Ultrasonic-Assisted Synthesis of Zinc Borates: Effect of Boron Sources

2020 ◽  
Vol 42 (6) ◽  
pp. 839-839
Author(s):  
Fatma Tugce Senberber Dumanli Fatma Tugce Senberber Dumanli ◽  
Azmi Seyhun Kipcak Azmi Seyhun Kipcak ◽  
Duygu Sena Vardar and Nurcan Tugrul Duygu Sena Vardar and Nurcan Tugrul

Sonochemistry meaning ultrasound-assisted chemistry plays an important role in the synthesis of inorganic compounds. Among these inorganic compounds, zinc borates are used for the flame-retarding agent. In this study using zinc chloride (ZnCl2), boric acid (H3BO3), Na2B4O7and#183;10H2O, Na2B4O7and#183;5H2O and NaOH as raw materials, a zinc borate compound in the formulae of Zn3B6O12and#183;3.5H2O was obtained using an ultrasonic probe. Crystal structures of samples were identified using X-ray diffraction (XRD). The symmetric and asymmetric stretching between boron and oxygen atoms were searched by Fourier-transform infrared (FT-IR) and Raman spectroscopies. The effects of boron sources on sample morphology were examined by scanning electron microscopy (SEM). From the results, it was seen that Zn3B6O12and#183;3.5H2O can easily be produced from these raw materials with the synthesis parameters of 80-90and#176;C and 40-55 min. From the SEM results, it was seen that the minimum particle size obtained was 172 nm. Reaction efficiencies were calculated between 79.6 and 94.0 and#177; 0.5%. Thermal feature of the obtained pure phase, investigated with the thermogravimetric analyses. The dehydration of the synthesized Zn3B6O12and#183;3.5H2O was seen between 262 and 413and#176;C with a total mass loss of 13.25%.

2020 ◽  
Vol 43 (1) ◽  
pp. 7-14
Author(s):  
Ali Can Ersan ◽  
Azmi Seyhun Kipcak ◽  
Meral Yildirim Ozen ◽  
Nurcan Tugrul

AbstractRecently, sonochemistry has been used for the synthesis of inorganic compounds, such as zinc borates. In this study using zinc sulphate heptahydrate (ZnSO4·7H2O) and boric acid (H3BO3) as starting materials, a zinc borate compound in the form of Zn3B6O12·3.5H2O was synthesized using an ultrasonic probe. Product’s characterization was carried out with using X-ray diffraction (XRD), Scanning electron microscopy (SEM), Fourier-transform infrared spectroscopy (FT-IR) and Raman spectroscopy. Zinc borate compound’s chemical bond structure was observed with Raman and FTIR. From the XRD results it was seen that Zn3B6O12·3.5H2O can be quickly synthesized upon heating at 80°C and 85°C (55 min) or 90°C (45 min) in very high yield (>90%). The minimum particle size obtained was ~143 μm from the SEM results. Zinc borate compound was synthesized at a lower temperature in less time than other synthesized zinc metal compound in literature.


2014 ◽  
Vol 2014 ◽  
pp. 1-12 ◽  
Author(s):  
Azmi Seyhun Kipcak ◽  
Nil Baran Acarali ◽  
Emek Moroydor Derun ◽  
Nurcan Tugrul ◽  
Sabriye Piskin

Magnesium borate (MB) is a technical ceramic exhibiting high heat resistance, corrosion resistance, great mechanical strength, great insulation properties, lightweightness, high strength, and a high coefficient of elasticity. Zinc borate (ZB) can be used as a multifunctional synergistic additive in addition to flame retardant additives in polymers. In this study, the raw materials of zinc oxide (ZnO), magnesium oxide (MgO), and boric acid (H3BO3) were used in the mole ratio of 1 : 1 : 9, which was obtained from preexperiments. Using the starting materials, hydrothermal synthesis was applied, and characterisation of the products was performed using X-Ray diffraction (XRD) and Fourier transform infrared (FT-IR) and Raman spectroscopies. The forms of Zn3B6O12·3.5H2O, MgO(B2O3)3·7(H2O), and Mg2(B6O7(OH)6)2·9(H2O) were synthesised successfully. Moreover, the surface morphology was investigated using scanning electron microscopy (SEM), and the B2O3content was determined. In addition, the reaction yields were calculated. The results of the B2O3content analysis were in compliance with the literature values. Examination of the SEM images indicated that the obtained nanoscale minerals had a reaction efficiency ranging between 63–74% for MB and 87–98% for ZB. Finally, the fire-retarding properties of the synthesised pure MBs, pure ZBs, and mixtures of MB and ZB were determined using differential thermal analysis and thermal gravimetry (DTA-TG) and differential scanning calorimetry (DSC).


