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Fabrication of Atom Probe Tomography Specimens from Nanoparticles Using a Fusible Bi–In–Sn Alloy as an Embedding Medium

Published online by Cambridge University Press:  04 February 2019

Se-Ho Kim ,
Ji Yeong Lee ,
Jae-Pyoung Ahn  and
Pyuck-Pa Choi
Se-Ho Kim
Affiliation:
Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology (KAIST), 291 Daehak-ro, Yuseong-gu, Daejeon 34141, Republic of Korea
Ji Yeong Lee
Affiliation:
Advanced Analysis Center, Korea Institute of Science and Technology (KIST), Seoul 136-791, Republic of Korea
Jae-Pyoung Ahn
Affiliation:
Advanced Analysis Center, Korea Institute of Science and Technology (KIST), Seoul 136-791, Republic of Korea
Pyuck-Pa Choi*
Affiliation:
Department of Materials Science and Engineering, Korea Advanced Institute of Science and Technology (KAIST), 291 Daehak-ro, Yuseong-gu, Daejeon 34141, Republic of Korea
*
*Author for correspondence: Pyuck-Pa Choi, E-mail: p.choi@kaist.ac.kr
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Abstract

We propose a new method for preparing atom probe tomography specimens from nanoparticles using a fusible bismuth–indium–tin alloy as an embedding medium. Iron nanoparticles synthesized by the sodium borohydride reduction method were chosen as a model system. The as-synthesized iron nanoparticles were embedded within the fusible alloy using focused ion beam milling and ion-milled to needle-shaped atom probe specimens under cryogenic conditions. An atom probe analysis revealed boron atoms in a detected iron nanoparticle, indicating that boron from the sodium borohydride reductant was incorporated into the nanoparticle during its synthesis.

Keywords

atom probe tomographyfusible alloynanoparticles
Type
Instrumentation and Experimental Methodology
Information
Microscopy and Microanalysis , Volume 25 , Special Issue 2: Atom Probe Tomography and Microscopy APT&M 2018 , April 2019 , pp. 438 - 446
Copyright
Copyright © Microscopy Society of America 2019 

