反应温度对电石渣合成纳米碳酸钙形貌的影响

为了提高电石渣的附加值,在未使用晶型诱导剂的情况下,研究反应温度对电石渣合成纳米碳酸钙形貌的影响。结果表明:反应温度为3、8℃时,分别生成板片状和类球状方解石型碳酸钙;温度为10、80℃时,分别生成球状球霰石型碳酸钙和针状文石型碳酸钙,且球状、类球状和针状碳酸钙纳米颗粒的平均颗粒粒径分别为90、70、80 nm。     

立方纳米氧化镁的制备及形貌表征

利用直接沉淀法得到片状氢氧化镁前驱体,再结合煅烧法得到立方纳米氧化镁;为优化实验条件,讨论氢氧化镁前驱体及氧化镁的形貌影响因素。实验结果表明:当氢氧化钠的物质的量浓度为0. 5 mol/L、镁盐物质的量浓度为0. 4 mol/L时,可得到分散性较好的片状氢氧化镁前驱体;当氯化镁的纯度较高时,氢氧化镁结晶度进一步提高,呈现出分散均匀的花瓣状薄片形貌;煅烧温度控制在1 150℃时,所得到的立方纳米氧化镁分散性较好。     

形貌可控的TiO2纳米晶的溶胶凝胶-水热法组合制备

以四烷基氢氧化铵为结构导向剂,正丁醇为结构导向助剂,采用溶胶凝胶-水热法组合制备了不同形貌的二氧化钛纳米晶.通过TG/DTA、TEM、XRD、DLS等手段对产物进行了结构和形貌表征.研究表明,通过选择结构导向剂的烷基种类可分别得到四方型和纺锤型纳米晶,在一定范围内改变其浓度则可以控制晶体的晶化度、分散性和颗粒尺寸.     

沉淀反应制备碳酸钙粒子及其形貌和结构控制

调节CaCl₂与Na₂CO₃简单沉淀反应的实验条件制备了微米及纳米级CaCO₃粒子, 探讨了晶型控制剂种类及用量、反应物浓度、分散方式等多种因素对CaCO₃粒子形貌及其分散性等性能的影响。使用光学显微镜、扫描电镜、动态光散射激光粒度仪、X射线衍射等对产物进行了表征。结果表明, 无晶型控制剂时, 所得产物主要为大小均一方解石晶型CaCO₃, 尺寸为4~5 μm。相对于机械搅拌, 超声波分散制备粒子的形貌更规整, 尺寸更均一。在超声波分散条件下, 分别采用三聚磷酸钠(STP)、羧甲基纤维素钠(CMC)和聚苯乙烯磺酸钠(PSS)为晶型控制剂, 并改变其用量通过沉淀反应制备了CaCO₃粒子, 对所得产物的结构及其形貌进行了表征。结果表明, 晶型控制剂及其用量对CaCO₃粒子的结构及其形貌有重要影响。使用STP为晶型控制剂时, 除了用量极低的条件下(≤0.10wt%)形成主要为球霰石结构的产物外, 一般都形成无定型CaCO₃; 使用CMC时, 一般都形成方解石结构产物; 与CMC相反, 使用PSS为晶型控制剂时, 得到的主要是球霰石结构产物, 掺杂少量方解石结构产物。对晶型控制剂在沉淀反应中的作用机理进行了讨论。     

超声模板法制备纳米二氧化铈的研究

采用超声模板法结合共沸蒸馏和水热法处理前驱体成功制备出了纳米CeO2颗粒,通过TEM、XRD、FT-IR、UV-Vis等分析方法对产物形貌、结构和性能进行了表征;研究了模板剂的性质、模板剂的用量、共沸蒸馏和水热处理对纳米CeO2颗粒形态、尺寸的影响。实验结果表明,与OP-10和SDBS比较,CTAB最适合应用于制备纳米CeO2颗粒。当模板剂用量为n(CTAB)∶n(Ce(NO3)3.6H2O)=1∶2,制备出粒径约为6.1nm的球形纳米CeO2;共沸蒸馏能有效去除前驱体中的模板剂和吸附水,丁氧基的取代吸附及其空间位阻作用有利于制得分散性好、粒度分布均匀、粒径约为1.5～2.2nm的纳米CeO2颗粒;水热处理改善了纳米CeO2颗粒的晶化度,避免了高温焙烧过程时硬团聚体的生成,颗粒尺寸为2.5～3.8nm;纳米CeO2颗粒具有良好的可见光透过和优异的紫外光吸收性能。     

