İkili ve üçlü kobalt bazlı metal borürlerin inorganik ergimiş tuz tekniği ile sentezi

Year 2020, Volume: 5 Issue: 1, 12 - 22, 29.03.2020

Zerrin Altıntaş Sina Khoshsima Mehmet Somer , Özge Balcı

https://doi.org/10.30728/boron.613117

Cited By: 1

Abstract

Kristalin metal borür tozları inorganik ergimiş tuz ortamında düşük sıcaklık yöntemi ile sentezlenmiş, ikili ve üçlü metal borür kompozit tozlarının eldesi susuz metal klorürler ve sodyum borhidrür toz karışımları kullanılarak incelenmiştir. Reaksiyonlar, argon altında dikey bir tüp fırında silika tüp içine yerleştirilmiş alüminyum pota içinde gerçekleştirilmiştir. Reaksiyon sonunda elde edilen toz karışımına sıcak su ile liç işlemi yapılarak istenmeyen klorür fazları giderilmiştir. Seçilen bazı saf tozlar, kristalin özelliği geliştirmek amacıyla 1100°C’de tavlama işlemine tabi tutulmuştur. Sentezlenen ve tavlanmış tozların karakterizasyonu, X-ışını difraktometresi (XRD), X-ışını floresans spektrometresi (XRF), taramalı elektron mikroskobu (SEM/EDX) ve dinamik ışık saçma tekniği (DLS) kullanılarak analiz edilmiştir. Sonuçlar, inorganik ergimiş tuz tekniğinin (LiCl/KCl ötektik karışımı) CoCl2, NiCl2 ve NaBH4 toz karışımları arasındaki reaksiyon sırasında oluşan fazlar üzerindeki olumlu etkisini ortaya koymuştur. 750-950°C sıcaklıkları arasında gerçekleşen reaksiyonlarda CoB-Ni2B-CoBx, CoB-Ni4B3 ve CoB-NiB-Ni2Co0.67B0.33 fazlarını içeren ikili ve üçlü metal borür tozları nano boyutta elde edilmiştir. Sentezlenen tozların partikül boyutu ortalama 60 nm civarında hesaplanmıştır.

Keywords

Kobalt, nikel, borür, faz analizi, mikroyapısal karakterizasyon

Supporting Institution

TUBITAK

Project Number

117F178

Thanks

Bu çalışma, “Kobalt – Metal – Bor (Metal=Ni, Fe, Ti) Esaslı Üçlü Metal Borürlerin Klorür Hammaddelerden Alternatif Düşük Sıcaklık Yöntemleri ile Sentezi, Karakterizasyonu ve Katalizör/Magnet/Hibrit Kompozit Üretimi Alanlarına Yönelik Uygulama Çalışmaları” isimli ve 117F178 numaralı “Türkiye Bilimsel ve Teknolojik Araştırma Kurumu (TÜBİTAK)” projesi tarafından desteklenmiştir. Enstrümantal destek için Koç Üniversitesi Yüzey Teknolojileri Araştırma Merkezi (KUYTAM) ve SEM analizleri için Dr. BarışYağcı’ya teşekkürlerimizi sunarız.

The synthesis of binary and ternary cobalt based metal borides by inorganic molten salt technique

Abstract

Crystalline metal boride powders were synthesized via low temperature method in inorganic molten salt medium, and binary and ternary metal boride composite powders were investigated using anhydrous metal chlorides and sodium borohydride powder mixtures. The reactions were carried out in an aluminum crucible placed in a silica tube under argon which was put in a vertical tube furnace. At the end of the reaction, the resulting powder mixture was leached with hot water to remove any undesirable chloride phases. In order to improve crystalline properties, some of pure powders were selected and annealed at 1100°C. Characterization of synthesized and annealed powders was carried out using X-ray diffractometer (XRD), X-ray fluorescence spectrometry (XRF), scanning electron microscopy (SEM / EDX) and dynamic light scattering technique (DLS). The results showed the positive effect of inorganic molten salt technique (LiCl/KCl eutectic mixture) on the formation of phases during the reaction between CoCl2, NiCl2 and NaBH4 powder mixtures. Following the reactions at between 750-950 °C, the binary and ternary metal boride powders consisting of CoB-Ni2B-CoBx, CoB-Ni4B3 ve CoB-NiB-Ni2Co0.67B0.33 phases were obtained. The measured particle size of the final particles had an average of 60 nm.

Keywords

Cobalt, nickel, boride, phase analysis, microstructural characterization

Project Number

117F178

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