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References

Berlin, J (2011). Analysis of boron with energy dispersive spectrometry. Imaging Microsc 13, 19–21.Google Scholar
Cento, C, Gislon, P and Prosini, PP (2009). Hydrogen generation by hydrolysis of NaBH4. Int J Hydrogen Energy 34, 4551–4554.Google Scholar
Demirci, UB and Miele, P (2010). Cobalt in NaBH4 hydrolysis. Phys Chem Chem Phys 12, 14651. http://xlink.rsc.org/?DOI=c0cp00295j.Google Scholar
Devaraj, A, Colby, R, Vurpillot, F and Thevuthasan, S (2014). Understanding atom probe tomography of oxide-supported metal nanoparticles by correlation with atomic-resolution electron microscopy and field evaporation simulation. J Phys Chem Lett 5, 1361–1367.Google Scholar
de Resende, VG, De Grave, E, da Costa, GM and Janssens, J (2007). Influence of the borohydride concentration on the composition of the amorphous Fe–B alloy produced by chemical reduction of synthetic, nano-sized iron-oxide particles. Part I: Hematite. J Alloys Compd 440, 236–247.Google Scholar
Eley, C, Li, T, Liao, F, Fairclough, SM, Smith, JM, Smith, G and Tsang, SCE (2014). Nanojunction-mediated photocatalytic enhancement in heterostructured CdS/ZnO, CdSe/ZnO, and CdTe/ZnO nanocrystals. Angew Chem: Int Ed 53, 7838–7842.Google Scholar
Felfer, P, Benndorf, P, Masters, A, Maschmeyer, T and Cairney, JM (2014). Revealing the distribution of the atoms within individual bimetallic catalyst nanoparticles. Angew Chem: Int Ed 53, 11190–11193.Google Scholar
Felfer, P, Li, T, Eder, K, Galinski, H, Magyar, AP, Bell, DC, Smith, GDW, Kruse, N, Ringer, SP and Cairney, JM (2015). New approaches to nanoparticle sample fabrication for atom probe tomography. Ultramicroscopy 159, 413–419.Google Scholar
Folcke, E, Lardé, R, Le Breton, JM, Gruber, M, Vurpillot, F, Shield, JE, Rui, X and Patterson, MM (2012). Laser-assisted atom probe tomography investigation of magnetic FePt nanoclusters: First experiments. J Alloys Compd 517, 40–44. http://dx.doi.org/10.1016/j.jallcom.2011.11.134.Google Scholar
Fu, F, Dionysiou, DD and Liu, H (2014). The use of zero-valent iron for groundwater remediation and wastewater treatment: A review. J Hazard Mater 267, 194–205.Google Scholar
Galiana, B, Oprea, B, Huttel, Y and Ballesteros, C (2014). Synthesis and characterization of Fe–B nanoparticles for potential magnetic applications. J Mater Sci: Mater Electron 25, 659–663.Google Scholar
Gault, B (2016). A brief overview of atom probe tomography research. Appl Microsc 46, 117–126. http://www.appmicro.org/journal/view.html?doi=10.9729/AM.2016.46.3.117.Google Scholar
Glavee, GN, Klabunde, KJ, Sorensen, CM and Hadjipanayis, GC (1995). Chemistry of borohydride reduction of iron(II) and iron(III) ions in aqueous and nonaqueous media. Formation of nanoscale Fe, FeB, and Fe2B powders. Inorg Chem 34, 28–35.Google Scholar
Gnaser, H (2014). Atom probe tomography of nanostructures. Surf Interface Anal 46, 383–388.Google Scholar
Heck, PR, Stadermann, FJ, Isheim, D, Auciello, O, Daulton, TL, Davis, AM, Elam, JW, Floss, C, Hiller, J, Larson, DJ, Lewis, JB, Mane, A, Pellin, MJ, Savina, MR, Seidman, DN and Stephan, T (2014). Atom-probe analyses of nanodiamonds from Allende. Meteorit Planet Sci 49, 453–467.Google Scholar
Huber, DL (2005). Synthesis, properties, and applications of iron nanoparticles. Small 1, 482–501.Google Scholar
Hyeon, T, Lee, SS, Park, J, Chung, Y and Na, HB (2001). Synthesis of highly crystalline and monodisperse maghemite nanocrystallites without a size-selection process. J Am Chem Soc 123, 12798–12801.Google Scholar
Kim, S-H and Choi, P-P (2017). Enhanced Congo red dye removal from aqueous solutions using iron nanoparticles: Adsorption, kinetics, and equilibrium studies. Dalton Trans 46, 15470–15479. http://dx.doi.org/10.1039/C7DT02076G.Google Scholar
Kim, S-H, Kang, PW, Park, OO, Seol, J-B, Ahn, J-P, Lee, JY and Choi, P-P (2018). A new method for mapping the three-dimensional atomic distribution within nanoparticles by atom probe tomography (APT). Ultramicroscopy 190, 30–38. http://linkinghub.elsevier.com/retrieve/pii/S0304399117304965.Google Scholar