多形貌纳米银粒子的制备工艺研究

随着电子元器件向微型化、精密化和柔性化等方向发展,金属导电填料纳米化成为电子封装用导电银浆发展的必然趋势。其中,多形貌纳米银粒子的制备成为该领域的研究热点。采用液相还原法,通过多种表面活性剂的添加调控纳米银晶粒的生长过程,制备出球状、片状、立方状等多种形貌的银纳米粒子,并揭示了它们的生长机理。结果表明,随着聚乙烯吡咯烷酮(PVP)浓度的增加,纳米银颗粒的分散性得到逐步优化,当PVP浓度为2mmol/L时,制备出平均粒径为20nm左右且分散性良好的球状银纳米粒子;柠檬酸钠和双氧水的添加能够诱导纳米银颗粒向片状结构转变,当柠檬酸钠浓度为20mmol/L,双氧水浓度为25mmol/L左右时,有大量片状银纳米粒子的形成;氯化钠(NaCl)能够诱导纳米银颗粒向立方体结构转变,当NaCl浓度为20mmol/L时能够得到形状规则的立方银纳米粒子。     

镁盐及晶种对氧化镁水化合成氢氧化镁的影响

采用氧化镁水化法制备氢氧化镁,研究硫酸镁、乙酸镁、氯化镁、硝酸镁4种镁盐的添加量对氧化镁水化率的影响,以及镁盐和晶种对氢氧化镁颗粒大小和形貌的影响,利用X射线衍射和扫描电子显微镜对合成的氢氧化镁晶体特性、颗粒大小和形貌进行表征,并对上述因素的影响机理进行探讨。结果表明,随着镁离子浓度的增大,氧化镁的水化率逐渐增大,氧化镁水化率最高可达到98.68%,水化产物氢氧化镁颗粒近似于六方片状,粒径约为200⁵00 nm。     

分散剂对低温固相法制备纳米氧化镁的影响

以氯化镁和草酸为原料,分别以淀粉和聚乙二醇1000为分散剂,采用低温固相法制备出不同形貌的纳米氧化镁.采用IR、TG-DTA、XRD和TEM分别对产物形貌和粒径大小进行了表征.结果表明,分散剂的种类和用量是影响纳米氧化镁颗粒大小和均匀度的重要因素.     

微观调控对二氧化钛光催化性能的影响

采用水热法,以钛酸四丁酯为原料制备形貌可控的TiO2纳米颗粒。利用HCl调控水热反应溶液的H+浓度,实现了对TiO2晶型的调控;通过改变钛酸丁酯与硫酸的反应时间,实现了对TiO2晶面的调控。采用多种表征手段对TiO2的晶型和晶面进行表征。通过在LED灯下降解10mg/L的罗丹明B溶液测定TiO2的光催化性能。研究结果表明:在晶型调控的实验中随着HCI浓度的增大,锐钛矿相和板钛矿相的比例逐渐减小,金红石相逐渐增大。当HCl浓度为0.5mol/L时锐钛矿比例约为75%,此时TiO2的光催化性能最好。控制晶面的实验中,钛酸丁酯与硫酸的反应促进了{001}高能面的暴露,在反应时间为15h时TiO2的光催化性能最好。     

不同模板剂对氢氧化镧的微观结构及光催化性能的影响

以La(NO3)3·6H2O和KOH为原料,以EDTA、PVP和HMTA等为模板剂,采用微波水热法制备得到纯相La(OH)3,使用X射线衍射分析(XRD)、扫描电子显微镜(SEM)对产物的物相和形貌进行了分析,结果表明,不添加模板剂和添加EDTA、PVP、HMTA为模板剂时,可分别制备得到具有纳米棒状、类球形纳米颗粒、片状、纳米棒组装的片状形貌的纯相La(OH)3。光催化测试结果表明,模板剂可有效调控产物的微观形貌,并进一步提升La(OH)3的光催化性能。其中添加EDTA得到的类球形La(OH)3在21min内对亚甲基蓝的降解率可达99%。     

H_2O_2处理碳包覆铁纳米颗粒的表面特性及分散行为

采用体积分数30%的H2O2处理碳包覆铁纳米粒子外层的非晶态类石墨碳层,并将其超声分散于水介质中,通过改变pH值分析测定碳包覆铁纳米粒子表面zeta电位和粒径。结果表明:碳包覆铁纳米粒子非晶碳层的特殊结构可通过双氧水化学处理使其表面产生羧基和羟基;在强碱性介质下,羟基和羧基可强化颗粒间的静电斥力,提高碳包覆铁纳米粒子在水介质中的分散性能。当pH值约为11.5时,碳包覆铁纳米粒子表面zeta电位为48 mV,水合粒子粒径可达到110 nm。     

水合肼还原氧化石墨烯的研究

通过改进的Hummers法制备氧化石墨,将获得的氧化石墨进行热剥离以及超声剥离得到双层甚至单层的氧化石墨烯片.然后采用化学还原-水合肼还原的方法去除氧化石墨烯所含的羧基COOH、羟基OH、羰基C=O和环氧基等化学基团.本实验着重研究了还原剂的用量和反应时间对各个化学基团的影响规律.     

