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Characterization and Physical Properties of Hydrated Zinc Borates Synthesized from Sodium Borates

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Characterization and Physical Properties of Hydrated Zinc Borates Synthesized from Sodium Borates Main Group Met. Chem. 2016; 39(1-2): 59–66 Azmi Seyhun Kipcak, Fatma Tugce Senberber, Meral Yildirim, Sureyya Aydin Yuksel, Emek Moroydor Derun and Nurcan Tugrul* Characterization and physical properties of hydrated zinc borates synthesized from sodium borates DOI 10.1515/mgmc-2016-0002 which enable them to be used as fire retardants in the Received January 12, 2016; accepted February 24, 2016; previously plastic and rubber industries. They also have applications published online March 25, 2016 as char promoters, as anti-arcing agents, in the preserva- tion of wood composites, as modifiers of electrical-optical Abstract: In this study, Zn B O ·3.5H O, a type of a zinc 3 6 12 2 properties and as after-glow suppressant additives (Shen borate hydrate, was synthesized from the sodium borate and Ferm, 1996; Ivankov et al., 2001; Tian et al., 2006; Shi mineral Na B O ·5H O. Two different zinc sources, i.e. 2 4 7 2 et al., 2008; Kilinc et al., 2010). One of the most common ZnSO ·7H O and ZnCl , were used in the hydrothermal syn- 4 2 2 commercial forms of zinc borate is 2ZnO·3B O ·3.5H O thesis. Products were characterized using X-ray diffraction 2 3 2 (Shen and Ferm, 1996). Particles of this material must be (XRD), Fourier transform infrared spectroscopy (FT-IR) and small in size to obtain an effective and uniform distribution. Raman spectroscopy. Product morphologies were studied Additionally, there are other forms of zinc borate hydrates using scanning electron microscopy (SEM). Then optical such as 2ZnO·2B O ·3H O, 4ZnO·B O ·H O, Zn B O ·3H O, absorption characteristics and electrical properties were 2 3 2 2 3 2 2 6 11 2 Zn B O ·7H O and Zn B O ·14H O (Shi et al., 2008; Tian investigated. Based on these results, Zn B O ·3.5H O was 2 6 11 2 3 10 18 2 3 6 12 2 et al., 2008; Gao and Liu, 2009; Gurhan et al., 2009; Zheng obtained under many synthetic conditions as a single phase et al., 2009; Bardakci et al., 2013; Gao et al., 2013). Hydro- with high reaction efficiencies and sub-micrometer (100 nm thermal synthesis is commonly preferred for the prepara- to 1 μm) particle sizes. The electrical resistivity and optical tion of zinc borates. In the hydrothermal procedure, the energy gap were found as 8.8 × 1010 Ω cm and 4.13 eV, respec- zinc and boron sources are dissolved in a liquid medium. tively. The novelty obtained in this study is the synthesis of They react due to the temperature increase and use of zinc borate hydrate compound with high crystallinity with- modification agents (Gurhan et al., 2009; Kilinc et al., out using any modification agent or organic solvent. 2010; Li et al., 2010; Tugrul and Acarali, 2011; Gao et al., Keywords: electrical properties; hydrothermal synthesis; 2013). The characterization of synthesized compounds optical properties; sodium borate; zinc borate hydrate. plays a significant role in scientific studies and industrial applications. The characterization of hydrated zinc borate minerals is commonly based on the determination of the Introduction hydrophobicity and thermal properties based on the ther- modynamic and dehydration behavior (Speghinia et al., Zinc borates are well-known members of the metal borate 2000; Gurhan et al., 2009; Kilinc et al., 2010; Li et al., family because of their high heat resistance properties, 2010; Tugrul and Acarali, 2011; Gao et al., 2013). Gao and Liu (2009) synthesized zinc borate hydrated minerals at the boiling point of the solvent and with a *Corresponding author: Nurcan Tugrul, Faculty of Chemical and reaction time of 11 h. Bardakci et al. (2013) synthesized Metallurgical Engineering, Department of Chemical Engineering, Davutpasa Campus, Davutpasa Street No.127, 34210 Esenler, zinc borate hydrate using the raw materials zinc oxide Istanbul, Turkey, e-mail: [email protected] (ZnO) and boric acid (H3BO3) at 95°C for 2 h. Tugrul and Azmi Seyhun Kipcak, Fatma Tugce Senberber, Meral Yildirim and Acarali (2011) studied the effects of different modification Emek Moroydor Derun: Faculty of Chemical and Metallurgical agents to obtain hydrophobic zinc borate hydrate min- Engineering, Department of Chemical Engineering, Davutpasa erals. Zheng et al. (2009) prepared 4ZnO·B O ·H O after Campus, Davutpasa Street No.127, 34210 Esenler, Istanbul, Turkey 2 3 2 Sureyya Aydin Yuksel: Faculty of Arts and Sciences, Department 7 h using phosphate esters as a modification agent. The of Physics, Davutpasa Campus, Davutpasa Street No. 127, 34210 mineral 2ZnO·3B2O3·3.5H2O was produced using oleic acid Esenler, Istanbul, Turkey as a modification agent at 95°C and 4 h (Li et al., 2010). 