RU2729277C1 - Method of producing ultrahigh-temperature ceramic material based on hafnium carbonitride - Google Patents
Method of producing ultrahigh-temperature ceramic material based on hafnium carbonitride Download PDFInfo
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- RU2729277C1 RU2729277C1 RU2019143363A RU2019143363A RU2729277C1 RU 2729277 C1 RU2729277 C1 RU 2729277C1 RU 2019143363 A RU2019143363 A RU 2019143363A RU 2019143363 A RU2019143363 A RU 2019143363A RU 2729277 C1 RU2729277 C1 RU 2729277C1
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- 229910052735 hafnium Inorganic materials 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 title claims abstract description 14
- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 6
- 239000011215 ultra-high-temperature ceramic Substances 0.000 title claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 20
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 17
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 17
- 238000004137 mechanical activation Methods 0.000 claims abstract description 13
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 11
- 238000007596 consolidation process Methods 0.000 claims abstract description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 6
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 5
- 238000002490 spark plasma sintering Methods 0.000 claims abstract description 5
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 5
- 239000010937 tungsten Substances 0.000 claims abstract description 5
- 230000000977 initiatory effect Effects 0.000 claims abstract description 3
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 abstract description 13
- 238000005516 engineering process Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 14
- 150000001875 compounds Chemical class 0.000 description 9
- 229910052757 nitrogen Inorganic materials 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910052719 titanium Inorganic materials 0.000 description 5
- 239000010936 titanium Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 150000004767 nitrides Chemical class 0.000 description 4
- 239000011575 calcium Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000004071 soot Substances 0.000 description 3
- PXIPVTKHYLBLMZ-UHFFFAOYSA-N Sodium azide Chemical compound [Na+].[N-]=[N+]=[N-] PXIPVTKHYLBLMZ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000000292 calcium oxide Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 150000001247 metal acetylides Chemical class 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000003870 refractory metal Substances 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910052723 transition metal Inorganic materials 0.000 description 2
- -1 transition metal nitrides Chemical class 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 150000001243 acetic acids Chemical class 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000002301 combined effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 101150100117 gfm1 gene Proteins 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 235000011167 hydrochloric acid Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229950011008 tetrachloroethylene Drugs 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
Description
Изобретение относится к области ракетно-космической техники и материаловедения, в частности, к разработке сверхвысокотемпературных материалов (Тпл≥3000°С) на основе гафния (Hf), которые могут быть использованы для протекции наиболее теплонагруженных узлов (воздушно-реактивные двигатели, носовые обтекатели, острые передние кромки крыльев) гиперзвуковых летательных аппаратов (ГЛА), а также могут быть применены в атомной промышленности.The invention relates to the field of rocket and space technology and materials science, in particular, to the development of ultra-high-temperature materials (T PL ≥3000 ° C) based on hafnium (Hf), which can be used to protect the most heat-loaded units (air-jet engines, nose cones , sharp leading edges of the wings) of hypersonic aircraft (GLA), and can also be used in the nuclear industry.
При изготовлении подобного рода материалов для эксплуатации в условиях сверхвысоких температур (выше 2000°С) необходимо обеспечить сочетание ключевых свойств: эффективный отвод тепла, высокая стойкость к окислению, тугоплавкость. Наибольший интерес представляют бинарные и тройные нестехиометрические соединения, а именно: карбиды, нитриды и карбонитриды, переходных металлов IVB и VB групп, в том числе гафния. Получение таких нестехиометрических соединений является непростой задачей из-за трудности регулирования количества азота и/или углерода в системе, а также из-за высоких температур плавления основных компонентов.In the manufacture of materials of this kind for operation at ultra-high temperatures (above 2000 ° C), it is necessary to ensure a combination of key properties: effective heat dissipation, high resistance to oxidation, and refractoriness. Of greatest interest are binary and ternary nonstoichiometric compounds, namely: carbides, nitrides and carbonitrides of transition metals of IVB and VB groups, including hafnium. The preparation of such non-stoichiometric compounds is not an easy task due to the difficulty of controlling the amount of nitrogen and / or carbon in the system, and also because of the high melting points of the main components.
