portion of the accelerator beam line before the ion beam is stirred to the different experiment beam lines. The experiment beam lines are also represented.There are four components that are important for this protocol. BM03 is a 90-degree sector magnet. It selects the ion beam energy during depth profiling.FC04 is a Faraday cup that can be inserted into the beam to read the ion beam current and prevent the beam from reaching the sample. MQ04 is a magnetic quadrupole lens used to focus the beam onto the sample. And BM04 is a bending magnet that directs the beam into the beam lines.Take steps to adjust the ion beam energy and direct the beam onto the target in the vacuum chamber. Set the MQ04 magnetic quadrupole lens, XCC and the YCC lens parameters to approximately focus the beam. Open the gate valves between the accelerator and the beam line and then open the Faraday cup, FC04.Use the monitor to observe the ion beam profile on the quart's plate in the target chamber. With this feedback, fine-tune the bending magnet, BM04 and the magnetic quadrupole lens settings. The goal is to obtain a well-focused ion beam in the center of the profile monitor plate.Close the Faraday cup and record the parameters before returning to the beam line. Back on beam line 1E, use the filament heater to flash heat the palladium sample to 600 Kelvin then set the filament heater to about 3.6 amps to maintain the sample temperature at 145 Kelvin. Isolate the chamber from the accelerator and NEG pump before exposing the sample to 2, 000 langmuirs of hydrogen at 145 Kelvin.Turn off the filament heater and when the temperature reaches 80 Kelvin, adjust the hydrogen background pressure to be one micropascal. Back in the control room, arrange for the nitrogen ion beam to have the desired starting energy. For this experiment, ensure that Faraday cup 04 registers a beam current of 10 to 20 nanoamps.Next, enter the parameters for the energy scan and the acquisition time into the control software before starting automated data acquisition. These are typical parameter values for BM03 to control the energy scan. Values are given for selecting the initial energy, the final energy, and the change in energy with each step.The acquisition time is 50 seconds. Measurements of bulk and interface hydrogen are done on beam line 2C. This manipulator has been removed from the beam line and is ready with a new sample in the sample holder.For these measurements, the sample is a thin film of silicon dioxide on a silicon 100 surface. With the sample aligned parallel to the transfer tube access, tighten the clamp screws to secure it in place. Retract the sample into the transfer tube and secure it with a locking screw.Move the manipulator to its position on the beam line and reinstall it on the gate valve. When the system is ready, lower the sample into position for the NRA measurement. As in this schematic, align the sample surface normal to the incident beam.Use a beam line camera and monitor for this purpose. At the manipulator head, connect the sample current line to the control room current integrator. Move to the control room to continue.Coursely align the beam by setting the bending magnet and the magnetic quadrupole lens parameters. Observe the beam profile on the profile monitor while further optimizing the parameters for beam transmission and keeping the profile on target. Next, set the BM03 parameter to determine the starting beam energy for the scan.At the computer, enter the desired parameters for the energy scan and start the automated scan of energy to acquire a depth profile. This near surface depth profile is from single crystal palladium that has had its 110 surface exposed to hydrogen gas. The experiment was performed in beam line 1E with a hydrogen background pressure of 1.3 micropascals.The bottom horizontal axis gives the nitrogen ion beam energy. The top axis provides a measure of the depth based on the stopping power of palladium. The open symbols correspond to an experiment with palladium that was pre-exposed in 100 seconds to 2, 000 langmuirs of hydrogen gas at 145 Kelvin.The data were taken at 90 Kelvin. The profile can be decomposed into a peak at depth zero in black and a plateau in blue. The area of the peak provides information on hydrogen surface density.In this case, the coverage is 1 1/2 hydrogens per surface palladium atom. The plateau reveals that hydrogen has been absorbed to a depth of at least 20 nanometers. The gray and black symbols are for experiments with no pre-dosage of hydrogen.These data were taken at 170 Kelvin. These plots represent data from a series of experiments with silicon dioxide on silicon performed in beam line 2C. As before, the ion energy is shown on the bottom axis.The depth along the top. The positions of the interface between the materials is indicated by a vertical dashed line. All profiles show two peaks indicating a non-uniform distribution of hydrogen including hydrogen just a few nanometers in front of the silicon oxide silicon interface.The experiments in this video demonstrate that the NRA technique can distinguish surface-absorbed and volume or interface-absorbed hydrogen in solid targets. NRA furthermore quantifies the hydrogen content at their respective depth locations without destroying the sample material. Please be aware that especially the temperature and pressure during hydrogen exposure, very critically influence the depth distribution of palladium-absorbed hydrogen.If these experimental parameters are changed, hydrogen profile is different from those shown in this video will likely result. After watching this video, you should have a good impression of how nuclear reaction analysis measurement is performed at MALT facility to quantitatively determine hydrogen densities on surfaces and in the interior of solid materials through nanoscale depth profile.

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Simultan multi overflade Anodizations og trappe-lignende Reverse bias udstationering af anodisk aluminium oxider i svovlsyre og oxalsyre elektrolyt

After reporting on the two-step anodization, nanoporous anodic aluminum oxides (AAOs) have been widely utilized in the versatile fields of fundamental ...

In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure

In Situ High Pressure Hydrogen Tribological Testing of Common Polymer Materials Used in the Hydrogen Delivery Infrastructure

In Situ Højt tryk brint tribologiske afprøvning af fælles Polymer materialer i brint levering infrastruktur

High pressure hydrogen gas is known to adversely affect metallic components of compressors, valves, hoses, and actuators. However, relatively little is ...

Processing of Bulk Nanocrystalline Metals at the US Army Research Laboratory

Behandling af Bulk Nanocrystalline metaller ved US Army Research Laboratory

Given their potential for significant property improvements relative to their large grained counterparts, much work has been devoted to the continued ...

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

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

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 ...

Bulk and Thin Film Synthesis of Compositionally Variant Entropy-stabilized Oxides

Bulk og tynd Film syntese af kompositorisk Variant entropi-stabiliseret oxider

Here, we present a procedure for the synthesis of bulk and thin film multicomponent (Mg0.25(1-x)CoxNi0.25(1-x)Cu0.25(1-x)Zn0.25(1-x))O (Co variant) and ...