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Microwave-assisted synthesis and characterisation of divalent metal tungstate nanocrystalline minerals: ferberite, hübnerite, sanmartinite, scheelite and stolzite

机译:微波辅助合成和表征二价金属钨酸盐纳米晶矿物:锰铁矿,硅钙石,三martinite,白钨矿和辉沸石

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摘要

A variety of metal tungstates have been synthesised in a microwave assisted oven atud100 and 150°C and corresponding autogenous water vapour pressure within a timeudframe of 30 minutes to 2 hours. The crystals formed are of submicrometer size andudshow equidimensional and needle-like crystals. Increasing the synthesis time andudtemperature results in the disappearance of the needles and the growth of theudequidimensional crystals. The Raman spectra are consistent with those reported forudthe natural equivalents of these tungstates. The lead tungstate ν1(Ag) mode is observedudat 904 cm-1, while the ν2(Ag) vibration is observed as a strong band at at 326 cm-1udaccompanied by a weak ν2(Bg) . at 356 cm-1. The ν3(Bg) vibration is located aroundud741 cm-1, whereas the ν3(Eg) is found at 751 cm-1. Finally, the ν4(Bg) vibration isudcompletely overlapping with the ν2(Ag) vibration. The band around 271 cm-1 may beudthe equivalent of the infrared active ν4(Au) activated due to strain in the crystal. Theudtwo bands at 190 and 177 cm-1 are ascribed to the ν(Pb-O) and as a translational modeudof the WO4 group in stolzite.
机译:在微波辅助烤箱中,在 ud100和150°C以及相应的自体水蒸气压力下,在30分钟至2小时的时间内合成了多种金属钨酸盐。所形成的晶体具有亚微米级的尺寸,并且显示等维和针状晶体。合成时间和高温的增加会导致针的消失和三维晶体的生长。拉曼光谱与报道的这些钨酸盐的天然等效物一致。观察到钨酸铅的ν1(Ag)模式为904 cm-1,而在326 cm-1处的uv2(Ag)振动为强带,同时伴有弱的ν2(Bg)。在356 cm-1。 ν3(Bg)振动位于 ud741 cm-1附近,而ν3(Eg)则位于751 cm-1。最后,ν4(Bg)振动与ν2(​​Ag)振动完全重叠。 271 cm-1附近的谱带可能等于因晶体中的应变而激活的红外活性ν4(Au)。在190和177 cm-1处的两个波段归因于v(Pb-O),并作为辉石中WO4基团的平移模式。

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