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探讨了一种合成氧化镁晶须的新的工艺方法。首先以活性氧化镁和氯化镁为原料合成了前驱体碱式氯化镁晶须,接着将碱式氯化镁焙烧成氧化镁晶须。分别用X射线衍射仪(XRD)、扫描电镜(SEM)、热重分析仪(TGA)和化学分析,分析了中间体碱式氯化镁和产品氧化镁晶须的成分、形貌和热化学行为。探讨了各个工艺条件对产物的影响,探索出最佳的工艺条件:活性氧化镁与氯化镁的物质的量比在0.08左右,氯化镁溶液的浓度为3mol/L,反应温度40~50℃,陈化时间在48-72h,陈化温度50℃。在此条件下制得了形貌良好的前驱物碱式氯化镁晶须。将碱式氯化镁晶须焙烧,控制升温速率在2—5℃/min,采取分段升温方式升温至600℃,即可制得氧化镁晶须。制得的晶须长度在100μm左右,直径约0.5μm。 相似文献
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碱式硫酸镁烧结法制备氧化镁晶须 总被引:5,自引:0,他引:5
以价格低廉的硫酸镁和氢氧化钠为原料,通过前驱体烧结法制备氧化镁晶须。首先以硫酸镁和氢氧化钠为原料,通过常温反应—水热晶化,制得了结晶良好、具有纤维状外形的前驱体碱式硫酸镁[MgSO4.5 Mg(OH)2.2 H2O]的单一物相。通过控制前驱体的分解速度使其在低温下缓慢分解以保持晶须状外形,然后在高温下烧结,得到烧结良好、分散均匀、长径比大的氧化镁晶须。利用SEM和XRD对产物进行表征,氧化镁晶须是由纳米氧化镁颗粒烧结而成的“假象”体,直径在0.2~1.5μm,长径比≥50。实验证明该工艺简捷、易行、条件温和,为氧化镁晶须的工业化生产提供了有效可行的新途径。 相似文献
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《Ceramics International》2016,42(15):16867-16871
Anew sol-gel route has been applied to synthetize dense Al2O3thin films from aluminum isopropoxide (Al(OPri)3)as raw precursor material. The results show that, in the solution, acetylacetone (AcAc) and aluminum form a complex compound which effectively suppresses the growth of colloidal particles and makes the sol very stable. Al2O3thin films fabricated by spin-coating method and calcined at 500 °C for 3 h possess an amorphous structure and exhibit a highly homogeneous surface texture without evidence of holes or cracks throughout the film. Moreover, the prepared films display a low leakage current and a high transmittance. This new sol-gel route appears to be a highly promising method to synthetize dense Al2O3 thin films from Al(OPri)3, and could provide a wide range of optical and electric applications. 相似文献
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以糖精为原料合成精胺。用1,4-二氯丁烷将糖精烃基化,然后将所碍烃基化产物1,6-二(邻酰基苯磺酰基)-1,6-二氮杂已烷(Ⅰ)在碱性条件下水解得到1,6-二(邻-羟基甲酰基苯磺酰基)-1,6-二氮杂己烷(Ⅱ),(Ⅱ)再与丙烯腈进行Michael加成反应,生成4,9-二(邻-羟基甲酰基苯磺酰基)-4,9-二氮杂十二二腈(Ⅲ),在双催化剂(Raney Ni-Pd/C)存在下使用催化加氢生成5,10-二(邻-羟基甲酰基苯磺酰基)-1,5,10,14-四氮杂十四烷(Ⅳ),后者在盐酸中水解生成精胺盐酸盐(Ⅴ),总收率达到26%。 相似文献
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《Journal of the European Ceramic Society》1999,19(2):155-163
A modified mixed oxide synthetic route has been developed for the synthesis of lead magnesium niobate [Pb(Mg1/3Nb2/3)O3; PMN] and lead iron niobate [Pb(Fe1/2Nb1/2)O3; PFN] powders. The formation of perovskite and pyrochlore phases in the calcined PMN and PFN powders has been investigated as a function of calcination temperature and time by XRD and DTA techniques. The particle size distribution of calcined powders was determined by laser diffraction, with the morphology, phase composition and crystal structure determined via SEM, TEM and EDX techniques. In both cases it has been found that cubic pyrochlore phases in the PbO–Nb2O5 system tend to form, as well as the perovskite phase. However, pyrochlore-free PMN and PFN powders were successfully obtained for a calcination temperature of 800°C for 4 and 3 h, respectively, without the introduction of excess PbO and/or MgO. 相似文献
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A facile route was introduced to prepare homogeneous silicone resin doped with titanium hybrid with high refractive index (RI). Specifically, the hybrids were obtained from the transesterification of hydroxyl-phenyl-vinyl silicone resin and titanium isopropoxide under anhydrous conditions. The structures of hybrid silicone and their corresponding intermediates (hydroxyl-phenyl-vinyl silicone) were characterized by nuclear magnetic resonance spectroscopy (1H NMR, 29Si NMR) as well as Fourier transform infrared spectroscopy (FTIR). The hybrids had a transmittance of more than 88% ranging from 450 nm to 800 nm, a high RI of 1.585, and a lower water vapor permeability of 3.58 g /m2.24h. Results from FTIR showed intensity of Ti-O-Si bond in hybrid decrease with extended the storage time, but the properties of cured hybrids including optical, mechanical, and gas permeability were not influenced. Compared to chips encapsulated with pure silicone, the luminous efficiency of the chips encapsulated with hybrids was improved from 138.6 lm/W to 156.4 lm/W. The thermal shock and hygrothermal aging test also demonstrated the hybrids had a wide range application in light-emitting diode (LED) packaging. © 2019 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47834. 相似文献
