水热法制备Sb_2Se_3纳米晶

以酒石酸锑钾(K(SbO)C4H4O6.1/2H2O)和硒粉作为锑源和硒源,自制的2-十一烷基-1-二硫脲乙基咪唑啉季铵盐(SUDEI)为表面活性剂,150℃水热反应24 h,得到不同形貌的Sb2Se3纳米晶。通过透射电镜(TEM)、X射线衍射(XRD)、X射线光电子能谱仪(XPS)对Sb2Se3纳米晶进行了表征。讨论了反应条件对Sb2Se3纳米晶形貌的影响。     

水热法制备均分散的硫化锌纳米晶聚集体

利用自制的月桂酸硫脲咪唑啉季铵盐(SUDEI)作为表面活性剂,在水热条件下制备出了均分散的面心立方β闪锌矿结构的ZnS纳米晶聚集体,聚集体粒径为20～50nm。通过透射电子显微镜、粒度分布仪、XRD和紫外可见吸收光谱等手段对硫化锌粒子进行了表征。得到制备均分散ZnS纳米晶聚集体的最佳条件为,月桂酸硫脲咪唑啉季铵盐2g·L-1,cZn2+=0.016mol·L-1,150℃放置12h,填充度为60%。     

溶剂热条件下钴微纳米颗粒的构筑习性

以乙酸钴为钴源,水合肼为还原剂,在不同表面活性剂下,溶剂热法制备出不同形貌的二维、三维钴微纳米颗粒。通过扫描电子显微镜(SEM)、X射线能量色散谱(EDS)和X射线衍射(XRD)对产物进行了表征。采用自制的2-十一烷基-1-二硫脲乙基咪唑啉季铵盐(SUDEI)为表面活性剂时,制备出直径400~600nm,厚度约100nm的六角盘状二维产物,采用其他表面活性剂只能制备出三维的花状钴。初步探讨了溶剂热条件下钴微纳米颗粒的构筑习性。     

SUDEI-CuS混凝构筑球的制备及表征

以适量的月桂酸硫脲咪唑啉季铵盐(SUDEI)为表面活性剂,采用溶剂热法在NN二甲基甲酰胺(DMF)/乙二醇中140℃反应24h,制备出了花状的SUDEI-CuS混凝球。通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、X射线衍射分析仪(XRD)与UV-Vis等进行了表征,对SUDEI-CuS混凝球形成机理、结构的材料性能进行探索。同时发现SUDEI-CuS混凝球,具有较强的紫外可见吸收。     

微溶剂法合成咪唑啉缓蚀剂及性能评价

以油酸和羟乙基乙二胺为原料,甲苯作溶剂,采用微溶剂法经过酰胺化和成环反应合成咪唑啉缓蚀剂(1),又通过与氯化苄进行季铵化反应得到咪唑啉季铵盐缓蚀剂(2),改善了水溶性.使用挂片失重法和电化学Tafel极化曲线法对缓蚀剂产品进行评价.并研究了缓蚀剂与KI复配后的缓蚀效果.结果表明,缓蚀效果随缓蚀剂浓度增加而增强,咪唑啉季铵盐的缓蚀性优于未季铵化的咪唑啉,缓蚀剂与KI复配后的缓蚀效果明显增强.极化曲线法标明咪唑啉季饺盐质量浓度为250mg/L,参与复配KI质量浓度为150mg/L时,其在20℃的1mol/L H2SO4腐蚀环境中的缓蚀率可达到98.2％.     