硬脂酸改性纳米ZnO的研究

采用酯化反应法,以水为溶剂,采用硬脂酸对纳米ZnO的表面进行改性,对改性效果进行测试表征。其最佳工艺条件为:硬脂酸质量分数为6%,反应温度为90℃,反应时间为90 min。结果表明,改性后的ZnO粒子呈纳米级的分散,亲油化度值达到72.31%,吸水率达到3.04%;经表面改性的纳米ZnO表现了很好的亲油疏水性;改性后的纳米ZnO表面引入了硬脂酸的官能团,使其表面羟基的数目明显减少,其改性机理为纳米ZnO表面羟基与硬脂酸分子中的羧基发生了类似醇和酸的酯化反应。     

纳米氢氧化镁粉体的制备及热分解动力学研究

以氯化镁和尿素为原料,采用均匀沉淀法制备出厚度约为20 nm的片状纳米氢氧化镁粉体。利用热重分析法对片状纳米氢氧化镁粉体在不同升温速率下的热分解动力学进行研究,以期深入认识由纳米氢氧化镁粉体热分解得到纳米氧化镁粉体过程的物理化学本质。分别采用Coats-Redfern方程和Dolye方程,对热重分析数据进行了处理和拟合,得到了片状纳米氢氧化镁粉体热分解反应属于Avrami-Erofeev(n=1)的成核和生长为控制步骤的反应机理,其表观活化能E=131 kJ/mol,指前因子A=1.56×1010。     

Green synthesis and characterization of hexagonal shaped MgO nanoparticles using insulin plant (Costus pictus D. Don) leave extract and its antimicrobial as well as anticancer activity

Green synthesis is an ecofriendly novel technology and attractive research area for the production of metal oxide nanoparticles in bio-medical and chemical applications. The green perspective includes solvents, reductants or stabilizing agents obtained from a natural resource as they are non-toxic and ecofriendly. In this study, a sustainable green synthetic strategy to synthesize magnesium oxide nanoparticles by employing Costus pictus D. Don plant leaf extract as a reducing agent. The successful formation of magnesium oxide nanoparticles was confirmed by comprehensive characterization techniques. The presence of biomolecules and metal oxides were confirmed by Fourier transform Infrared (FT-IR) spectral data analysis. The X-ray diffraction (XRD) revealed the formation of pure cubic MgO crystalline nanoparticles. The surface morphology of MgO particles observed by Scanning electron microscope (SEM) showed the hexagonal-shaped MgO crystallites. The average size of biosynthesized MgO nanoparticles was measured to be around 50?nm by Transmission Electron Microscopy (TEM). The mechanism for the formation of MgO nanoparticles was suggested in this study. The biosynthesized magnesium oxide particles showed good antimicrobial and exhibited maximum inhibition rate for MgO nanoparticles at 200?µg showing efficient anticancer activity.     

纳米氧化镁合成过程中颗粒粒度及形状控制研究

采用化学沉淀-热分解法,合成粒度在20～120 nm的氧化镁粉体。采用透射电镜及X射线衍射分析,研究纳米氧化镁的粒度和形状的控制因素对纳米氧化镁颗粒形成过程的影响。结果表明:镁源及分散剂的种类、沉淀反应温度、样品干燥方式都是影响氧化镁粒度和形状的重要因素。在以Mg(NO3)2为镁源、n(Mg2+):n(OH-)=2:1、沉淀温度为30℃、体积分数为8%的乙二醇为分散剂、微波低火干燥2 min条件下,得到平均粒径为40 nm的氧化镁产品。前驱物的形状与产物纳米氧化镁的形状存在对应关系。     

