Mechanically activated TiN nano-powders consolidated by spark plasma sintering and high-pressure methods

Titanium nitride (TiN) nano-powder was synthesized in a gas-pressure vessel steel via a mechanically induced reaction between Ti(α) and nitrogen gas for 40 h. Following mechanical activation, the precursor was consolidated using two distinct methods: spark plasma sintering (SPS) at 1600 °C for 10 mi...

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Main Authors: Jakub Kasprzycki, Katarzyna Stan-Głowińska, Piotr Ozga, Grzegorz Garzeł, Anna Sypień, Anna Góral, Sebastian Sobula, Karol Janus, Ganna Chyzhyk, Piotr Klimczyk, Urszula D. Wdowik, Lukasz Rogal
Format: Article
Language:English
Published: Elsevier 2025-07-01
Series:Journal of Materials Research and Technology
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Online Access:http://www.sciencedirect.com/science/article/pii/S2238785425016394
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author Jakub Kasprzycki
Katarzyna Stan-Głowińska
Piotr Ozga
Grzegorz Garzeł
Anna Sypień
Anna Góral
Sebastian Sobula
Karol Janus
Ganna Chyzhyk
Piotr Klimczyk
Urszula D. Wdowik
Lukasz Rogal
author_facet Jakub Kasprzycki
Katarzyna Stan-Głowińska
Piotr Ozga
Grzegorz Garzeł
Anna Sypień
Anna Góral
Sebastian Sobula
Karol Janus
Ganna Chyzhyk
Piotr Klimczyk
Urszula D. Wdowik
Lukasz Rogal
author_sort Jakub Kasprzycki
collection DOAJ
description Titanium nitride (TiN) nano-powder was synthesized in a gas-pressure vessel steel via a mechanically induced reaction between Ti(α) and nitrogen gas for 40 h. Following mechanical activation, the precursor was consolidated using two distinct methods: spark plasma sintering (SPS) at 1600 °C for 10 min under an applied pressure of 50 MPa, and a high-pressure-high-temperature (HPHT) process performed at 1300 °C and 1600 °C under 7.8 GPa for 1 min. The microstructure of the SPS-consolidated sample exhibited fine, uniform, pure TiN grains with an average size of 4.8 ± 2.0 μm. In contrast, the HPHT-consolidated material retains the TiN/TiN0.3 milled grains nanostructure. Additionally, localized reactions between grains with varying nitrogen content lead to the formation of new TiN nanoparticles ranging in size from 23.1 ± 7.7 nm to 27.5 ± 10 nm, depending on the consolidation temperature. Variations in mechanical properties are attributed to the increased porosity and inhomogeneous microstructure in HPHT-synthesized samples, which impair load transfer and grain boundary bonding, thereby reducing compressive strength (1779 and 1624 MPa) and hardness (1441 ± 98 and 1538 ± 62 HV). The higher density, which is obtained through SPS consolidation with stoichiometric TiN ensures better strength (2416 MPa) and hardness (1796 ± 160 HV).
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publishDate 2025-07-01
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spelling doaj-art-17d98b7b8dfd4d83b68fc640d72bbf972025-08-20T03:34:13ZengElsevierJournal of Materials Research and Technology2238-78542025-07-01373895390610.1016/j.jmrt.2025.06.217Mechanically activated TiN nano-powders consolidated by spark plasma sintering and high-pressure methodsJakub Kasprzycki0Katarzyna Stan-Głowińska1Piotr Ozga2Grzegorz Garzeł3Anna Sypień4Anna Góral5Sebastian Sobula6Karol Janus7Ganna Chyzhyk8Piotr Klimczyk9Urszula D. Wdowik10Lukasz Rogal11Institute of Metallurgy and Materials Science Polish Academy of Science, Krakow, Poland; Corresponding author.Institute of Metallurgy and Materials Science Polish Academy of Science, Krakow, PolandInstitute of Metallurgy and Materials Science Polish Academy of Science, Krakow, PolandInstitute of Metallurgy and Materials Science Polish Academy of Science, Krakow, PolandInstitute of Metallurgy and Materials Science Polish Academy of Science, Krakow, PolandInstitute of Metallurgy and Materials Science Polish Academy of Science, Krakow, PolandAGH University of Science and Technology, Kraków, PolandInstitute of Metallurgy and Materials Science Polish Academy of Science, Krakow, Poland; AGH University of Science and Technology, Kraków, PolandInstitute of Metallurgy and Materials Science Polish Academy of Science, Krakow, PolandŁukasiewicz Research Network, Krakow Institute of Technology, Krakow, PolandIT4Innovations, VSB - Technical University of Ostrava, 17. listopadu 2172/15, Ostrava-Poruba, CZ 708 00, Czech RepublicInstitute of Metallurgy and Materials Science Polish Academy of Science, Krakow, Poland; Corresponding author.Titanium nitride (TiN) nano-powder was synthesized in a gas-pressure vessel steel via a mechanically induced reaction between Ti(α) and nitrogen gas for 40 h. Following mechanical activation, the precursor was consolidated using two distinct methods: spark plasma sintering (SPS) at 1600 °C for 10 min under an applied pressure of 50 MPa, and a high-pressure-high-temperature (HPHT) process performed at 1300 °C and 1600 °C under 7.8 GPa for 1 min. The microstructure of the SPS-consolidated sample exhibited fine, uniform, pure TiN grains with an average size of 4.8 ± 2.0 μm. In contrast, the HPHT-consolidated material retains the TiN/TiN0.3 milled grains nanostructure. Additionally, localized reactions between grains with varying nitrogen content lead to the formation of new TiN nanoparticles ranging in size from 23.1 ± 7.7 nm to 27.5 ± 10 nm, depending on the consolidation temperature. Variations in mechanical properties are attributed to the increased porosity and inhomogeneous microstructure in HPHT-synthesized samples, which impair load transfer and grain boundary bonding, thereby reducing compressive strength (1779 and 1624 MPa) and hardness (1441 ± 98 and 1538 ± 62 HV). The higher density, which is obtained through SPS consolidation with stoichiometric TiN ensures better strength (2416 MPa) and hardness (1796 ± 160 HV).http://www.sciencedirect.com/science/article/pii/S2238785425016394Mechanical alloyingNitrogen pressureTitanium nitrideNanoparticlesConsolidation
spellingShingle Jakub Kasprzycki
Katarzyna Stan-Głowińska
Piotr Ozga
Grzegorz Garzeł
Anna Sypień
Anna Góral
Sebastian Sobula
Karol Janus
Ganna Chyzhyk
Piotr Klimczyk
Urszula D. Wdowik
Lukasz Rogal
Mechanically activated TiN nano-powders consolidated by spark plasma sintering and high-pressure methods
Journal of Materials Research and Technology
Mechanical alloying
Nitrogen pressure
Titanium nitride
Nanoparticles
Consolidation
title Mechanically activated TiN nano-powders consolidated by spark plasma sintering and high-pressure methods
title_full Mechanically activated TiN nano-powders consolidated by spark plasma sintering and high-pressure methods
title_fullStr Mechanically activated TiN nano-powders consolidated by spark plasma sintering and high-pressure methods
title_full_unstemmed Mechanically activated TiN nano-powders consolidated by spark plasma sintering and high-pressure methods
title_short Mechanically activated TiN nano-powders consolidated by spark plasma sintering and high-pressure methods
title_sort mechanically activated tin nano powders consolidated by spark plasma sintering and high pressure methods
topic Mechanical alloying
Nitrogen pressure
Titanium nitride
Nanoparticles
Consolidation
url http://www.sciencedirect.com/science/article/pii/S2238785425016394
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