Preprint Article Version 1 Preserved in Portico This version is not peer-reviewed

Carbonization of Zr-Loaded Thiourea-Functionalized Styrene-Divinylbenzene Copolymers: An Easy Way to Synthesize Nano-ZrO2@C and Nano-(ZrC, ZrO2)@C Composites

Alejandro Martiz
ORCID logo ,
Zoltán Károly
ORCID logo ,
Laura Bereczki
ORCID logo ,
László Trif
,
Attila Farkas
,
Alfréd Menyhárd
,
László Kótai
*
Version 1 : Received: 29 June 2023 / Approved: 30 June 2023 / Online: 30 June 2023 (14:57:52 CEST)

A peer-reviewed article of this Preprint also exists.

Martiz, A.; Károly, Z.; Bereczki, L.; Trif, L.; Farkas, A.; Menyhárd, A.; Kótai, L. Carbonization of Zr-Loaded Thiourea-Functionalized Styrene-Divinylbenzene Copolymers: An Easy Way to Synthesize Nano-ZrO2@C and Nano-(ZrC, ZrO2)@C Composites. J. Compos. Sci. 2023, 7, 306. Martiz, A.; Károly, Z.; Bereczki, L.; Trif, L.; Farkas, A.; Menyhárd, A.; Kótai, L. Carbonization of Zr-Loaded Thiourea-Functionalized Styrene-Divinylbenzene Copolymers: An Easy Way to Synthesize Nano-ZrO2@C and Nano-(ZrC, ZrO2)@C Composites. J. Compos. Sci. 2023, 7, 306.

Abstract

Thermal processing of Zr-loaded ion-exchangers is a facile route to synthetize (ZrO2, ZrC)@C composites. The chemical character of the functional groups in the cation exchanger is an essential factor in the composition and properties of the (ZrO2, ZrC)@C composites. In the present paper furnace and RF-thermal plasma processing of ZrOCl2 loaded thiourea-functionalized styrene-divinylbenzene copolymer was investigated that led to various composites containing ZrO2 and ZrC. Depending on the synthesis conditions, different ZrO2@C composites were formed between 1000 and 1400 °C in 2 h, whereas the composite containing ZrC was created at 1400 °C in 8 h. The ratio of ZrO2/ZrC, the prevailing ZrO2 modifications, and the crystallite sizes strongly depend on the synthesis conditions. The ZrC-containing composites formed only at 1400 °C in 8 hours and by the plasma treatment of the ZrO2@C sample prepared in the furnace, resulting in 8 and 16% ZrC content, with 44 and 41 nm ZrC crystallite sizes, respectively. The ZrO2-containing composites (tetragonal, monoclinic, and cubic modifications with 65–88 nm ZrO2 crystallite sizes and 15–43 m2/g BET surface areas, depending on the carbonization temperature) formed in a tube furnace between 1000 and 1400 °C in 2 h. The tube furnace–prepared sample formed at 1400 °C in 8 h contained ZrC, ZrO2 modifications, and amorphous carbon, whereas the plasma-treated sample contained ZrC, ZrO2 modifications, and graphite. All ZrO2@C composites had both amorphous carbon and graphite, and their ratio is temperature-dependent. The carbonaceous compounds of the prepared composites were characterized by Raman spectroscopy, with analysis of the G and D band intensities. XPS studies showed the surface oxidation of ZrC.

Keywords

zirconium carbide; zirconium dioxide; carbon matrix; graphite; RF plasma; carbonization; thiourea; styrene-divinylbenzene copolymer; Raman spectroscopy

Subject

Chemistry and Materials Science, Materials Science and Technology

Copyright: This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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