磁性复合凝胶球对Pb(Ⅱ)的吸附特性与机制

以海藻酸钠(SA)作为基体前驱材料,通过离子交联法包埋固化L-甲硫氨酸(L-met)和纳米Fe₃O₄形成磁性复合凝胶球SA@Fe₃O₄/L-met。实验探究了SA@Fe₃O₄/L-met在不同pH、投加量和初始离子浓度条件下对Pb(Ⅱ)吸附能力的影响。结果表明,在pH=5、投加量为0.5 g·L?1、初始浓度为20 mg·L?1时,SA@Fe₃O₄/L-met对Pb(Ⅱ)能达到较好的吸附效率,最大吸附量可达到328.02 mg·g?1,远大于Fe₃O₄@SA与SA的吸附量142.5 mg·g?1和152.8 mg·g?1。吸附动力学和热力学研究表明该吸附过程分别对准二级动力学方程和Langmuir方程的拟合程度更大,且反应过程是一个熵增吸热的过程。最后采用SEM、XPS、VSM等对SA@Fe₃O₄/L-met的结构与性能进行表征分析,发现SA@Fe₃O₄/L-met中的氨基和羧基通过配位反应与Pb(Ⅱ)结合,同时还存在着离子交换作用。经过5次解吸后SA@Fe₃O₄/L-met的吸附量仍能达到210.5 mg·g?1,是一种较理想的环保吸附剂。      

Influence of titanium doping on the structure and morphology of MgO prepared by coprecipitation method

Ti-doped magnesium oxide powders were prepared by a chemical coprecipitation technique using magnesium nitrate hexahydrate and titanium tetrabutoxide as starting materials and ammonia hydroxide as precipitator. The influence of titanium doping on the structure and morphology of MgO powders was investigated by X-ray diffraction, X-ray fluorescence, X-ray photoelectron spectroscopy and transmission electron microscopy. The results show that titanium ion (Ti⁴⁺) was successfully incorporated into the MgO crystal lattice, and consequently, caused the changing of MgO crystal lattice parameter. However, titanium doping resulted in varied particle sizes, and enhanced slightly the particle aggregation. It is attributed to the difference between the solubility product (K_sp) of the two precursors, Mg(OH)₂ and TiO(OH)₂, which is one of important factors in the chemical coprecipitation process.     

Application of a by-product of Lentinus edodes to the bioremediation of chromate contaminated water

The agricultural by-product of Lentinus edodes was used as a novel biosorbent for bioremediation of chromate contaminated waste water in the simulated experimental conditions. The contact time, particle size, biosorbent dosage and optimum pH range were investigated to optimize the sorption condition. The biosorption by the biomass was strongly affected by pH. At pH 1.0-2.5, all hexavalent chromium was diminished, either removed by the biosorbent or reduced to less toxic trivalent chromium even in very high concentration of 1000 mg/L. The adsorbed hexavalent chromium and reduced trivalent chromium were both linearly dependent on the initial chromium concentration. Most uptake of Cr occurred at pH around 4. The maximum uptake of chromium was 21.5 mg/g when simulated with Langmuir model, which showed the potential biosorption capacity of this biomaterial. The change of oxidation-reduction potential (ORP) during biosorption process revealed strong reduction ability of this biosorbent. Comparing analysis from Fourier transform infrared spectrums indicated that nitrogen oxide and carboxyl groups were increased after biosorption. The energy-dispersive X-ray microanalyzer revealed the mechanism of cation exchange during biosorption.     

Synthesis of biosurfactant‐coated magnesium oxide nanoparticles for methylene blue removal and selective Pb2+ sensing

Dyes and lead (Pb²⁺) are toxic compounds that can contaminant water. In this study, magnesium oxide (MgO) nanoparticles (NPs) prepared using clove, i.e. Syzygium aromaticum extract [clove extract (CE)] were used for methylene blue (MB) removal and Pb²⁺ ion sensing in aqueous solution. Maximum 90% MB removal was achieved using MgO NPs. The MB adsorption on MgO NPs surface followed second‐order kinetics and Langmuir isotherm. MB dye was adsorbed as a monolayer on the surface of MgO NPs with maximum adsorption capacity, 5555 mg g⁻¹. MgO NPs were also able to selectively detect lead (Pb²⁺) in 1 nM–200 µM range with 24 µM (3σ) limit of detection. So, CE prepared MgO NPs are useful for MB dye adsorption and metal ion sensing applications.Inspec keywords: magnesium compounds, nanoparticles, dyes, lead, chemical sensors, adsorptionOther keywords: biosurfactant‐coated magnesium oxide nanoparticles, methylene blue removal, selective lead sensing, dyes, toxic compounds, Syzygium aromaticum extract, clove extract, MB adsorption, second‐order kinetics, Langmuir isotherm, maximum adsorption capacity, MgO, Pb²⁺