Production of TİN Ceramic Powders via Dynamic Carbothermal Reduction-Nitridation Method

Abstract

Carbothermal reduction – nitridation (CRN) technique is based on the method of producing ceramic powders in an atmosphere controlled environment with the help of thermal activation, where oxides are being reduced and remaining in the system are reacted following the several chemical reactions simultaneously with nitrogen to form metal-nitrides. In the dynamic CRN method (DCRN), reactants in solid form are moved continuously during reaction period within the system. This has positive effects on the formation time of nitrides and the physical properties of the powders produced. In this study, titanium nitride (TiN) powders of high purity and fine grain size was aimed to produce from high-purity ninosized titanium oxide (TiO2) powders and carbon black under nitrogen atmosphere using the DCRN process. TiO2+C mixture, having high volatility due to very fine grain size, was granulated (Ø 0,5 – 2mm) before taken them in to the CRN and DCRN processes.The XRD analysis made on the final powders after CRN and DCRN revealed that fully conversion of TiN in the static (CRN) system could be achieved above 8 hours at 1400 oC, whereas only 4 hours was sufficient to obtain TiN powders using DCRN system. © Afyon Kocatepe Üniversitesİ

Keywords

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Dinamik Karbotermal İndirgeme-Nitrürleme Yöntemiyle TİN Seramik Tozu Üretimi

Öz

Seramik toz üretiminde karbotermal indirgeme – nitrürleme (KTİN) yöntemi atmosfer kontrollü bir ortamda termal aktivasyon sonucu metal oksit(ler)in indirgenmesi suretiyle sistemde oluşan kalıntıların eş zamanlı olarak ortamda mevcut nitrojenle bir dizi kimyasal tepkimeler sonucu reaksiyona girmesi ile ince tozlar halinde metal-nitrürlerin oluşturulması ilkesine dayanmaktadır. Dinamik KTİN (DKTİN) yönteminde ise katı formda reaksiyon bileşenleri reaksiyon süresince hareket ettirilmektedir. Bu durum nitrür oluşum süresini ve oluşan seramik yapının (tozun) fiziksel özelliklerini olumlu yönde etkilemektedir. Bu çalışmada yüksek saflıkta (%99,5) titanyum oksit (TiO2) ve karbon karası kullanılarak DKTİN ile azot atmosferi altında yüksek saflığa ve çok küçük tane boyutuna sahip titanyum nitrür (TiN) tozu üretimi hedeflenmiştir. Nanometre ölçülerde başlangıç tane boyutuna sahip ve uçuculuğu yüksek olan TiO2+C karışımı kontrollü granülleme (Ø 0,5 – 2mm) yapılmış, elde edilen granüller tüp fırın içerisinde statik ve dinamik ortamlarda karbotermik reaksiyona tabi tutulmuştur. Süreç sonrası ürünlerin XRD ile yapılan faz analizleri statik sistemde 1400 o C`de 8 saatin üzerine çıkılmasıyla üretilebilen TiN tozlarının DKTİN sistemi kullanılarak 1400 o C`de 4 saatte elde edilebileceğini göstermiştir.

Anahtar Kelimeler

• Titanyum Nitrür, Dinamik Karbotermal İndirgeme–Nitürleme, Toz Üretimi

Kaynakça

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