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《Reactive and Functional Polymers》2007,67(2):104-112
A novel procedure for synthesizing cellulose acetate particles from ramie fiber was developed. The optimum conditions for preparing cellulose acetate (CA) by reaction of ramie fiber with acetic anhydride under an acidic condition were determined. Reaction was carried out in a ratio of ramie fiber to acetic anhydride of 1:6 (w/w) at 80 °C for 0.5–1 h. When CA was added to a mixture of water and acetone, CA particles with a well-distributed diameter ranging from 5 to 15 μm were obtained. The difference of the CA particle surface was resulting from different washing methods of CA particles with water or aqueous sodium bicarbonate. The highest degree of substitution (DS) of 2.50 for CA by titration method was achieved. A new adsorbent was prepared from CA, which is an excellent sorption regent for organic waste in water. The scanning electron microscopy (SEM) and particle size distribution results showed that the average size of CA particles is about 5–15 μm in diameter. The thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) were used to determine the stability of ramie fiber and CA particle. 相似文献
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We report on a novel, efficient, and one-step approach to prepare single-layer reduced graphene oxide (RGO) suspensions and films using hydroxylamine hydrochloride. The effective chemical reduction of GO was evidenced by a significant increase in the C/O ratio and five orders of magnitude decrease in the GO resistance. Field-effect transistor gas sensors were fabricated using as-produced RGO sheets and the resulting sensor exhibited a fast response and a high sensitivity to low-concentration target gases at room temperature. 相似文献
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Supported nickel phosphides were prepared by treating an amorphous Ni–B alloy on silica–alumina support with phosphine (15 vol.% PH3/H2) at relatively low temperature. The amorphous Ni–B/SiO2–Al2O3 precursors were synthesized by silver-induced electroless plating. The amorphous precursors and catalysts were characterized by X-ray diffraction, high-resolution transmission electron microscopy, selected area electron diffraction, BET surface area and inductively coupled plasma measurements. The transmission electron micrographs of the Ni2P/SiO2–Al2O3 particles with their size ranging from 60 to 80 nm showed that they were homogeneously dispersed over the SiO2–Al2O3 support. The as-prepared catalysts exhibited an excellent catalytic activity in the hydrodesulfurization (HDS) of dibenzothiophene. 相似文献
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《Journal of Industrial and Engineering Chemistry》2014,20(5):3141-3149
Flower shaped PbS nanostructures were prepared by the solvothermal method using propylene glycol and a new sulfuring agent. Novelty of this work is application of a new thio Schiff-base as complexing and sulfuring agent for synthesizing of PbS nanostructures. SEM and TEM was used to examine the surface morphology of the grown samples; also the products were characterized by XRD, SEAD, UV–vis and FT-IR spectra. The results of this paper indicate that the shape and size of lead sulfide nanocrystals can be controlled systematically by setting certain reaction parameters. 相似文献
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Electrochemical synthesis of magnesium borate whisker 总被引:2,自引:0,他引:2
This study successfully synthesised magnesium borate (Mg2B2O5) whiskers using a simpler electrochemical method and lower energy consumption compared with traditional methods. Metallic magnesium was anodised under low-voltage conditions in a borate solution containing ethanol/water mixtures and poisoning agents. The composition and morphology of the magnesium borate whiskers were determined by X-ray diffraction and scanning electron microscope measurements, respectively. The magnesium borate whiskers were 6–8 μm long, each with a diameter of 500 nm. The ratio of the length to the diameter ranges from 12:1 to 16:1. The average current efficiency was 72.6%. 相似文献
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