咪唑啉季铵盐的复配及缓蚀性能评价

用自制的油酸咪唑啉、月桂酸咪唑啉、苯甲酸咪唑啉季铵盐分别与丙炔醇(PRAL)、十二烷基苯磺酸钠(SDBS)及二乙烯三胺五甲叉膦酸(DETPMP)进行复配,利用静态挂片失重法得出最佳复配条件∶油酸咪唑啉季铵盐质量浓度60 mg/L,按照质量比1∶0.6加入DETPMP,最高缓蚀率可达到93.7%。并用极化曲线法考察了复配缓蚀剂在饱和CO_2油田水中的协同缓蚀作用。     

油酸咪唑啉季铵盐缓蚀剂的复配及在饱和CO2油田水中的缓蚀作用

以自制的有机膦酸为复配剂对油酸咪唑啉季铵盐缓蚀剂进行了复配研究,利用静态挂片失重法考察了复配对咪唑啉缓蚀剂在饱和CO_2油田水中缓蚀性能的影响。研究表明,当油酸咪唑啉季铵盐与多胺缩聚物有机膦酸(PAMMP)质量比达到1∶0.75时缓蚀效果最好,缓蚀率可以达到95.3%,而油酸咪唑啉季铵盐与乙二胺四甲叉膦酸(EDTMP)的质量比为1∶1时缓蚀效果的稳定性最强,经过72 h之后,其缓蚀率仍可达到88.5%。     

咪唑啉季铵盐的改性研究

以油酸、四乙烯五胺和氯化苄为主要原料合成了咪唑啉季铵盐,采用有机酸对其进行改性制得水溶性好的咪唑啉缓蚀剂。考察了反应物物质的量比、反应时间、反应温度对缓蚀率的影响。结果表明,当有机酸与咪唑啉委铵盐的物质的量比为1.1、反应时间为3h、反应温度为150℃时,得到的改性咪唑啉季铵盐溶解分散性良好。利用红外光谱对改性后的咪唑啉季铵盐的结构进行了表征,考察了咪唑啉缓蚀剂在水中的溶解分散性。结果表明,在质量分数为15%的盐酸介质中,90℃时咪唑啉缓蚀剂对碳钢的缓蚀率可以达到85%以上。     

无机复配体咪唑啉缓蚀剂的合成与应用

采用油酸和二乙烯三胺为原料合成出了咪唑啉季铵盐缓蚀荆，在50℃、5％的盐酸介质中用静态失重法对咪唑啉季铵盐与阴离子表面活性剂和无机阴离子的协同作用进行了研究，得到了一个与咪唑啉季铵盐有最佳复配效果的复配体，咪唑啉季铵盐与I^-复配比为1：1（质量比）时，缓蚀剂的缓蚀效果最佳，在不同时间和不同温度下对复合型缓蚀剂的缓蚀效率进行了研究。结果表明，新型缓蚀剂对A3钢的缓蚀率达到99％以上，较单独用咪唑啉季铵盐缓蚀效率提高了0．7％左右。     

咪唑啉季铵盐的合成及性能评价

以油酸、二乙烯三胺为原料合成了咪唑啉中间体,对其改性得到了水溶性咪唑啉基季铵盐,利用红外光谱对其结构进行了表征,通过静态挂片、极化曲线法等测试方法评价了在1 mol/L的HCl中对Q235碳钢的缓蚀性能,并探讨了咪唑啉季铵盐的清蜡性能.实验结果表明：该缓蚀剂溶解分散性及表面活性好,能有效阻止盐水介质中的腐蚀,对Q235碳钢在1 mol/L的HCl体系中的腐蚀具有明显的抑制作用;通过将咪唑啉季铵盐与异丙醇复配,咪唑啉季铵盐不但具有缓蚀、防腐性能,还具有清蜡性能.     

Eu2Zr2O7纳米晶的硬脂酸法制备

以硝酸锆和硝酸铕作为原材料,硬脂酸作为溶剂和分散剂,通过硬脂酸燃烧法制备了具有立方晶系的萤石型Eu2Zr2O7纳米晶.通过热重和红外光谱对其反应过程进行跟踪.产物经X-射线粉末衍射、透射电镜、高分辨电子显微镜、能谱以及荧光光谱进行了表征.热处理温度对产物的形成有较大的影响,在800℃单一相的Eu2Zr2O7纳米晶已完全形成.所制得的纳米晶由平均粒径为5~20 nm的球状粒子组成.从透射电镜上（222）面的晶面距分别为0.307 nm,与理论值一致.实验检测到Eu2Zr2O7具有较强的荧光性质.     

