سنتز و مشخصه یابی نانو ذرات ZrB2 با استفاده از روش سل- ژل
محورهای موضوعی : سنتز موادابوالحسن نجفی 1 , غلامرضا خلج 2 , میلاد رحمانی آزاد 3
1 - دانشگاه آزاد اسلامی واحد ساوه
2 - دانشگاه آزاد اسلامی واحدساوه
3 - دانشگاه آزاد اسلامی، واحد ساوه
کلید واژه: فرایند سل-ژل, مزوپور, نانومواد, دی بوراید زیرکونیوم,
چکیده مقاله :
درتحقیق حاضر، نانوذرات ZrB2 با استفاده از روش سل-ژل سنتز شدند.از آلکوکسیدزیرکونیوم به عنوان منبع Zr واز اسید بوریک به عنوان منبع بور استفاده گردید.اندازه ذرات پیش سازنده در ابعاد نانومتری با استفاده از پارامتر pH در داخل سل کنترل شدندو تشکیل جوانه های اولیه فاز ZrB2 و میزان بلوری شده آنها با استفاده از پارامتر دما بررسی گردید. نتایج DLS نشان داد که اندازه ذرات پیش سازنده در داخل سل در عدد pH کمتر از5، زیر 10 نانومتر بودند. مخلوط کردن ذرات پیش سازنده در ابعاد مولکولی در داخل سل یکی از دلایل مهم در کاهش دمای سنتز ذرات ZrB2 بود. نتایج FTIR روی پیوندهای شیمیایی نشان داد که پیوندZr-B در داخل پودر ژل تشکیل شده است. نتایج DTA نشان داد که جوانه های اولیه ذرات ZrB2 در دمای حدود 1320 درجه سانتی گراد تشکیل شده است. مشاهدات XRD نشان داد که جوانه های اولیه فاز ZrB2در دمای حدود1500 درجه سانتی گراد کریستالیزه شده و رشد یافته اند.تحقیقات سطحی نشان داد که سطح ویژه ذرات سنتز شده ZrB2 معادل 115 متر مربع در گرم است و همچنین سطوح این ذرات متخلخل بوده و اندازه این تخلخل ها در محدوده مزو است. تجزیه و تحلیل SEM نشان داد که اندازه ذرات ZrB2 با مورفولوژی همگن در محدوده 50 نانومتر است. در نهایت، تجزیه و تحلیل ریزساختاری TEM نشان داد که ذرات ZrB2 به طور یکنواخت و منظم در ابعاد بسیار ریز تشکیل شده است.
In the present study, ZrB2 nano powders were synthesized using sol-gel method. Zirconium alkoxide was used as the source of zirconium and boric acid as the source of boron. The size of precursor nanoparticle was controlled using the pH parameter inside the sol, and the formation of primary nuclei of ZrB2 phase and their crystallized amount were investigated using the temperature parameter. To evaluate the mechanism of product formation during the sol-gel process, DLS analysis showed that the size of precursor particle inside the sol at pH less than 5 was below 10 nm. Mixing of precursor particles at molecular level inside the sol was one of the important reasons in reducing the synthesis temperature of ZrB2 particles. FTIR analysis on chemical bonds showed that Zr-O-B bond was formed inside the gel powder.DTA analysis showed that the primary nuclei of ZrB2 particles were formed at a temperature of about 1400 °C. XRD observations proved that the primary nuclei of the ZrB2 phase crystallized and grew at a temperature of about 1500°C. Surface research revealed that the specific surface area of the synthesized ZrB2 particles is equivalent to 115 m2/g, and also the surfaces of these particles are porous, and the size of these porosities is in meso range. SEM analysis showed that the particle size of ZrB2 having homogeneous morphology is about 50 nm. TEM microstructural analysis revealed that ZrB2 particles were formed uniformly and orderly in very fine dimensions.
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