Direct bottom-up high pressure high temperature (BU_HPHT) synthesis of nanodiamonds (NDs) from organic precursors excels in the ability to control the size of the resulting BU_HPHT NDs via the temperature of the synthesis. Here we investigated size-dependent thermal, colloidal, and structural properties of the BU_HPHT NDs and focused on the transition in morphology and properties occurring at around 900 °C (≈2 nm). Using transmission electron microscopy, small angle X-ray scattering and atomic force microscopy we show that the sub-900 °C samples (<2 nm NDs) do not have nanoparticle character but 2D platelet morphology with sub-nm unit thickness. Correspondingly, sub-900 °C samples (<2 nm NDs) have a negative zeta potential and hydrophobic character and should be considered as a form of a molecular diamond. The above-900C (>2 nm NDs) samples have nanocrystalline character, positive zeta potential and are dispersible in water similarly to other types of hydrogenated NDs. By in situ Raman spectroscopy experiments, we show that the transition is also related to the structural instability of the oxidized sub-2 nm BU_HPHT NDs.

Department of Material Science and Metallurgy Faculty of Mechanical Engineering University of West Bohemia Pilsen Czech Republic

Faculty of Electrical Engineering Czech Technical University Prague Czech Republic

Faculty of Environment Jan Evangelista Purkyně University in Ústí nad Labem Ústí nad Labem Czech Republic

Institute of Inorganic Chemistry of the Czech Academy of Sciences Husinec Řež Czech Republic

Institute of Physics of the Czech Academy of Sciences Prague Czech Republic

New Technologies Research Centre University of West Bohemia in Pilsen Pilsen Czech Republic

Vereshchagin Institute for High Pressure Physics Russian Academy of Sciences Troitsk Russia

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Xue Y. Feng X. Roberts S. C. Chen X. Funct. Diam. 2021;1:221–242. doi: 10.1080/26941112.2021.2013716. DOI

Zhang T. Pramanik G. Zhang K. Gulka M. Wang L. Jing J. Xu F. Li Z. Wei Q. Cigler P. Chu Z. ACS Sens. 2021;6:2077–2107. doi: 10.1021/acssensors.1c00415. PubMed DOI

Wang C. Sun X. Zhang J. Zhai X. Zhang X. Li Z. Li H. Chem. Eng. J. 2023;466:143191. doi: 10.1016/j.cej.2023.143191. DOI

Liu K. Sun M. Yang S. Gan G. Bu S. Zhu A. Lin D. Zhang T. Luan C. Zhi C. Wang P. Huang B. Hong G. Zhang W. Adv. Energy Mater. 2024:2401479. doi: 10.1002/aenm.202401479. DOI

Wang M. Zhang J. Wu M. Yang D. Sun P. Sun J. Zhang Z. Chen X. Ba J. Wang Y. Qiu J. Wei Y. Adv. Funct. Mater. 2024:2315757. doi: 10.1002/adfm.202315757. DOI

Henych J. Stehlík Š. Mazanec K. Tolasz J. Čermák J. Rezek B. Mattsson A. Österlund L. Appl. Catal., B. 2019;259:118097. doi: 10.1016/j.apcatb.2019.118097. DOI

Marchal C. Saoudi L. Girard H. A. Keller V. Arnault J. Adv. Energy Sustainability Res. 2023:2300260.

Bland H. A. Centeleghe I. A. Mandal S. Thomas E. L. H. Maillard J.-Y. Williams O. A. ACS Appl. Nano Mater. 2021;4:3252–3261. doi: 10.1021/acsanm.1c00439. PubMed DOI PMC

Molavi H. Mirzaei K. Jafarpour E. Mohammadi A. Salimi M. S. Rezakazemi M. Nadagouda M. M. Aminabhavi T. M. J. Environ. Manage. 2024;349:119349. doi: 10.1016/j.jenvman.2023.119349. PubMed DOI

Turner S. Lebedev O. I. Shenderova O. Vlasov I. I. Verbeeck J. Van Tendeloo G. Adv. Funct. Mater. 2009;19:2116–2124. doi: 10.1002/adfm.200801872. DOI

Turner S. Shenderova O. Da Pieve F. Lu Y. Yücelen E. Verbeeck J. Lamoen D. Van Tendeloo G. Phys. Status Solidi A. 2013;210:1976–1984. doi: 10.1002/pssa.201300315. DOI