Surfactant-assisted synthesis and magnetic properties of monodispersed manganese ferrite nanocrystals

Monodispersed manganese ferrite (MnFe₂O₄) nanocrystals could be successfully synthesized in large quantities via a facile synthetic technique based on the pyrolysis of organometallic compound precursor, in which octadecene was used as solvent, and oleic acid and oleylamine were used as capping ligands. MnFe₂O₄ nanocrystals were obtained with size in a tunable range of 4–15 nm and their morphologies could be tuned from spherical to triangle-shaped by varying the surfactants. The phase structure, morphology, and size of the products were characterized in detail by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Magnetic properties of MnFe₂O₄ nanocrystals with different morphologies were measured using a superconducting quantum interference device (SQUID). Both monodisperse MnFe₂O₄ nanocrystals with spherical and triangle-shapes are superparamagnetic at room temperature while ferromagnetic at 2 K. The pyrolysis method may provide an effective route to synthesize other spinel ferrites or metal oxides nanocrystals.     

Enhanced photocatalytic activity of （La, N） co-doped TiO2 by TiCl4 sol-gel autoigniting synthesis

(La, N) co-doped TiO2 photocatalysts were synthesized using TiCl4 sol-gel autoigniting synthesis (SAS) starting from a plished in the formation of TiO2 nanocrystals. The prepared samples were characterized by using X-ray diffraction (XRD), X-ray photoemission spectroscopy (XPS) and UV-vis diffuse reflectance spectra. The results indicated that nitrogen and lanthanum were incorporated into the lattice and interstices of titania nanocrystals, which resulted in narrowing the band gap and promoting the separation of photoexcited hole-electron pairs, respectively, and showing expected red-shifts and enhanced photocatalytic activity under visible light. The mechanism on nitrogen doping and enhancement in photocatalytic activity of (La, N) co-doped titania by SAS was discussed in detail.     

Growth Mechanism and Characterization of ZnO 3D Nanocrystals by Laser Irradiation & Coaxially Transporting O2

Different three-dimension (3D) nanotetrapods,containing club-like nanocrystals,nanotetrapods and four-foot-like nanocrystals were synthesized from Zinc sheet via CO2 laser irradiation and coaxially transporting O2.Different nanoproducts were fabricated by changing the content of oxygen in the experiment.The morphologies,components,phase structures and optical properties of the products were investigated by a field-emission scanning electron microscopy,an X-ray diffraction,an energy dispersed X-ray spectrometer and a photoluminescence spectroscope.The X-ray diffraction spectra were obtained on a Rigaku D/max 2500PC diffractometer.The experimental results reveal that high quality ZnO nanotetrapods can be fabricated on the special parameters,and growth of ZnO nanotetrapods depends on Vapour-Liquid-Solid(VLS) model,and the content of oxygen in the gas,namely,oxygen partial pressure is one of main factors to control morphologies and optical properties of ZnO nanotetrapods;these advantages above are important for realization of optoelectronic devices.     

Enhanced photocatalytic activity of (La, N) co-doped TiO_2 by TiCl_4 sol-gel autoigniting synthesis

(La, N) co-doped TiO2 photocatalysts were synthesized using TiCl4 sol-gel autoigniting synthesis (SAS) starting from a complex compound system of TiCl4-La(NO3)3-citric acid-NH4NO3-NH3?H2O, in which the (La, N) co-doped process was accom- plished in the formation of TiO2 nanocrystals. The prepared samples were characterized by using X-ray diffraction (XRD), X-ray photoemission spectroscopy (XPS) and UV-vis diffuse reflectance spectra. The results indicated that nitrogen and lanthanum were incorporated into the lattice and interstices of titania nanocrystals, which resulted in narrowing the band gap and promoting the sepa- ration of photoexcited hole-electron pairs, respectively, and showing expected red-shifts and enhanced photocatalytic activity under visible light. The mechanism on nitrogen doping and enhancement in photocatalytic activity of (La, N) co-doped titania by SAS was discussed in detail.     

