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Title: Synthesis of Uniform Diameter Boron-Based Nanostructures Using a Mesoporous Mg-Al2O3 Template and Tests for Superconductivity

Journal Article · · Journal of Physical Chemistry C
DOI:https://doi.org/10.1021/jp904304t· OSTI ID:1020140

Mg incorporated mesoporous alumina with high surface area and narrow pore size distribution was prepared by the sol-gel method to use as a template for the synthesis of boron-based nanostructures by the CVD method. The mesoporous nature of the Mg-Al{sub 2}O{sub 3} was confirmed by low-angle XRD and N{sub 2} adsorption analyses. The randomly ordered pores were observed by TEM. The growth of boron-based nanostructures, such as nanowires and nanotubes, over Mg-Al{sub 2}O{sub 3} is evidenced by TEM analysis. Use of BCl{sub 3} as the boron source resulted in nanowires of around 20 nm in diameter and several micrometers in length. When using B{sub 2}H{sub 6} as the boron source, the diameter of the obtained nanostructures was in the range 3-4 nm, reflective of the pore diameter of Mg-Al{sub 2}O{sub 3}. Further loading of Mg in the form of Rieke Mg by sonication over 1% Mg-Al{sub 2}O{sub 3} resulted in the growth of straight nanotubes with a uniform diameter of 3-4 nm. The NEXAFS of the boron K-edge of purified boron-based nanostructures shows characteristic peaks for the existence of Mg-B and Al-B bonding. The STEM and EELS of the obtained individual nanostructures confirm the presence of B, Mg, and Al in the nanostructures. The appearance of a boron prepeak at 186 eV in EELS indicates that the boron hole states are not filled by the aluminum present in the nanostructures. Both field dependent DC magnetization (SQUID) and AC magnetic susceptibility measurements of Mg{sub x}B{sub y} nanostructures grown over 2 wt % Rieke Mg sonicated 1% Mg-Al{sub 2}O{sub 3} using B{sub 2}H{sub 6} as the boron source show evidence of a diamagnetic transition at about 80 K. The diamagnetic nature of Mg{sub x}B{sub y} nanostructures is suppressed significantly when the grown Mg{sub x}B{sub y} nanostructures are washed with NaOH solution to remove the template.

Research Organization:
Brookhaven National Lab. (BNL), Upton, NY (United States). National Synchrotron Light Source
Sponsoring Organization:
DOE - OFFICE OF SCIENCE
DOE Contract Number:
DE-AC02-98CH10886
OSTI ID:
1020140
Report Number(s):
BNL-95990-2011-JA; TRN: US201116%%121
Journal Information:
Journal of Physical Chemistry C, Vol. 113, Issue 41; ISSN 1932-7447
Country of Publication:
United States
Language:
English