Comparative Study of Cold Sintering Process and Autoclave Thermo-Vapor Treatment on a ZnO Sample

Analysis of scanning electron microscopy images was used to study the changes in the crystal size distribution of ZnO, which occurred during its processing in an aqueous medium at 220–255 °C and an equilibrium vapor pressure in an autoclave. The results were compared with those of ZnO placed in a di...

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Main Authors: Yurii Ivakin, Andrey Smirnov, Anastasia Kholodkova, Alexander Vasin, Mikhail Kormilicin, Maxim Kornyushin, Vladimir Stolyarov
Format: Article
Language:English
Published: MDPI AG 2021-01-01
Series:Crystals
Subjects:
Online Access:https://www.mdpi.com/2073-4352/11/1/71
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author Yurii Ivakin
Andrey Smirnov
Anastasia Kholodkova
Alexander Vasin
Mikhail Kormilicin
Maxim Kornyushin
Vladimir Stolyarov
author_facet Yurii Ivakin
Andrey Smirnov
Anastasia Kholodkova
Alexander Vasin
Mikhail Kormilicin
Maxim Kornyushin
Vladimir Stolyarov
author_sort Yurii Ivakin
collection DOAJ
description Analysis of scanning electron microscopy images was used to study the changes in the crystal size distribution of ZnO, which occurred during its processing in an aqueous medium at 220–255 °C and an equilibrium vapor pressure in an autoclave. The results were compared with those of ZnO placed in a die for treatment under similar conditions supplemented with mechanical pressure application in the cold sintering process. In both cases, ZnO was treated in the presence of an activating additive: either zinc acetate or ammonium chloride. During autoclaving, a powder consisting of fine ZnO monocrystals was obtained, while the cold sintering process led to ceramics formation. Under vapor pressure and mechanical pressure, the aqueous medium affected ZnO transformation by the same mechanism of solid-phase mobility activation due to the additives’ influence. The higher the content of additives in the medium, and the higher the mechanical pressure, the more pronounced activating effect was observed. Mass transfer during the cold sintering process occurred mainly by the coalescence of crystals, while without mechanical pressure, the predominance of surface spreading was revealed. In the initial ZnO powder, the average crystal size was 0.193 μm. It grew up to 0.316–0.386 μm in a fine-crystalline powder formed in the autoclave and to an average grain size of 0.244–0.799 μm in the ceramics, which relative density reached 0.82–0.96. A scheme explaining the influence of an aqueous medium on the solid-phase mobility of ZnO structure was proposed. It was found that the addition of 7.6 mol% ammonium chloride to the reaction medium causes the processes of compaction and grain growth similar to those observed in ZnO Cold Sintering Process with the addition of 0.925 mol% zinc acetate.
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spelling doaj.art-c174fe6bbb5f48deb593b6ceb3967f682023-12-03T13:30:41ZengMDPI AGCrystals2073-43522021-01-011117110.3390/cryst11010071Comparative Study of Cold Sintering Process and Autoclave Thermo-Vapor Treatment on a ZnO SampleYurii Ivakin0Andrey Smirnov1Anastasia Kholodkova2Alexander Vasin3Mikhail Kormilicin4Maxim Kornyushin5Vladimir Stolyarov6Chemistry Department, M. V. Lomonosov Moscow State University, 119991 Moscow, RussiaMobile Solutions Engineering Center, MIREA-Russian Technological University, 119454 Moscow, RussiaChemistry Department, M. V. Lomonosov Moscow State University, 119991 Moscow, RussiaMobile Solutions Engineering Center, MIREA-Russian Technological University, 119454 Moscow, RussiaMobile Solutions Engineering Center, MIREA-Russian Technological University, 119454 Moscow, RussiaMobile Solutions Engineering Center, MIREA-Russian Technological University, 119454 Moscow, RussiaDepartment of Friction and Wear, Mechanical Engineering Research Institute of RAS, 101990 Moscow, RussiaAnalysis of scanning electron microscopy images was used to study the changes in the crystal size distribution of ZnO, which occurred during its processing in an aqueous medium at 220–255 °C and an equilibrium vapor pressure in an autoclave. The results were compared with those of ZnO placed in a die for treatment under similar conditions supplemented with mechanical pressure application in the cold sintering process. In both cases, ZnO was treated in the presence of an activating additive: either zinc acetate or ammonium chloride. During autoclaving, a powder consisting of fine ZnO monocrystals was obtained, while the cold sintering process led to ceramics formation. Under vapor pressure and mechanical pressure, the aqueous medium affected ZnO transformation by the same mechanism of solid-phase mobility activation due to the additives’ influence. The higher the content of additives in the medium, and the higher the mechanical pressure, the more pronounced activating effect was observed. Mass transfer during the cold sintering process occurred mainly by the coalescence of crystals, while without mechanical pressure, the predominance of surface spreading was revealed. In the initial ZnO powder, the average crystal size was 0.193 μm. It grew up to 0.316–0.386 μm in a fine-crystalline powder formed in the autoclave and to an average grain size of 0.244–0.799 μm in the ceramics, which relative density reached 0.82–0.96. A scheme explaining the influence of an aqueous medium on the solid-phase mobility of ZnO structure was proposed. It was found that the addition of 7.6 mol% ammonium chloride to the reaction medium causes the processes of compaction and grain growth similar to those observed in ZnO Cold Sintering Process with the addition of 0.925 mol% zinc acetate.https://www.mdpi.com/2073-4352/11/1/71oxide ceramicszinc oxidecold sintering processthermo-vapor treatmentsolid-phase mobility in a water mediumcrystal size distribution
spellingShingle Yurii Ivakin
Andrey Smirnov
Anastasia Kholodkova
Alexander Vasin
Mikhail Kormilicin
Maxim Kornyushin
Vladimir Stolyarov
Comparative Study of Cold Sintering Process and Autoclave Thermo-Vapor Treatment on a ZnO Sample
Crystals
oxide ceramics
zinc oxide
cold sintering process
thermo-vapor treatment
solid-phase mobility in a water medium
crystal size distribution
title Comparative Study of Cold Sintering Process and Autoclave Thermo-Vapor Treatment on a ZnO Sample
title_full Comparative Study of Cold Sintering Process and Autoclave Thermo-Vapor Treatment on a ZnO Sample
title_fullStr Comparative Study of Cold Sintering Process and Autoclave Thermo-Vapor Treatment on a ZnO Sample
title_full_unstemmed Comparative Study of Cold Sintering Process and Autoclave Thermo-Vapor Treatment on a ZnO Sample
title_short Comparative Study of Cold Sintering Process and Autoclave Thermo-Vapor Treatment on a ZnO Sample
title_sort comparative study of cold sintering process and autoclave thermo vapor treatment on a zno sample
topic oxide ceramics
zinc oxide
cold sintering process
thermo-vapor treatment
solid-phase mobility in a water medium
crystal size distribution
url https://www.mdpi.com/2073-4352/11/1/71
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