Growth Mechanism and Characterization of ZnO 3D Nanocrystals by Laser Irradiation ＆ Coaxially Transporting O2

Different three-dimension （3D） nanotetrapods, containing club-like nanocrystals, nanotetrapods and four-foot-like nanocrystals were synthesized from Zinc sheet via CO2 laser irradiation and coaxially transporting O2. Different nanoproducts were fabricated by changing the content of oxygen in the experiment. The morphologies, components, phase structures and optical properties of the products were investigated by a field-emission scanning electron microscopy, an X-ray diffraction, an energy dispersed X-ray spectrometer and a photoluminescence spectroscope. The X-ray diffraction spectra were obtained on a Rigaku D/max 2500PC diffractometer. The experimental results reveal that high quality ZnO nanotetrapods can be fabricated on the special parameters, and growth of ZnO nanotetrapods depends on Vapour-Liquid-Solid（VLS） model, and the content of oxygen in the gas, namely, oxygen partial pressure is one of main factors to control morphologies and optical properties ofZnO nanotetrapods; these advantages above are important for realization of optoelectronic devices.     

Grain growth kinetics of SnO<Subscript>2</Subscript> nanocrystals synthesized by precipitation method

Monodispersed spheroidal SnO₂ nanocrystals with the grain size of 8–30 nm were synthesized by the precipitation method using SnCl₄·5H₂O (stannic chloride hydrate) as raw materials. Differential scanning calorimetry/thermogravimetry (DSC/TG), X-ray diffraction (XRD) and transmission electron microscope (TEM) were used to characterize the structure of SnO₂ nanocrystals. The influences of the calcination temperature and time on the lattice constant, the lattice distortion and the grain size of SnO₂ nanocrystals were discussed based on the XRD results. The grain growth kinetics of SnO₂ nanocrystals during calcination process was simulated with a conventional grain growth model which only took into account of diffusion and with a new isothermal model proposed by our group, which took into account of both diffusion and surface reactions. Using conventional model, the grain growth rate constant of SnO₂ crystals is 1.55×10⁴ nm⁵/min with a pre-exponential factor of 5 and an activation energy of 108.62 kJ/mol. Compared with the convention model, the new isothermal model is more realistic in reflecting the grain growth behavior of SnO₂ nanocrystals during the calcination process. This indicates that the grain growth of SnO₂ nanocrystals is controlled by both diffusion and reaction factors, and the effect of surface reactivity on the grain growth of SnO₂ nanocrystals could not be ignored. A combined activation energy estimated with the new isothermal model is 53.46 kJ/mol.     

Facile Synthesis of 2PbCO3·Pb(OH)2 Microcrystals and Its Catalytic Behavior for Transesterification of Dimethyl Carbonate with Phenol

Polyhedron lead hydroxide carbonate （2PbCO3·Pb（OH）2 ） microcrystals have been prepared in solution phase via a facile method in the presence of surfactant cetyltrimethylammonium bromide （CTAB）. All the samples were characterized by powder X-ray diffraction ,pattern （XRD）, field-emission scanning electron mi- croscopy （FE-SEM）, high-resolution transmission electron microscopy （HRTEM）, and selected area electron diffraction （SAED）. The possible growth mechanism was discussed. 2PbCO3·Pb（OH）2 microcrystals were found to be a novel and efficient catalyst for the synthesis of diphenyl carbonate （DPC） by transesterification of dimethyl carbonate （DMC） with phenol. Compared with some other catalysts, such as AlCl3, ZnCl2, and Mg5（CO3）4（OH）2, 2PbCO3·Pb（OH）2 microcrystals are stable and show relatively high activity at low catalyst amount. When the reaction was carried out at 180 12, with a molar ratio of phenol to DMC of 2：1, a reaction time 14 h, and a catalyst amount 0.2% （molar ratio to phenol）, the selectivity of DPC and methyl phenyl carbonate （MPC） was 14.7% and 78.8%, respectively.