Materials ◽  
2021 ◽  
Vol 14 (13) ◽  
pp. 3474
Author(s):  
Katarzyna Uram ◽  
Milena Leszczyńska ◽  
Aleksander Prociak ◽  
Anna Czajka ◽  
Michał Gloc ◽  
...  

Rigid polyurethane foams were obtained using two types of renewable raw materials: bio-polyols and a cellulose filler (ARBOCEL® P 4000 X, JRS Rettenmaier, Rosenberg, Germany). A polyurethane system containing 40 wt.% of rapeseed oil-based polyols was modified with the cellulose filler in amounts of 1, 2, and 3 php (per hundred polyols). The cellulose was incorporated into the polyol premix as filler dispersion in a petrochemical polyol made using calenders. The cellulose filler was examined in terms of the degree of crystallinity using the powder X-ray diffraction PXRD -and the presence of bonds by means of the fourier transform infrared spectroscopy FT-IR. It was found that the addition of the cellulose filler increased the number of cells in the foams in both cross-sections—parallel and perpendicular to the direction of the foam growth—while reducing the sizes of those cells. Additionally, the foams had closed cell contents of more than 90% and initial thermal conductivity coefficients of 24.8 mW/m∙K. The insulation materials were dimensionally stable, especially at temperatures close to 0 °C, which qualifies them for use as insulation at low temperatures.


2010 ◽  
Vol 123-125 ◽  
pp. 1291-1294 ◽  
Author(s):  
Bin Lü ◽  
Jian Zhong Ma ◽  
Dang Ge Gao ◽  
Lei Hong

Modified rapeseed oil(MRO) was prepared by using rapeseed oil, ethylene diamine and acrylic acid as the raw materials. Modified rapeseed oil/montmorillonite(MRO/MMT) nanocomposite was prepared by using modified rapeseed oil and montmorillonite. The emulsifying properties of MRO and MRO/MMT were determined respectively. Fourier transforms infrared spectrometry (FT-IR) and Transmission Electron microscope (TEM) results showed that MRO/MMT was prepared successfully. X-ray diffraction (XRD) results showed that modified rapeseed oil could smoothly enter the interlayer of montmorillonite, and modified the montmorillonite; with an increase in the amount of montmorillonite, the layer spacing of montmorillonite in the MRO/MMT lower after the first increase. The results of emulsifying properties indicated that emulsifying properties of MRO/MMT was better than MRO.


2016 ◽  
Vol 703 ◽  
pp. 321-325
Author(s):  
Hai Feng Chen ◽  
Jia Mei Chen ◽  
Zhi Xue Pan

In this work, novel Cu/BiVO4 photocatalyst were prepared by a low-temperature solid state grinding method using Bi (NO3)3•5H2O, NH4VO3 and Cu (NO3)2•2H2O as raw materials. The structure and properties of the samples were characterized by Infrared Spectroscopy (FT-IR), X-ray diffraction (XRD) and UV-vis diffused reflectance spectroscopy (DRS); Using the degradation of methyl orange (MO) as the probe, it was simulated as the degradation of sewage under the visible light to study the influence of the illumination time and the amount of photocatalysts. Compared with the pure BiVO4, the visible-light absorption scope of BiVO4 was broadened by doping Cu, the UV-Visible absorption edges were slightly red shift and the band gap was narrower. Comparatively speaking, the results indicted that the doped Cu enhanced the photocatalytic activities of BiVO4.


2017 ◽  
Vol 19 (1) ◽  
pp. 81-88 ◽  
Author(s):  
Meral Yildirim ◽  
Azmi Seyhun Kipcak ◽  
Emek Moroydor Derun

Abstract In this study, sonochemical-assisted magnesium borate synthesis is studied from different boron sources. Various reaction parameters are successfully applied by a simple and green method. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and Raman spectroscopies are used to characterize the synthesized magnesium borates on the other hand surface morphologies are investigated by using scanning electron microscope (SEM). The XRD analyses showed that the products were admontite [MgO(B2O3)3 · 7(H2O)] with JCPDS (Joint Committee on Powder Diffraction Standards) no. of 01-076-0540 and mcallisterite [Mg2(B6O7(OH)6)2 · 9(H2O)] with JCPDS no. of 01-070-1902. The results that found in the spectroscopic studies were in a good agreement with characteristic magnesium borate bands in both regions of infra-red and visible. According to SEM results, obtained borates were in micro and sub-micro scales. By the use of ultrasonication, reaction yields were found between 84.2 and 97.9%. As a result, it is concluded that the sonochemical approach is a practicable synthesis method to get high efficiency and high crystallinity in the synthesis magnesium borate compounds.


