powderИзвестия вузов. Порошковая металлургия и функциональные покрытияPowder Metallurgy аnd Functional Coatings (Izvestiya Vuzov. Poroshkovaya Metallurgiya i Funktsional'nye Pokrytiya)1997-308X2412-8767НИТУ "МИСИС"10.17073/1997-308X-2024-3-38-48powder-894Research ArticleТугоплавкие, керамические и композиционные материалыRefractory, Ceramic, and Composite MaterialsСамораспространяющийся высокотемпературный синтез и искровое плазменное спекание высокоэнтропийного карбонитрида (Hf,Ta,Nb)(C,N)Self-propagating high-temperature synthesis and spark plasma sintering of high-entropy (Hf,Ta,Nb)(C,N) carbonitridehttps://orcid.org/0000-0002-0335-9153СувороваВ. С.SuvorovaV. S.

Вероника Сергеевна Суворова – к.т.н., науч. сотрудник НИЦ «Конструкционные керамические наноматериалы»

Россия, 119049, г. Москва, Ленинский пр-т, 4, стр. 1

Veronika S. Suvorova – Cand. Sci. (Eng.), Researcher at the Research Center of Engineering Ceramic Nanomaterials

4 Bld 1 Leninskiy Prosp., Moscow 119049, Russia

buynevich.vs@misis.ruhttps://orcid.org/0000-0001-9017-9937НепапушевА. А.NepapushevA. A.

Андрей Александрович Непапушев – к.т.н., ст. науч. сотрудник НИЦ «Конструкционные керамические наноматериалы»

Россия, 119049, г. Москва, Ленинский пр-т, 4, стр. 1

Andrey A. Nepapushev – Cand. Sci. (Eng.), Researcher at the Research Center of Engineering Ceramic Nanomaterials

4 Bld 1 Leninskiy Prosp., Moscow 119049, Russia

anepapushev@gmail.comhttps://orcid.org/0000-0002-0358-9987СуворовД. С.SuvorovD. S.

Дмитрий Сергеевич Суворов – инженер кафедры функциональных наносистем и высокотемпературных материалов

Россия, 119049, г. Москва, Ленинский пр-т, 4, стр. 1

Dmitry S. Suvorov – Engineer at the Department of Functional Nanosystems and High Temperature Materials

4 Bld 1 Leninskiy Prosp., Moscow 119049, Russia

suvorov.ds@misis.ruhttps://orcid.org/0000-0002-9387-0237КусковК. В.KuskovK. V.

Кирилл Васильевич Кусков – вед. эксперт НИЦ «Конструкционные керамические наноматериалы»

Россия, 119049, г. Москва, Ленинский пр-т, 4, стр. 1

Kirill V. Kuskov – Leading Expert at the Research Center of Engineering Ceramic Nanomaterials

4 Bld 1 Leninskiy Prosp., Moscow 119049, Russia

kkuskov@misis.ruhttps://orcid.org/0000-0001-5168-4885МосковскихД. О.MoskovskikhD. O.

Дмитрий Олегович Московских – к.т.н., директор НИЦ «Конструкционные керамические наноматериалы»

Россия, 119049, г. Москва, Ленинский пр-т, 4, стр. 1

Dmitry O. Moskovskikh – Cand. Sci. (Eng.), Director of the Research Center of Engineering Ceramic Nanomaterials

4 Bld 1 Leninskiy Prosp., Moscow 119049, Russia

mos@misis.ruНациональный исследовательский технологический университет «МИСИС»РоссияNational University of Science and Technology “MISIS”Russian Federation2024160620241833848Copyright © Суворова В.С., Непапушев А.А., Суворов Д.С., Кусков К.В., Московских Д.О., 20242024Суворова В.С., Непапушев А.А., Суворов Д.С., Кусков К.В., Московских Д.О.Suvorova V.S., Nepapushev A.A., Suvorov D.S., Kuskov K.V., Moskovskikh D.O.Данная работа распространяется под лицензией Creative Commons Attribution 4.0.This work is licensed under a Creative Commons Attribution 4.0 License.https://powder.misis.ru/jour/article/view/894