Kuchibhatla, SVNT, Shutthanandan, V, Prosa, TJ, Adusumilli, P, Arey, B, Buxbaum, A, Wang, YC, Tessner, T, Ulfig, R, Wang, CM and Thevuthasan, S (2012). Three-dimensional chemical imaging of embedded nanoparticles using atom probe tomography. Nanotechnology 23, 215704. http://stacks.iop.org/0957-4484/23/i=21/a=215704?key=crossref.48c33fd57ee74bada321684fa3bb082f.Google Scholar
Larson, DJ, Giddings, AD, Wu, Y, Verheijen, MA, Prosa, TJ, Roozeboom, F, Rice, KP, Kessels, WMM, Geiser, BP and Kelly, TF (2015). Encapsulation method for atom probe tomography analysis of nanoparticles. Ultramicroscopy 159, 420–426.Google Scholar
Larson, D, Prosa, T and Kelly, T (2013). Local Electrode Atom Probe Tomography—A user's guide. http://link.springer.com/content/pdf/10.1007/978-1-4614-8721-0.pdf.Google Scholar
Lee, JK, Ann, HH, Yi, Y, Lee, KW, Uhm, S and Lee, J (2011). A stable Ni–B catalyst in hydrogen generation via NaBH4 hydrolysis. Catal Commun 16, 120–123.Google Scholar
Lewis, JB, Isheim, D, Floss, C, Daulton, TL and Seidman, DN (2016). Analysis of Allende nanodiamond residue by correlated transmission electron microscopy and atom-probe tomography. Lunar Planet Sci Conf 47, 2248.Google Scholar
Li, H, Wu, Y, Luo, H, Wang, M and Xu, Y (2003). Liquid phase hydrogenation of acetonitrile to ethylamine over the Co–B amorphous alloy catalyst. J Catal 214, 15–25.Google Scholar
Li, T, Bagot, PAJ, Christian, E, Theobald, BRC, Sharman, JDB, Ozkaya, D, Moody, MP, Tsang, SCE and Smith, GDW (2014). Atomic imaging of carbon-supported Pt, Pt/Co, and Ir@Pt nanocatalysts by atom-probe tomography. ACS Catal 4, 695–702.Google Scholar
Li, T, Bagot, PAJ, Marquis, EA, Tsang, SCE and Smith, GDW (2012). Characterization of oxidation and reduction of Pt–Ru and Pt–Rh–Ru alloys by atom probe tomography and comparison with Pt–Rh. J Phys Chem C 116, 17633–17640.Google Scholar
Li, X, Elliott, DW and Zhang, W (2006). Zero-valent iron nanoparticles for abatement of environmental pollutants: Materials and engineering aspects. Crit Rev Solid State Mater Sci 31, 111–122. http://www.tandfonline.com/doi/abs/10.1080/10408430601057611.Google Scholar
Linderoth, S, Mrup, S and Bentzon, MD (1990). Influence of pH on the composition and structure of Fe–Co–B alloy particles prepared by borohydride reduction in aqueous solutions. J Magn Magn Mater 83, 457–459.10.1016/0304-8853(90)90585-EGoogle Scholar
Miller, MK and Forbes, RG (2009). Atom probe tomography. Mater Charact 60, 461–469. http://dx.doi.org/10.1016/j.matchar.2009.02.007.Google Scholar
Miller, MK and Kenik, EA (2004). Atom probe tomography: A technique for nanoscale characterization. Microsc Microanal 10, 336–341.Google Scholar
Miller, MK, Russell, KF, Thompson, K, Alvis, R and Larson, DJ (2007). Review of atom probe FIB-based specimen preparation methods. Microsc Microanal 13, 428–436.Google Scholar
Ocon, JD, Tuan, TN, Yi, Y, De Leon, RL, Lee, JK and Lee, J (2013). Ultrafast and stable hydrogen generation from sodium borohydride in methanol and water over Fe–B nanoparticles. J Power Sources 243, 444–450.Google Scholar
Okamoto, H (2010). Desk Handbook: Phase Diagram for Binary Alloys, 2nd ed. https://www.asminternational.org/home/-/journal_content/56/10192/57751G/PUBLICATION/.Google Scholar
Oprea, B, Martínez, L, Román, E, Espinosa, A, Ruano, M, Llamosa, D, García-Hernández, M, Ballesteros, C and Huttel, Y (2014). Growth and characterization of FeB nanoparticles for potential application as magnetic resonance imaging contrast agent. Mater Res Express 1, 025008.Google Scholar
Perea, DE, Arslan, I, Liu, J, Ristanović, Z, Kovarik, L, Arey, BW, Lercher, JA, Bare, SR and Weckhuysen, BM (2015). Determining the location and nearest neighbours of aluminium in zeolites with atom probe tomography. Nat Commun 6, 7589. http://www.nature.com/doifinder/10.1038/ncomms8589.Google Scholar