2012 ◽  
Vol 573-574 ◽  
pp. 110-114 ◽  
Author(s):  
Jin Xia ◽  
Ri Ya Jin ◽  
Kai Xuan Guo ◽  
Si Jing Yang

Titanium dioxide powders were synthesized by ultrasonic-assisted hydrolysis reaction of titanium tetra-isopropoxide at the low-temperature. The samples were characterized by Fourier transform infrared spectroscopy (FT-IR), powder X-ray diffraction (XRD). The photocatalytic activity of samples were investigated by the degradation of methyl orange under UV light radiation (6W, λ= 352nm) at room temperature. The results indicated that the products were mainly composed of high homogeneity anatase phases, and the methyl orange degradation rate can reach more than 90% under ultraviolet irradiation 180min. The photocatalytic activity of the samples prepared by ultrasonic method is higher than that of the samples prepared by conventional hydrolysis method.


2011 ◽  
Vol 121-126 ◽  
pp. 3401-3405 ◽  
Author(s):  
Ju Hua Luo

Lithium niobate powders were prepared by mechanochemical treatments using Li2CO3 and Nb2O5 as raw materials. Scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR) were employed to evaluate the morphologies and structures of samples. The mechanism of LiNbO3 formation of the ground mixture samples was discussed. The crystal structure of mixture was collapsed into a disordered structure, which increased with increasing grinding time. At the same time, the specific surface area increase and the bond energy reduction of the mixture occurred. Consequently, high energy ball milling enables increase of the internal energy, reduction of the activation energy, and improvement of the uniform mixing stage, which resulted in direct formation of singal phase LiNbO3 at a low temperature (500°C). However, the temperature must reach 1200°C for the traditional method.


2011 ◽  
Vol 284-286 ◽  
pp. 2268-2271 ◽  
Author(s):  
Ju Hua Luo

Mn-ferrite powders were prepared by mechanochemical treatments using MnO2and Fe2O3as raw materials. Scanning electron microscopy (SEM), X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), vibrating sample magnetometry (VSM) were employed to evaluated the morphologies and structures of samples. The results indicated that the starting mixture became amorphous stage after ball-milled for 40h, and single phase MnFe2O4could be obtained after annealed at 1200°C for 2h. In comparison with the traditional firing method , the mechanochemical method benefited achieving the higher saturation magnetization, which indicated that the samples had a better magnetic properties.


2012 ◽  
Vol 1376 ◽  
Author(s):  
J.C. Pérez-Reyes ◽  
G. Carbajal-De la Torre ◽  
M. A. Espinosa-Medina ◽  
L. A. Ibarra-Bracamontes ◽  
M. Villagómez-Galindo ◽  
...  

ABSTRACTOsteoarthritis is a very complex illness of the joints that affects cartilage and subcondral bone. At the last years, researching has been focused in the development and characterization of composite materials, evaluating their structural properties. Some o those composite materials are constituted by organic and inorganic compounds forming hybrids. These materials can improve their properties due to the interaction of reinforcement hard particles in the polymeric matrix. The interest on the composite biomaterials has been increased on the biomedical applications such as tissue regenerating based in synthetic polymers with biodegradable and biocompatible properties whose can be reinforced by calcium phosphates. In this sense, hydroxyapatite [Ca10(PO4)6(OH)2] is often used for biological implants due its mineral phase similitude with bone microstructure and tissue compatibility. Similarly, polylactic acid (PLA) is a used polymer for implant applications due physicochemical and biocompatibility properties, and short degradation time also. In order to obtain a composite that can be used as a regenerating material on the osteoarthritis problem, in this work a (90/10 wt.%) polylactic/hydroxyapatite hybrid composite was produced by chemical synthesis and characterized by X-ray diffraction, SEM, FT-IR and TGA/DSC techniques.


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