Rehor I. Cigler P. Diamond Relat. Mater. 2014;46:21–24. doi: 10.1016/j.diamond.2014.04.002. DOI

Stehlik S. Szabo O. Shagieva E. Miliaieva D. Kromka A. Nemeckova Z. Henych J. Kozempel J. Ekimov E. Rezek B. Carbon Trends. 2024;14:100327. doi: 10.1016/j.cartre.2024.100327. DOI

Ekimov E. A. Lyapin S. G. Grigoriev Yu. V. Zibrov I. P. Kondrina K. M. Carbon. 2019;150:436–438. doi: 10.1016/j.carbon.2019.05.047. DOI

Ekimov E. A. Kondrin M. V. Lyapin S. G. Grigoriev Yu. V. Razgulov A. A. Krivobok V. S. Gierlotka S. Stelmakh S. Diamond Relat. Mater. 2020;103:107718. doi: 10.1016/j.diamond.2020.107718. DOI

Ekimov E. Shiryaev A. A. Grigoriev Y. Averin A. Shagieva E. Stehlik S. Kondrin M. Nanomaterials. 2022;12:351. doi: 10.3390/nano12030351. PubMed DOI PMC

Ekimov E. A. Kudryavtsev O. S. Khomich A. A. Lebedev O. I. Dolenko T. A. Vlasov I. I. Adv. Mater. 2015;27:5518–5522. doi: 10.1002/adma.201502672. PubMed DOI

Ekimov E. A. Kondrin M. V. Krivobok V. S. Khomich A. A. Vlasov I. I. Khmelnitskiy R. A. Iwasaki T. Hatano M. Diamond Relat. Mater. 2019;93:75–83. doi: 10.1016/j.diamond.2019.01.029. DOI

Stelmakh S. Skrobas K. Gierlotka S. Palosz B. J. Phys.: Condens. Matter. 2021;33:175002. doi: 10.1088/1361-648X/abe26a. PubMed DOI

Stehlik S. Varga M. Ledinsky M. Jirasek V. Artemenko A. Kozak H. Ondic L. Skakalova V. Argentero G. Pennycook T. Meyer J. C. Fejfar A. Kromka A. Rezek B. J. Phys. Chem. C. 2015;119:27708–27720. doi: 10.1021/acs.jpcc.5b05259. PubMed DOI PMC

Stehlik S. Varga M. Ledinsky M. Miliaieva D. Kozak H. Skakalova V. Mangler C. Pennycook T. J. Meyer J. C. Kromka A. Rezek B. Sci. Rep. 2016;6:38419. doi: 10.1038/srep38419. PubMed DOI PMC

Bradac C. Osswald S. Carbon. 2018;132:616–622. doi: 10.1016/j.carbon.2018.02.102. DOI

Williams O. A. Hees J. Dieker C. Jäger W. Kirste L. Nebel C. E. ACS Nano. 2010;4:4824–4830. doi: 10.1021/nn100748k. PubMed DOI

Petit T. Girard H. A. Trouvé A. Batonneau-Gener I. Bergonzo P. Arnault J.-C. Nanoscale. 2013;5:8958. doi: 10.1039/C3NR02492J. PubMed DOI

Ginés L. Mandal S. Ashek-I-Ahmed A.-I.-A. Cheng C.-L. Sow M. Williams O. A. Nanoscale. 2017;9:12549–12555. doi: 10.1039/C7NR03200E. PubMed DOI

Yoshikawa T. Zuerbig V. Gao F. Hoffmann R. Nebel C. E. Ambacher O. Lebedev V. Langmuir. 2015;31:5319–5325. doi: 10.1021/acs.langmuir.5b01060. PubMed DOI

Shvidchenko A. V. Eidelman E. D. Vul’ A. Ya. Kuznetsov N. M. Stolyarova D. Yu. Belousov S. I. Chvalun S. N. Adv. Colloid Interface Sci. 2019;268:64–81. doi: 10.1016/j.cis.2019.03.008. PubMed DOI

Crawford K. G. Maini I. Macdonald D. A. Moran D. A. J. Prog. Surf. Sci. 2021;96:100613. doi: 10.1016/j.progsurf.2021.100613. DOI

Vlk A. Ledinsky M. Shiryaev A. Ekimov E. Stehlik S. J. Phys. Chem. C. 2022;126:6318–6324. doi: 10.1021/acs.jpcc.2c00446. DOI

