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High Pressure Synthesis of Ultrasmall Nanodiamonds with Nitrogen Vacancy Centers

Dalmieda, Johnson [Columbia Univ., New York, NY (United States)] (ORCID:0000000238828191)·Tencio, Daybis [Columbia Univ., New York, NY (United States)]·Khan, Rohma [City Univ. of New York (CUNY), NY (United States)]·Myers, Caden J. [Columbia Univ., New York, NY (United States)] (ORCID:000900091333656X)·Shanahan, James P. [Columbia Univ., New York, NY (United States)]·Karube, Yuzuka [Columbia Univ., New York, NY (United States)]·Pagliero, Daniela [City Univ. of New York (CUNY), NY (United States)]·Wolcott, Abraham [City Univ. of New York (CUNY), NY (United States); San Jose State Univ., CA (United States)] (ORCID:0000000240253040)·Xu, Kang [City Univ. of New York (CUNY), NY (United States)] (ORCID:0009000805485293)·Ziffer, Mark E. [Columbia Univ., New York, NY (United States)]·Ghose, Sanjit K. [Brookhaven National Laboratory (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)] (ORCID:0000000302458560)·Lee, Sang-Jun [SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)] (ORCID:0000000281993993)·Nordlund, Dennis [SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)]·Schuck, P. James [Columbia Univ., New York, NY (United States)] (ORCID:0000000192442671)·Billinge, Simon J. L. [Univ. of California, Santa Barbara, CA (United States)]·Ercius, Peter [Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States). Molecular Foundry] (ORCID:0000000267629976)·Meriles, Carlos A. [City Univ. of New York (CUNY), NY (United States)] (ORCID:0000000321971474)·Walker, David [Columbia Univ., New York, NY (United States)]·Whitaker, Matthew L. [Brookhaven National Laboratory (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II); Stony Brook Univ., NY (United States)]·Braun, Augustin [Columbia Univ., New York, NY (United States)] (ORCID:0000000294875769)·Owen, Jonathan S. [Columbia Univ., New York, NY (United States)] (ORCID:0000000155023267)
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Abstract

C–H terminated nanometer scale diamonds ( d = 1 to 15 nm) are synthesized from 1-fluoroadamantane at high pressure (6–8 GPa) and high temperature (500–1500 °C) in a multianvil press. High resolution transmission electron microscopy, X-ray diffraction, Raman, diffuse reflectance Fourier transform infrared, and X-ray absorption spectroscopies demonstrate the excellent crystallinity and atomically flat C–H terminated surfaces of nanodiamonds with (111) and (110) facets. The importance of hydrogen to the synthesis of nanodiamond and its faceting is discussed. Following vacancy generation, annealing and oxidation of the nanodiamonds, optically detected magnetic resonance and electron spin resonance coherence times ( T 2 = 0.9 and 2.1 μs) of nitrogen vacancy (NV) centers are measured. Finally, the obtained T 2 values are equivalent to the shallow NV centers (depth <10 nm) in bulk diamond crystals and larger nanocrystals prepared by mechanical milling.

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36 MATERIALS SCIENCEhigh pressurenanodiamondsnitrogen vacancy centersspin coherencewell defined facets

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Dalmieda, Johnson [Columbia Univ., New York, NY (United States)] (ORCID:0000000238828191), Tencio, Daybis [Columbia Univ., New York, NY (United States)], Khan, Rohma [City Univ. of New York (CUNY), NY (United States)], Myers, Caden J. [Columbia Univ., New York, NY (United States)] (ORCID:000900091333656X), Shanahan, James P. [Columbia Univ., New York, NY (United States)], Karube, Yuzuka [Columbia Univ., New York, NY (United States)], Pagliero, Daniela [City Univ. of New York (CUNY), NY (United States)], Wolcott, Abraham [City Univ. of New York (CUNY), NY (United States); San Jose State Univ., CA (United States)] (ORCID:0000000240253040), Xu, Kang [City Univ. of New York (CUNY), NY (United States)] (ORCID:0009000805485293), Ziffer, Mark E. [Columbia Univ., New York, NY (United States)], Ghose, Sanjit K. [Brookhaven National Laboratory (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II)] (ORCID:0000000302458560), Lee, Sang-Jun [SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)] (ORCID:0000000281993993), Nordlund, Dennis [SLAC National Accelerator Laboratory (SLAC), Menlo Park, CA (United States). Stanford Synchrotron Radiation Lightsource (SSRL)], Schuck, P. James [Columbia Univ., New York, NY (United States)] (ORCID:0000000192442671), Billinge, Simon J. L. [Univ. of California, Santa Barbara, CA (United States)], Ercius, Peter [Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States). Molecular Foundry] (ORCID:0000000267629976), Meriles, Carlos A. [City Univ. of New York (CUNY), NY (United States)] (ORCID:0000000321971474), Walker, David [Columbia Univ., New York, NY (United States)], Whitaker, Matthew L. [Brookhaven National Laboratory (BNL), Upton, NY (United States). National Synchrotron Light Source II (NSLS-II); Stony Brook Univ., NY (United States)], Braun, Augustin [Columbia Univ., New York, NY (United States)] (ORCID:0000000294875769), Owen, Jonathan S. [Columbia Univ., New York, NY (United States)] (ORCID:0000000155023267). 2026-07-01. High Pressure Synthesis of Ultrasmall Nanodiamonds with Nitrogen Vacancy Centers. https://doi.org/10.1021/acs.nanolett.6c02324

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