60 A.S. Kipcak et al.: Characterization of hydrated zinc borates Gao et al. (2013) investigated the effects of different modi- are given in Table 1 [XRD scores can be explained as; when fication agents on the morphological properties of syn- all of the peak intensities (%) and peak locations matched thesized zinc borate hydrates. Mergen et al. (2012) studied perfectly with the pdf card number of reference mineral, the effects of zinc borate addition to PVC to strengthen the the XRD score of analyzed mineral is equal to 100 (İbroşka flame retardant features. Additionally, the electrical and et al., 2015)]. The type of synthesized zinc borate was optical characterizations of the zinc borate compounds found to be zinc oxide borate hydrate (Zn3B6O12·3.5H2O), have only been studied in the dehydrated forms (Longo with pdf number 00-035-0433. The same zinc borate com- et al., 1998; Speghinia et al., 2000; Ivankov et al., 2001). pound was synthesized in the studies of Bardakci et al. As observed in the literature, the synthesis of zinc (2013), Kipcak et al. (2014a,b) and Kipcak et al. (2015). The borate particles with higher crystallinities requires high XRD scores obtained from the reactions of ZnSO4·7H2O, reaction temperatures ( ≥ 95°C), long reaction times ( ≥ 2 h) Na2B4O7·5H2O, H3BO3 (ZS-T) and ZnCl2, Na2B4O7·5H2O, H3BO3 and modification agents (i.e. oleic acid) to obtain homo- (ZC-T) were plotted against the reaction time and tempera- geneous particle size distributions (Longo et al., 1998; ture using StatSoft Statistica software, where the y-axis Speghinia et al., 2000; Ivankov et al., 2001; Shete et al., shows the XRD score, the z-axis shows the reaction tem- 2004; Tian et al., 2008; Gao and Liu, 2009; Gurhan et al., perature and the x-axis shows the reaction time; this plot 2009; Zheng et al., 2009; Kilinc et al., 2010; Li et al., 2010; is given in Figure 1. The results shown in Figure 1 indicate Tugrul and Acarali, 2011; Mergen et al., 2012; Bardakci that the XRD scores of the zinc borates increased with et al., 2013; Gao et al., 2013). There are two novel contribu- increasing time and temperature. tions of this study. The first contribution is the preparation In the ZS-T experiments, zinc borate was formed of zinc borate hydrate minerals with high crystallinities using a reaction temperature of 70°C and a reaction time under moderate conditions without using any type of of 4 h. In contrast, at the same temperature, the formation organic solvent or modification agent. Second, the effects of zinc borate did not occur in the ZC-T experiments. The of the reaction temperature and reaction time on the zinc borates were coded in the format ‘set code-reaction morphologies of the synthesized minerals were investi- temperature-reaction time’, where the set codes were ‘ZS-T’ gated. Hence the electrical and optical characterizations and ‘ZC-T’. For example, the product synthesized at 80°C of zinc borate compounds have been studied only in the and 4 h using ‘ZnSO7·7H2O-Na2B4O7·5H2O-H3BO3’ was coded dehydrated form, the investigation of the electrical and as ‘ZS-T-80-4’. At a reaction temperature of 80°C, the zinc optical properties of hydrated zinc borate compounds is borate formation started after 1 h of reaction, but complete the second novel contribution of the study. formation was only achieved after 4 h of reaction in the ZS-T set. In contrast, in the ZC-T set after 1 h of reaction, amor- phous zinc borate was obtained. Crystalline zinc borate Results and discussion formed after 2 h of reaction, and better XRD scores were obtained after 3 and 4 h of reaction. At reaction tempera- tures of 80°C and 90°C in the ZS-T set, the formation of zinc Results of the raw material characterization borate began after 1 h of reaction. Complete formation was Based on the X-ray diffraction (XRD) results of the start- ing materials, the zinc source of zinc sulfate heptahydrate Table 1: XRD scores of the synthesized zinc borates. (ZnSO ·7H O) was identified as a mixture of Bianchite 4 2 Temperature (°C) Time (h) Set 1 (ZS-T) Set 2 (ZC-T) (ZnSO4·7H2O, powder diffraction file (pdf) number 01-075- 90 1 6a – 0949) and Goslarite (ZnSO4·6H2O, pdf: 00-009-0395). The a other zinc source was determined to be a mixture of two 2 63 72 3 72 76 different zinc chlorides (ZnCl ) with pdf numbers ‘01-074- 2 4 77 80 0519’ and ‘01-070-1284’. The boron sources were identi- 80 1 6a – a fied as sassolite (H3BO3, pdf: 01-073-2158) and tincalconite 2 27 70 3 68a 75 (Na2B4O7·5H2O, pdf: 00-007-0277). 4 72 77 70 1 14a 23a XRD results of the synthesized zinc borates 2 26a 32a 3 40a 48a 4 69 68a The XRD scores of the zinc borates, which were synthe- sized at different temperatures and different reaction times aCrystal formation was not completed.
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