Известен способ получения нитридов переходных металлов, который включает в себя приготовление смеси, содержащей оксид азотируемого металла, порошок азотируемого металла (Hf, Ti, Nb, Zr) и азид щелочного металла, например, азид натрия, формовку образцов, воспламенение образцов при помощи вольфрамовой спирали в атмосфере азота. Данный способ позволяет получать порошки нитридов металлов с выходом нитрида не менее 96% и содержанием азота не меньше 7,17%. (RU 2256604, С01В 21/076, 20.07.2005)There is a known method of obtaining transition metal nitrides, which includes the preparation of a mixture containing a nitrided metal oxide, a nitrided metal powder (Hf, Ti, Nb, Zr) and an alkali metal azide, for example, sodium azide, forming samples, igniting the samples using a tungsten coil in a nitrogen atmosphere. This method makes it possible to obtain powders of metal nitrides with a nitride yield of at least 96% and a nitrogen content of at least 7.17%. (RU 2256604, С01В 21/076, 20.07.2005)
Недостатками данного способа получения материалов являются отсутствие 100% выхода продукта реакции, использование не только порошков, но и их оксидов, что приводит к значительному удорожанию процесса, а также невозможность варьирования количества азота в соединении.The disadvantages of this method of obtaining materials are the absence of 100% yield of the reaction product, the use of not only powders, but also their oxides, which leads to a significant increase in the cost of the process, as well as the impossibility of varying the amount of nitrogen in the compound.
Известен способ получения карбонитрида титана, который включает в себя высокотемпературный синтез титансодержащих соединений в атмосфере азота в ходе магниетермического восстановления смеси тетрахлорида титана и тетрахлорэтилена в соотношении 4,5-5,1 в температурном интервале от 1010°С до 1080°С. Данный способ позволяет получать титансодержащие соединения, в том числе карбонитрид титана, с минимальным содержанием примесей. (RU 2175021, С22В 34/12, С22В 5/04, С01В 31/30, С01В 21/076, 20.10.2001)A known method for producing titanium carbonitride, which includes high-temperature synthesis of titanium-containing compounds in a nitrogen atmosphere in the course of magnesium-thermal reduction of a mixture of titanium tetrachloride and tetrachlorethylene in a ratio of 4.5-5.1 in the temperature range from 1010 ° C to 1080 ° C. This method makes it possible to obtain titanium-containing compounds, including titanium carbonitride, with a minimum content of impurities. (RU 2175021, С22В 34/12, С22В 5/04, С01В 31/30, С01В 21/076, 20.10.2001)
Недостатками данного способа являются невозможность варьирования соотношения C/N по всему диапазону состава, наличие свободного углерода в синтезированном соединении, необходимость использования металла-восстановителя, а также высокая энергозатратность, связанная с поддержанием высоких температур, необходимых для синтеза.The disadvantages of this method are the impossibility of varying the C / N ratio over the entire composition range, the presence of free carbon in the synthesized compound, the need to use a reducing metal, as well as the high energy consumption associated with maintaining the high temperatures required for the synthesis.
Наиболее близким аналогом к заявляемому материалу и способу его получения является способ получения карбидов, нитридов, карбонитридов тугоплавких металлов, который включает в себя смешивание окисла тугоплавкого металла, например, HfO2, ZrO2 или TiO2, с неметаллом, например, с сажей или кальцийсодержащим соединением CaC2, Ca3N2, CaCN2, добавление восстанавливающего металла - кальция, синтез в трубообразном реакторе в атмосфере аргона при температуре от 450 до 800°С, удаление образовавшегося оксида кальция СаО путем растворения в соляной или уксусной кислотах (RU 2225837, С01В 31/30, С01В 21/06, B22F 3/23, 20.03.2004).The closest analogue to the claimed material and the method for its production is a method for producing carbides, nitrides, carbonitrides of refractory metals, which includes mixing an oxide of a refractory metal, for example, HfO 2 , ZrO 2 or TiO 2 , with a non-metal, for example, with soot or calcium-containing compound CaC 2 , Ca 3 N 2 , CaCN 2 , addition of a reducing metal - calcium, synthesis in a pipe-like reactor in an argon atmosphere at a temperature of 450 to 800 ° C, removal of the formed calcium oxide CaO by dissolving in hydrochloric or acetic acids (RU 2225837, С01В 31/30, С01В 21/06, B22F 3/23, 03/20/2004).
