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ACS Omega ■ Article AUTHOR INFORMATION Corresponding Author *E-mail: takahiro@ims.tsukuba.ac.jp. ORCID Junko N. Kondo: 0000-0002-7940-1266 Tadahiro Fujitani: 0000-0002-1225-3246 Hideo Hosono: 0000-0001-9260-6728 Takahiro Kondo: 0000-0001-8457-9387 Notes T■he authors declare no competing financial interest. ACKNOWLEDGMENTS This work was supported by the JSPS KAKENHI nos. JP 18K18989, JP 19H05046, and JP 19H02551 and Murata Science Foundation, KUMAGAI, Ogasawara, and Samco foundations for the Promotion of Science & Engineering. T.K., S.-i.I., and H.H. were supported by the MEXT Element Strategy Initiative to Form Core Research Center. ■ Ltd., Osaka, Japan) was mixed with a solution of an ion- exchange resin (60 mL, Amberlite IR120B hydrogen form, Organo Corp., Tokyo, Japan) and acetonitrile (200 mL) in a Schlenk flask under a nitrogen atmosphere, where water inclusion is sensitive to the product35 and thus careful removal of water was done beforehand. This mixture was stirred using a magnetic stirrer at 400 rpm for 2 days at room temperature. The supernatant was then kept for 1 day at 255 K to physically separate the byproduct B(OH)3. Dried HB sheets were prepared by heating the resulting liquid at 343 K while pumping with a liquid nitrogen trap. For all of the syntheses, we carefully confirmed the product by X-ray photoelectron spectroscopy to confirm the absence of Mg and the presence of negatively charged B without oxidized B as reported previously.13 Moreover, we recently confirmed using atomic force microscopy (AFM) that our HB sheets mostly consist of a few to several tens of layers. The details of AFM with statistical analysis will be published in our future work. Catalytic Activity Measurements. To determine the catalytic activity, gaseous ethanol was introduced into the HB sheets using an argon carrier gas under atmospheric pressure in a homemade fixed-bed flow reactor. The product gas was then analyzed using a thermal conductivity detector in a gas chromatograph (GC-8A, Shimadzu, Kyoto, Japan) equipped with Molecular Sieve 5A and Porapak Q at the downstream end of the reactor. The catalytic conversion was estimated from the total amount of hydrocarbon production using the following relation ethanol conversion (%) = [(number of total carbon in detected hydrocarbon molecules)(mol/min)] /[introduced ethanol molecules × 2 (mol/min)] × 100 As shown in Figure 2a, the conversion was also estimated from ethanol consumption as follows ethanol conversion (%) = [(introduced ethanol molecules − detected ethanol molecules) (mol/min)] /[introducedethanolmolecules(mol/min)] × 100 The selectivity was estimated using the following relation REFERENCES selectivity of specific product (%) (1) Wang, Y.; Mao, J.; Meng, X.; Yu, L.; Deng, D.; Bao, X. Catalysis with Two-Dimensional Materials Confining Single Atoms: Concept, Design, and Applications. Chem. Rev. 2019, 119, 1806−1854. (2) Deng, D.; Novoselov, K. S.; Fu, Q.; Zheng, N.; Tian, Z.; Bao, X. Catalysis with Two-Dimensional Materials and Their Heterostruc- tures. Nat. Nanotechnol. 2016, 11, 218−230. (3) Zhang, Z.; Penev, E. S.; Yakobson, B. I. Two-Dimensional Boron: Structures, Properties and Applications. Chem. Soc. Rev. 2017, 46, 6746−6763. (4) Kondo, T. Recent Progress in Boron Nanomaterials. Sci. Technol. Adv. Mater. 2017, 18, 780−804. (5) Jiao, Y.; Ma, F.; Bell, L.; Bilic, A.; Du, A. Two-Dimensional Boron Hydride Sheets:High Stability, Massless Dirac Fermions, and Excellent Mechanical Properties. Angew. Chem. Int. Ed. 2016, 55, 10292−10295. (6) Oganov, A. R.; Solozhenko, V. L. Boron: A Hunt for Superhard Polymorphs. J. Superhard Mater. 2009, 31, 285−291. (7) Mannix, A. J.; Kiraly, B.; Hersam, M. C.; Guisinger, N. P. Synthesis and Chemistry of Elemental 2D Materials. Nat. Rev. Chem. 2017, 1, 0014. (8) Boustani, I. New Quasi-Planar Surfaces of Bare Boron. Surf. Sci. 1997, 370, 355−363. (9) Penev, E. S.; Bhowmick, S.; Sadrzadeh, A.; Yakobson, B. I. Polymorphism of Two-Dimensional Boron. Nano Lett. 2012, 12, 2441−2445. (10) Wu, X.; Dai, J.; Zhao, Y.; Zhuo, Z.; Yang, J.; Zeng, X. C. Two- Dimensional Boron Monolayer Sheets. ACS Nano 2012, 6, 7443− 7453. (11) Zhang, X.; Wu, T.; Wang, H.; Zhao, R.; Chen, H.; Wang, T.; Wei, P.; Luo, Y.; Zhang, Y.; Sun, X. Boron Nanosheet: An Elemental Two-Dimensional (2D) Material for Ambient Electrocatalytic N2 -to- NH3 Fixation in Neutral Media. ACS Catal. 2019, 9, 4609−4615. (12) Chen, Y.; Yu, G.; Chen, W.; Liu, Y.; Li, G.; Zhu, P.; Tao, Q.; Li, Q.; Liu, J.; Shen, X.; et al. Highly Active, Nonprecious Electrocatalyst Comprising Borophene Subunits for the Hydrogen Evolution Reaction. J. Am. Chem. Soc. 2017, 139, 12370−12373. (13) Nishino, H.; Fujita, T.; Cuong, N. T.; Tominaka, S.; Miyauchi, M.; Iimura, S.; Hirata, A.; Umezawa, N.; Okada, S.; Nishibori, E.; et al. Formation and Characterization of Hydrogen Boride Sheets Derived from MgB2 by Cation Exchange. J. Am. Chem. Soc. 2017, 139, 13761−13769. (14) Tateishi, I.; Cuong, N. T.; Moura, C. A. S.; Cameau, M.; Ishibiki, R.; Fujino, A.; Okada, S.; Yamamoto, A.; Araki, M.; Ito, S.; et al. Semimetallicity of Free-Standing Hydrogenated Monolayer Boron from MgB2. Phys. Rev. Mater. 2019, 3, No. 024004. DOI: 10.1021/acsomega.9b02020 ACS Omega 2019, 4, 14100−14104 = total amount of specific product (mol) total amount of products (mol) × 100 The catalytic activity was determined under various W/F conditions (g·min/mmol), which is the weight of the catalyst (g) divided by the flow rate of C2H5OH (mmol/min); W/F was controlled by adjusting the flow rate of C2H5OH and the weight of the sample. The W/F conditions used in this work are listed in Table S1. ■ ASSOCIATED CONTENT *S Supporting Information The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acsome- ga.9b02020. Origin of the induction period, TDS, effect of water, and catalytic activity of HB without pretreatment heating (PDF) 14103PDF Image | Hydrogenated Borophene Shows Catalytic Activity as Solid Acid
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