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

Yıl 2014, Cilt: 14 Sayı: 3, 565 - 570, 01.12.2014

Engin Berkan Türker Ali Osman Kurt

Öz

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

Anahtar Kelimeler

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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

• Ananthapadmanabhan, P.V., Taylor, P.R. and Zhu, W., 1999. Synthesis of titanium nitride in a thermal plasma reactor. Journal of Alloys and Compounds, 287, 126-129.
• Castro, D.T. and Ying, J.Y., 1997. Synthesis and sintering of nanocrystalline titanium nitride. Nanostructed Materials, Vol. 9, pp. 67-70.
• Huang, Y., Gu, Y., Zheng, M., Xu, Z., Zeng, W. and Liu, Y., 2007. Synthesis of nanocrystalline titanium nitride by reacting titanium dioxide with sodium amide. Materials Letters, 61, 1056-1059.
• Kocatepe Üniversitesi Fen Bilimleri Dergisi, Özel Sayı, 125-130.
• Kurt, A.O. ve Güzelvardar, Y., 2009. Dinamik karbotermal yöntem ile α-Si3N4 seramik tozu üretimi. Afyon Wu, M., 2009. Low temperature synthesis of nanocrystalline titanium nitride from single-source precursor of titanium and nitrogen. Journal of Alloys and Compounds, 486, 223-226.
• Ma, J., Wu, M., Du, Y., Chen, S., Li, G. and Hu, J., 2009. Synthesis of nanocrystalline titanium nitride at low temperature and its thermal stability. Journal Alloys and Compounds, 476, 603-605.
• Sun, J.F., Wang, M.Z., Zhao, Y.C., Li, X.P. and Liang ,B.Y., 2009. Synthesis of titanium nitride powders by reactive ball milling of titanium and urea. Journal of Alloys and Compounds, 482, L29-L31.
• Strokova, Y.I., Gromov, A.A. and Vereshchagin, V.I., 2008. Preparation of ceramic powders based on titanium nitride on heating commercial titanium powder in air. Refractories and Industrial Ceramics, Vol.49 no.4.
• Shiganova, L.A., Bichurov, G.V., Amosov A.P., Titova, Y.P., Ermoshkin, A.A. and Bichurova, P.G., 2011. The self-propagating high-temperature synthesis of a nanostructured titanium nitride powder. Russian Journal of Non-ferrous Metals, 52, no.1, 91-95.
• Peelamedu, R.D., Flemin, M., Agrawal, D.K. and Roy, R., 2002. Preparation of tianium nitride: Microwave- induced carbothermal reaction of titanium dioxide. Journal American Ceramic Society, 85 [1], 117-22.
• Tan, G., Miao, H., Dong, M., and Ren, H., 2006. International Journal and Nanoscience, 5, No.4 & 5, 571-577.
• Zhang, H., Li F., and Jia, Q., 2009. Preparation of titanium nitride ultrafine powders by sol-gel and microwave carbothermal reduction nitridation methods. Ceramics International, Vol. 35, p.1071-1075.
• Xiang, D., Liu, Y., Zhao, Z., Gao, S. and Tu, M., 2007. Reaction sequences and influence factors during carbothermal synthesis of ultrafine TiN powders. Journal Material Science, 42 , 4630-4635.