Недостатками данного способа получения материалов являются наличие оксида восстанавливающего металла, который необходимо удалять из полученного соединения, энергозатратность, связанная с нагревом трубообразного реактора до температур 450-800°С.The disadvantages of this method of obtaining materials are the presence of a reducing metal oxide, which must be removed from the resulting compound, energy consumption associated with heating the pipe-like reactor to temperatures of 450-800 ° C.
Техническим результатом предлагаемого изобретения является упрощение, значительное уменьшение энергозатрат и времени синтеза материала, в части материала, а также возможность получение компактного керамического материала нестехиометрического состава.The technical result of the proposed invention is to simplify, significantly reduce energy consumption and synthesis time of the material, in terms of material, as well as the possibility of obtaining a compact ceramic material of non-stoichiometric composition.
Технический результат достигается тем, что смесь исходных компонентов Hf и С подвергают предварительной механической активации в высокоэнергетической шаровой планетарной мельнице, затем осуществляют самораспространяющийся высокотемпературный синтез (СВС) подготовленной смеси Hf и С и консолидируют синтезированные порошки. Предварительная механическая активация осуществляется в течение 5-10 минут при соотношении массы шаров к массе смеси 20:1-40:1 и скорости вращения планетарного диска 694-900 об/мин, затем проводится СВС в реакторе в атмосфере азота 0,1-0,8 МПа, инициирование самоподдерживающейся экзотермической реакции осуществляется за счет раскаленной вольфрамовой спирали, консолидация синтезированного порошка карбонитрида гафния осуществляется методом искрового плазменного спекания, при этом в камере создают атмосферу азота и через спекаемый образец пропускают импульсный ток от 1000-5000 А при нагрузке 30-70 МПа, температура консолидации и время выдержки составляют 1900-2200°С и 2-10 минут соответственно.The technical result is achieved by the fact that the mixture of the initial components Hf and C is subjected to preliminary mechanical activation in a high-energy planetary ball mill, then self-propagating high-temperature synthesis (SHS) of the prepared mixture of Hf and C is carried out and the synthesized powders are consolidated. Preliminary mechanical activation is carried out for 5-10 minutes at the ratio of the mass of balls to the mass of the mixture 20: 1-40: 1 and the rotation speed of the planetary disk 694-900 rpm, then SHS is carried out in the reactor in a nitrogen atmosphere of 0.1-0, 8 MPa, the initiation of a self-sustaining exothermic reaction is carried out due to a hot tungsten spiral, the consolidation of the synthesized hafnium carbonitride powder is carried out by the method of spark plasma sintering, while a nitrogen atmosphere is created in the chamber and a pulse current from 1000-5000 A is passed through the sintered sample at a load of 30-70 MPa , the consolidation temperature and the holding time are 1900-2200 ° C and 2-10 minutes, respectively.
Консолидированный сверхвысокотемпературный материал, полученный вышеизложенным способом, представляет собой керамический материал со следующими свойствами: карбонитрид гафния состава HfC0,5Nx, где х варьируются в зависимости от давления азота в камере СВС реактора, с относительной плотностью 95,8-98,7%, твердостью по Виккерсу 20,3-21,3 ГПа и трещинностойкостью 3,1-4,7 МПа м1/2.The consolidated ultra-high-temperature material obtained by the above method is a ceramic material with the following properties: hafnium carbonitride of the composition HfC 0.5 N x , where x varies depending on the nitrogen pressure in the SHS reactor chamber, with a relative density of 95.8-98.7% , Vickers hardness 20.3-21.3 GPa and fracture toughness 3.1-4.7 MPa m 1/2 .
В качестве исходных компонентов для получения сверхвысокотемпературных керамических материалов на основе карбонитрида гафния для протекции наиболее теплонагруженных узлов гиперзвуковых летательных аппаратов используются порошки металлов Hf (порошок гафния) марки ГФМ-1 (ТУ 48-4-176-85 (97)) и С (порошок сажи) П804Т (ТУ 38-1154-88), а также газообразный азот (ГОСТ 9293-74).Powders of metals Hf (hafnium powder) grade GFM-1 (TU 48-4-176-85 (97)) and C (powder) are used as initial components for the production of ultra-high-temperature ceramic materials based on hafnium carbonitride for the protection of the most heat-loaded units of hypersonic aircraft. soot) P804T (TU 38-1154-88), as well as gaseous nitrogen (GOST 9293-74).
