Co-synthesis of zirconium boride/silicide/oxide composite powders by magnesiothermic reduction

Year 2022, , 552 - 559, 31.12.2022

Didem Ovalı Döndaş

https://doi.org/10.30728/boron.1177551

Abstract

This study uses a magnesiothermic reduction method to investigate the co-synthesis of zirconium boride, silicides, and oxide powder composites using ZrO2, B2O3, Si, and Mg initial powders. The synthesis of high-temperature ceramic powders is examined through milling durations, reduction temperatures, and excess magnesium addition. Thermochemical analysis of probable reaction products was conducted by the Factsage software. According to the results, the thermochemical predictions and resultant powder phases showed good coherency. High-energy milling has a significant effect on the formation of the zirconium boride phase after annealing. However, extended milling time and higher annealing temperature have no significant effects on the composition of the constituted composite powders according to the X-ray diffraction results. An annealing temperature of 600 ºC was enough to obtain ZrB2-based ceramic composite powders. In the final powder phases, the excess magnesium addition to the stoichiometric displays an important feature. After the milling, annealing, and leaching procedure, the stoichiometric powder composition comprises ZrB2, ZrSi, ZrSi2, ZrO2, and MgSiO2, and excess Mg added powders have the ZrB2, ZrSi, ZrSi2, ZrO2 phases in their structure. Scanning electron microscopy analysis was utilized to observe the morphologies of the powders throughout each step of the synthesis procedure and revealed the finely structured morphology of synthesized powders.

Keywords

ZrB2, ZiSi2, Magnesiothermic reduction, High-energy ball milling, X-ray diffraction

Zirkonyum borür/silisit/oksit kompozit tozlarının magnezyotermik indirgeme ile sentezi

Abstract

Bu çalışmada, ZrO2, B2O3, Si ve Mg başlangıç tozları kullanılarak zirkonyum borür, silisit ve oksit kompozit tozlarının magnezyotermik indirgeme yöntemi kullanılarak birlikte sentezlenmesi araştırılmıştır. Seramik tozlarının sentezlenmesinde incelenen üretim parametreleri farklı öğütme süreleri, tavlama sıcaklıkları ve fazla magnezyum ilavesidir. Kullanılan başlangıç toz sisteminin termokimyasal analizi, Factsage yazılımı kullanılarak yapılmıştır. Sonuçlara göre, termokimyasal tahminler ve elde edilen toz kompozisyonları tutarlılık göstermiştir. Yüksek enerjili öğütmenin, tavlama sonrası zirkonyum borür fazının oluşuması üzerinde önemli bir etkisi olduğu görülmüştür. Bunun yanında, x-ışını kırınımı sonuçlarına göre, uzatılan öğütme süresinin ve farklı tavlama sıcaklıklarının, oluşturulan kompozit tozların bileşimi üzerinde çok belirgin bir etkiye sahip olmadığı görülmüştür. ZrB2 esaslı seramik kompozit tozlarının elde edilmesi için 600 ºC tavlama sıcaklığının yeterli olduğu görülmüştür. Stokiyometrik başlangıç toz kompozisyonuna, yapılan fazla magnezyum ilavesinin sentezlenen toz kompozisyonlarındaki fazları değiştirdiği saptanmıştır. Öğütme, tavlama ve liç işlemlerinden sonra stokiyometrik toz bileşimi ZrB2, ZrSi, ZrSi2, ZrO2 ve Mg2SiO4 içerirken, fazla Mg katkılı tozların yapısında ZrB2, ZrSi, ZrSi2, ZrO2 fazları bulunmaktadır. Sentez prosedürünün her aşaması boyunca tozların morfolojilerini gözlemlemek için taramalı elektron mikroskobu analizi kullanılmıştır ve sentezlenen tozların ince yapılı bir morfolojiye sahip olduğu görülmüştür.

Keywords

ZrB2, ZiSi2, Magnezyotermik reaksiyon, Yüksek enerjili öğütme, X-ışınları difraksiyonu

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