Kondo T. Neitzel I. Mochalin V. N. Urai J. Yuasa M. Gogotsi Y. J. Appl. Phys. 2013;113:214307. doi: 10.1063/1.4809549. DOI

Osswald S. Yushin G. Mochalin V. Kucheyev S. O. Gogotsi Y. J. Am. Chem. Soc. 2006;128:11635–11642. doi: 10.1021/ja063303n. PubMed DOI

Mermoux M. Crisci A. Petit T. Girard H. A. Arnault J.-C. J. Phys. Chem. C. 2014;118:23415–23425. doi: 10.1021/jp507377z. DOI

Ilavsky J. Jemian P. R. J. Appl. Crystallogr. 2009;42:347–353. doi: 10.1107/S0021889809002222. DOI

Stehlik S. Henych J. Stenclova P. Kral R. Zemenova P. Pangrac J. Vanek O. Kromka A. Rezek B. Carbon. 2021;171:230–239. doi: 10.1016/j.carbon.2020.09.026. DOI

Beaucage G. J. Appl. Crystallogr. 1995;28:717–728. doi: 10.1107/S0021889895005292. DOI

Ozawa M. Inaguma M. Takahashi M. Kataoka F. Krüger A. Ōsawa E. Adv. Mater. 2007;19:1201–1206. doi: 10.1002/adma.200601452. DOI

Turcheniuk K. Trecazzi C. Deeleepojananan C. Mochalin V. N. ACS Appl. Mater. Interfaces. 2016;8:25461–25468. doi: 10.1021/acsami.6b08311. PubMed DOI

Damasceno J. P. V. Kubota L. T. Angew. Chem., Int. Ed. 2022;61:e202214995. doi: 10.1002/anie.202214995. PubMed DOI

Kudin K. N. Car R. J. Am. Chem. Soc. 2008;130:3915–3919. doi: 10.1021/ja077205t. PubMed DOI

Houska V. Ukraintsev E. Vacek J. Rybáček J. Bednárová L. Pohl R. Stará I. G. Rezek B. Starý I. Nanoscale. 2023;15:1542–1553. doi: 10.1039/D2NR04209F. PubMed DOI

Ekimov E. A. Shiryaev A. A. Sidorov V. A. Grigoriev Y. V. Averin A. A. Kondrin M. V. Diamond Relat. Mater. 2023;136:109907. doi: 10.1016/j.diamond.2023.109907. DOI

Ekimov E. A. Kudryavtsev O. S. Mordvinova N. E. Lebedev O. I. Vlasov I. I. ChemNanoMat. 2018;4:269–273. doi: 10.1002/cnma.201700349. DOI

Stehlik S. Mermoux M. Schummer B. Vanek O. Kolarova K. Stenclova P. Vlk A. Ledinsky M. Pfeifer R. Romanyuk O. Gordeev I. Roussel-Dherbey F. Nemeckova Z. Henych J. Bezdicka P. Kromka A. Rezek B. J. Phys. Chem. C. 2021;125:5647–5669. doi: 10.1021/acs.jpcc.0c09190. DOI

Kudryavtsev O. S. Bagramov R. H. Pasternak D. G. Satanin A. M. Lebedev O. I. Filonenko V. P. Vlasov I. I. Diamond Relat. Mater. 2023;133:109770. doi: 10.1016/j.diamond.2023.109770. DOI

Chaigneau M. Picardi G. Girard H. A. Arnault J.-C. Ossikovski R. J. Nanopart. Res. 2012;14:955. doi: 10.1007/s11051-012-0955-9. DOI

Mochalin V. N. Shenderova O. Ho D. Gogotsi Y. Nat. Nanotechnol. 2011;7:11–23. doi: 10.1038/nnano.2011.209. PubMed DOI

Wolcott A. Schiros T. Trusheim M. E. Chen E. H. Nordlund D. Diaz R. E. Gaathon O. Englund D. Owen J. S. J. Phys. Chem. C. 2014;118:26695–26702. doi: 10.1021/jp506992c. PubMed DOI PMC

Gouadec G. Colomban P. Prog. Cryst. Growth Charact. Mater. 2007;53:1–56. doi: 10.1016/j.pcrysgrow.2007.01.001. DOI

Kaviani M. Deák P. Aradi B. Köhler T. Frauenheim T. Diamond Relat. Mater. 2013;33:78–84. doi: 10.1016/j.diamond.2013.01.002. DOI