Предварительная механическая активация (МА), включающая в себя размол и перемешивание исходных порошков гафния и сажи, осуществляют в высокоэнергетической планетарной шаровой мельнице «Активатор-2S». МА осуществляется в стальных барабанах при помощи стальных шаров в течение 5-10 минут при частоте вращения водила 694-900 об/мин, соотношении массы мелющих шаров к массе порошка 20:1-40:1. МА исходных смесей проводят в атмосфере аргона, давлении которого в барабанах составляет 0,4 МПа. В ходе МА образуются новые поверхности без оксидов, происходит равномерное распределение частиц, а также увеличивается площадь контакта между реагентами, что приводит к ускорению реакции между ними. Предварительная МА является первым этапом предлагаемого способа.Preliminary mechanical activation (MA), which includes grinding and mixing of the initial hafnium and soot powders, is carried out in a high-energy planetary ball mill "Activator-2S". MA is carried out in steel drums using steel balls for 5-10 minutes at a carrier speed of 694-900 rpm, the ratio of the mass of grinding balls to the mass of powder 20: 1-40: 1. MA of the initial mixtures is carried out in an argon atmosphere, the pressure of which in the drums is 0.4 MPa. During MA, new surfaces without oxides are formed, a uniform distribution of particles occurs, and the contact area between the reagents increases, which leads to an acceleration of the reaction between them. Preliminary MA is the first stage of the proposed method.
На втором этапе после предварительной МА активированную порошковую смесь Hf+0,5С подвергают СВС в лабораторном реакторе в атмосфере азота, с целью получения карбонитрида гафния HfC0,5Ny. Давление газа в реакторе при этом составляет 0,1-0,8 МПа.At the second stage, after preliminary MA, the activated powder mixture Hf + 0.5C is subjected to SHS in a laboratory reactor under nitrogen atmosphere in order to obtain hafnium carbonitride HfC 0.5 N y . The gas pressure in the reactor is 0.1-0.8 MPa.
Состав получаемых соединений, а именно значение х, варьируется в зависимости от от давления азота в реакторе.The composition of the compounds obtained, namely the value of x, varies depending on the nitrogen pressure in the reactor.
На третьем этапе способа синтезированные нестехиометрический порошок HfC0,5Ny консолидируют на установке искрового плазменного спекания (ИПС) Spark Plasma Sintering - Labox 650, SinterLand, Япония.At the third stage of the method, the synthesized non-stoichiometric powder HfC 0.5 N y is consolidated in a Spark Plasma Sintering (SP) unit - Labox 650, SinterLand, Japan.
Метод ИПС основан на совместном воздействии высокой температуры и осевого давления при одновременном пропускании импульсов постоянного электрического тока большой амплитуды (до 5000 А) через спекаемый материал и графитовую матрицу, в которой он находится. Импульсный ток способствует равномерному прогреву образца и минимальному воздействию на микроструктуру. Консолидацию осуществляют под нагрузкой 30-70 МПа, при этом время выдержки и температура спекания составляют 2-10 минут и 1900-2200°С соответственно.The IPC method is based on the combined effect of high temperature and axial pressure while simultaneously passing high-amplitude DC electric current pulses (up to 5000 A) through the sintered material and the graphite matrix in which it is located. The pulsed current promotes uniform heating of the sample and minimal impact on the microstructure. Consolidation is carried out under a load of 30-70 MPa, with the holding time and sintering temperature being 2-10 minutes and 1900-2200 ° C, respectively.
Обязательной частью каждого этапа является контроль качества получаемых образцов, который осуществляется как визуальным осмотром, так и при помощи аппаратурных методик.An obligatory part of each stage is quality control of the samples obtained, which is carried out both by visual inspection and by means of instrumental techniques.