Perea, DE, Liu, J, Bartrand, J, Dicken, Q, Thevuthasan, ST, Browning, ND and Evans, JE (2016). Atom probe tomographic mapping directly reveals the atomic distribution of phosphorus in resin embedded ferritin. Sci Rep 6, 22321. http://www.nature.com/articles/srep22321.Google Scholar
Shahwan, T, Abu Sirriah, S, Nairat, M, Boyaci, E, Eroĝlu, AE, Scott, TB and Hallam, KR (2011). Green synthesis of iron nanoparticles and their application as a Fenton-like catalyst for the degradation of aqueous cationic and anionic dyes. Chem Eng J 172, 258–266.Google Scholar
Shen, J, Li, Z and Chen, Y (1994). Preparation of Fe-B ultrafine amorphous alloy particles by the reaction of ferric chloride and potassium borohydride in aqueous solution. J Mater Sci Lett 13, 1208–1210.Google Scholar
Shi, LN, Zhang, X and Chen, ZL (2011). Removal of chromium(VI) from wastewater using bentonite-supported nanoscale zero-valent iron. Water Res 45, 886–892.Google Scholar
Sun, Y-P, Li, X, Cao, J, Zhang, W and Wang, HP (2006). Characterization of zero-valent iron nanoparticles. Adv Colloid Interface Sci 120, 47–56. http://linkinghub.elsevier.com/retrieve/pii/S000186860600025X.Google Scholar
Tedsree, K, Li, T, Jones, S, Chan, CWA, Yu, KMK, Bagot, PAJ, Marquis, EA, Smith, GDW and Tsang, SCE (2011). Hydrogen production from formic acid decomposition at room temperature using a Ag–Pd core–shell nanocatalyst. Nat Nanotechnol 6, 302–307. http://www.nature.com/doifinder/10.1038/nnano.2011.42.Google Scholar
Thompson, K, Lawrence, D, Larson, DJ, Olson, JD, Kelly, TF and Gorman, B (2007). In situ site-specific specimen preparation for atom probe tomography. Ultramicroscopy 107, 131–139.Google Scholar
Vilayurganapathy, S, Devaraj, A, Colby, R, Pandey, A, Varga, T, Shutthanandan, V, Manandhar, S, El-Khoury, PZ, Kayani, A, Hess, WP and Thevuthasan, S (2013). Subsurface synthesis and characterization of Ag nanoparticles embedded in MgO. Nanotechnology 24, 095707. http://iopscience.iop.org/article/10.1088/0957-4484/24/9/095707.Google Scholar
Walter, JC, Zurawski, A, Montgomery, D, Thornburg, M and Revankar, S (2008). Sodium borohydride hydrolysis kinetics comparison for nickel, cobalt, and ruthenium boride catalysts. J Power Sources 179, 335–339.Google Scholar
Wang, CB and Zhang, WX (1997). Synthesizing nanoscale iron particles for rapid and complete dechlorination of TCE and PCBs. Environ Sci Technol 31, 2154–2156.Google Scholar
Wells, S, Charles, SW, Mørup, S, Linderoth, S, Van Wonterghem, J, Larsen, J and Madsen, MB (1989). A study of Fe–B and Fe–Co–B alloy particles produced by reduction with borohydride. J Phys: Condens Matter 1, 8199–8208.Google Scholar
Wu, C, Bai, Y and Wu, F (2008). Fast hydrogen generation from NaBH4 solution accelerated by ferric catalysts. Mater Lett 62, 4242–4244.10.1016/j.matlet.2008.07.020Google Scholar
Xiang, Y, Chitry, V, Liddicoat, P, Felfer, P, Cairney, J, Ringer, S and Kruse, N (2013). Long-chain terminal alcohols through catalytic CO hydrogenation. J Am Chem Soc 135, 7114–7117.Google Scholar
Yu, KMK, Tong, W, West, A, Cheung, K, Li, T, Smith, G, Guo, Y and Tsang, SCE (2012). Non-syngas direct steam reforming of methanol to hydrogen and carbon dioxide at low temperature. Nat Commun 3, 1230. http://www.nature.com/doifinder/10.1038/ncomms2242.Google Scholar
Yuvakkumar, R, Elango, V, Rajendran, V and Kannan, N (2011). Preparation and characterization of zero valent iron nanoparticles. Dig J Nanomater Biostruct 6, 1771–1776.Google Scholar
Zhang, D, Wei, S, Kaila, C, Su, X, Wu, J, Karki, AB, Young, DP and Guo, Z (2010). Carbon-stabilized iron nanoparticles for environmental remediation. Nanoscale 2, 917. http://xlink.rsc.org/?DOI=c0nr00065e.Google Scholar
Zhang, WX (2003). Nanoscale iron particles for environmental remediation: An overview. J Nanopart Res 5, 323–332.Google Scholar
Zysler, RD, Ramos, CA, Romero, H and Ortega, A (2001). Chemical synthesis and characterization of amorphous Fe-Ni-B magnetic nanoparticles. J Mater Sci 36, 2291–2294.Google Scholar