Amorf ve nano-boyutlu HoBO3.2.8H2O bileşiğinin sentezi ve karakterizasyonu

Bu çalışmada ilk defa amorf ve nano-yapılı HoBO3.2.8H2O bileşiği, tamponlu-çöktürme yöntemiyle başarılı bir şekilde sentezlendi. Sentezlenen bileşiğin FTIR spektrumunda, 1393 cm-1 ([BO3] asimetrik gerilme), 935 cm-1 ([BO3] simetrik gerilme) ve 681 cm-1 ([BO3] düzlem dışı bükülme) dalga sayılarında üç temel titreşim bandı gözlendi. Bu titreşim bantları, HoBO3.2.8H2O bileşiğinin kimyasal yapısında, düzlem üçgen [BO3] gruplarının bulunduğunu ortaya koydu. XRD analizi ile sentezlenen ürünün amorf özellikte olduğu belirlendi. ICP-MS kullanılarak bileşikteki Ho/B oranı 1.02 olarak hesaplandı. TG/DTG eğrisinde, 303K ve 523 K sıcaklık aralığındaki, yaklaşık % 17.5' lik ilk kütle kaybı, bileşiğin yapısında 2.8 mol kristal su bulunduğunu gösterdi. 523 K ve 693 K sıcaklık aralığındaki ikinci kütle kaybı ise, HoBO3.2.8H2O nano-parçacıklarının yüzeyinde yaklaşık % 4 oranında PEG-2000 moleküllerinin tutunduğunu ortaya koydu. Nano-parçacıkların SEM ve TEM fotoğrafları ile ortalama parçacık boyutu ve standart sapmasının 15±6 nm., şeklinin ise küresele benzer özellikte olduğu ispatlandı. Enerji bant aralığı 5.3 eV olarak hesaplandı. Sentezlenen HoBO3.2.8H2O bileşiğinin ve polimerler ile hazırlanan nano-kompozitlerinin malzeme bilimi ve tıp alanlarındaki uygulamalarda kullanılması öngörülmektedir.

Synthesis and characterization of amorphous and nano-sized HoBO3 .2.8H2O compound

In this study, amorphous and nano-structured HoBO3.2.8H2O compound was successfully synthesized for the first time by the buffered-precipitation method. Three basic vibration bands were observed in the wave numbers of 1393 cm-1 (asymmetric stretching [BO3]), 935 cm-1 ([BO3] symmetric stretching) and 681 cm-1 ([BO3] out-of-plane bending) in the FTIR spectrum of the synthesized compound. These vibration bands revealed that trigonal plane [BO3] groups were present in the chemical structure of the HoBO3.2.8H2O compound. It was determined that the synthesized product was amorphous by XRD analysis. The Ho/B ratio in the compound was calculated as 1.02 using by ICP/MS. The initial mass loss of about 17.5% in the temperature range of 303K and 523K showed 2.8 mol crystal water in the structure of the compound in the TG/DTG curve. The second mass loss in the 523 K and 693 K temperature range revealed that about 4% of the PEG-2000 molecules were retained on the surface of HoBO3.2.8H2O nano-particles. The mean particle size of the nano-particles was 15 nm with 6nm standard deviation and the shape was similar to the sphere according to the SEM and TEM photographs. The Band-gap energy was calculated as 5.3 eV. It is envisaged that the synthesized HoBO3.2.8H2O compound and the nano-composites prepared with the polymers will be used in the applications of material science and medicine.

Keywords:

Holmium borate, nano-structure, amorphous buffered-precipitation method,

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