Для исследования микроструктуры и фазового состава синтезированных порошков и консолидированных порошков использовались методы растровой электронной микроскопии (РЭМ), рентгеновской дифракции (рентгенофазовый анализ (РФА)) и др. Для консолидированных сверхвысокотемпературных керамик на основе нестехиометрического карбонитрида гафния также осуществлялся контроль пористости, твердости, трещинностойкости, микроструктуры.To study the microstructure and phase composition of the synthesized powders and consolidated powders, methods of scanning electron microscopy (SEM), X-ray diffraction (X-ray phase analysis (XRD)), etc. were used. microstructure.
Сущность способа подтверждается примерами.The essence of the method is confirmed by examples.
Пример 1Example 1
Исходные компоненты Hf и С смешивают в мольном соотношении 2:1 (96,7 масс. % Hf и 3,3 масс. % С). Подготовленную смесь исходных компонентов подвергают предварительной механической активации, в ходе которой происходит перемешивание, измельчение и очистка поверхностей реагентов от оксидов, в планетарной шаровой мельнице в атмосфере аргона, давление которого составляет 0,4 МПа, при частоте вращения мельницы 900 об/мин при соотношении массы шаров к массе порошка 20:1. Использовались шары диаметром 6 мм. Время предварительной механической активации 10 минут.The starting components Hf and C are mixed in a 2: 1 molar ratio (96.7 wt% Hf and 3.3 wt% C). The prepared mixture of the initial components is subjected to preliminary mechanical activation, during which there is mixing, grinding and cleaning the surfaces of the reagents from oxides, in a planetary ball mill in an argon atmosphere, the pressure of which is 0.4 MPa, at a mill speed of 900 rpm with a mass ratio balls to a powder mass of 20: 1. Balls 6 mm in diameter were used. The pre-mechanical activation time is 10 minutes.
Полученную реакционную порошковую смесь подвергают СВС в реакторе при давлении азота 0,1 МПа. Инициируют самоподдерживающуюся экзотермическую реакцию посредствам раскаленной вольфрамовой спирали. В результате получают порошок карбонитрида гафния.The resulting reaction powder mixture is subjected to SHS in a reactor at a nitrogen pressure of 0.1 MPa. A self-sustaining exothermic reaction is initiated by means of an incandescent tungsten coil. As a result, a hafnium carbonitride powder is obtained.
Синтезированный порошок консолидируют, используя метод ИПС. Для этого порошок размещают в цилиндрической графитовой матрице и фиксируют между двумя пуансонами, в тоже время являющимися электродами, затем матрицу помещают в рабочее пространство установки ИПС, в камере создают атмосферу азота, затем через спекаемый образец пропускают импульсный электрический ток. При этом к образцу прикладывают нагрузку в 50 МПа. Консолидацию осуществляют при температуре 1900°С и времени выдержки 2 минуты. Скорость нагрева до температуры спекания составляет 100°С/мин. В результате получают образцы в форме дисков диаметром 15-50 мм и толщиной 2-10 мм.The synthesized powder is consolidated using the IPA method. To do this, the powder is placed in a cylindrical graphite matrix and fixed between two punches, which at the same time are electrodes, then the matrix is placed in the working space of the IPA unit, a nitrogen atmosphere is created in the chamber, then a pulsed electric current is passed through the sintered sample. In this case, a load of 50 MPa is applied to the sample. Consolidation is carried out at a temperature of 1900 ° C and a holding time of 2 minutes. The heating rate to the sintering temperature is 100 ° C / min. As a result, samples are obtained in the form of disks with a diameter of 15-50 mm and a thickness of 2-10 mm.
Сверхвысокотемпературный материал имеет следующие характеристики: относительная плотность 95,8%, твердость по Виккерсу - 20,3 ГПа, трещинностойкость - 3,1 МПа м1/2.The ultrahigh-temperature material has the following characteristics: relative density 95.8%, Vickers hardness - 20.3 GPa, fracture toughness - 3.1 MPa m 1/2 .
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| CN115806277A (en) * | 2021-09-15 | 2023-03-17 | 中南大学 | Novel preparation method of ultrahigh-melting-point hafnium carbonitride powder |
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| CN115151358A (en) | 2022-10-04 |
| WO2021133226A1 (en) | 2021-07-01 |
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