В работе комбинацией методов механического активирования (МА), самораспространяющегося высокотемпературного синтеза (СВС) и искрового плазменного спекания (ИПС) получен плотный высокоэнтропийный карбонитрид (Hf,Ta,Nb)(C,N) и исследованы его свойства. Для реализации процесса СВС смесь исходных металлов с углеродом подвергали предварительной обработке в планетарной мельнице в низкоэнергетическом режиме, при котором скорость вращения барабанов составляла 350 об/мин. Была исследована эволюция микроструктуры и фазового состава в процессе МА. Установлено, что после обработки в течение 60 мин происходит формирование слоистых композиционных частиц Hf/Ta/Nb/C, имеющих средний размер порядка 15 мкм и состоящих из субмикронных слоев Hf, Ta, Nb и C. При этом, согласно данным рентгенофазового анализа, взаимодействия компонентов в барабане не происходило. СВС реакционных смесей Hf/Ta/Nb/C проводили в атмосфере азота (P = 0,8 МПа), после синтеза в порошке были обнаружены две изоморфные фазы (Hf,Ta,Nb)(C,N) пространственной группы Fm-3m (225) с различными параметрами решетки: а = 0,4476 нм (71 мас. %) и a = 0,4469 нм (22 мас. %). Морфология частиц после СВС повторяла морфологию композиционных частиц после МА, средний размер агломератов составлял 10 мкм. Сформировавшиеся в процессе СВС агломераты состояли из частиц округ­лой формы размером от 0,5 до 2 мкм и пор, что обусловлено плавлением металлических компонентов в зоне горения, быстрой кристаллизацией зерен продукта из расплава и их последующей рекристаллизацией. Процесс ИПС при температуре 2000 °С, давлении прессования 50 МПа и времени выдержки 20 мин позволил получить однофазный высоко­энтропийный материал (Hf0,33Ta0,33Nb0,33)C0,5N0,3 с параметром решетки 0,4482 нм, который характеризовался высокой относительной плотностью 98 %, твердостью 21,5 ± 0,4 ГПа, модулем Юнга 458 ± 10 ГПа и значением трещиностойкости 3,7 ± 0,3 МПа∙м1/2.

In this research, we combined mechanical activation (MA), self-propagating high-temperature synthesis (SHS), and spark plasma sintering (SPS) methods to obtain a dense high-entropy (Hf,Ta,Nb)(C,N) carbonitride and studied its properties. To implement the SHS process, a mixture of initial metals and carbon was subjected to pre-treatment in a planetary mill in the low-energy mode, in which the jar rotation speed reached 350 rpm. We studied the evolution of microstructure and phase composition during the MA process. It has been established that after 60 min of treatment, Hf/Ta/Nb/C layered composite particles consisting of Hf, Ta, Nb and C submicron layers, with an average size of about 15 μm, were formed. However, according to the X-ray diffraction analysis, the components in the jar did not interact. SHS of Hf/Ta/Nb/C reactive mixtures was performed in a nitrogen atmosphere (P = 0.8 MPa); after synthesis, two isomorphic (Hf,Ta,Nb)(C,N) phases of the Fm-3m (225) space group with lattice parameters of a = 0.4476 nm (71 wt. %) and a = 0.4469 nm (22 wt. %) were revealed in the powder. After SHS, the average size of agglomerates was 10 μm and their morphology resembled that of composite particles after MA. The agglomerates formed during SHS consisted of pores and round-shaped particles ranging in size from 0.5 to 2 μm, which was caused by the melting of metal components in the combustion zone and rapid crystallization of product grains from the melt, followed by subsequent recrystallization. Spark plasma sintering at a temperature of 2000 °C, a pressure of 50 MPa and a holding time of 20 min enabled to obtain a single-phase high-entropy (Hf0.33Ta0.33Nb0.33 )C0.5N0.3 material with a lattice parameter of 0.4482 nm characterized by a high relative density of 98 %, a hardness of 21.5 ± 0.4 GPa, a Young’s modulus of 458 ± 10 GPa, and a fracture toughness value of 3.7 ± 0.3 MPa∙m1/2.

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The authors declare that there are no conflicts of interest present.