复合超分子紫外屏蔽材料的制备和性能及在涂料中的应用

以Mg/Zn/Al-CO3–LDHs(层间复合金属氢氧化物)为前驱体,通过成核/晶化隔离法将2-(2-羟基-4-氨基苯基)-5-磺酸基氢化苯并三唑(HASB)插入到前驱体层间,得到了一种新型的无机–有机复合超分子紫外屏蔽材料──苯并三唑类插层水滑石Mg/Zn/Al–HASB–LDHs。研究了Mg、Zn、Al不同摩尔比对前躯体紫外吸收性能的影响,确定了较佳的配比:n(Mg)/n(Zn)/n(Al)=1∶2∶1。采用X射线粉末衍射(XRD)、扫描电镜(SEM)、红外光谱(IR)、热分析(TG–DTA)等手段对Mg/Zn/Al–HASB–LDHs进行了表征,并将其作为紫外屏蔽材料加入到丙烯酸涂料中,通过紫外–可见光谱研究了Mg/Zn/Al–HASB–LDHs的用量对涂料紫外吸收性能的影响。结果表明,HASB成功取代了前驱体层间的23CO-离子,并能与主体形成较强的超分子间相互作用,使插层水滑石的热稳定性明显提高。随着Mg/Zn/Al–HASB–LDHs摩尔分数的增加,丙烯酸涂料的紫外屏蔽作用增强,紫外吸收范围变宽。     

Zn-Al类水滑石的合成及表征

用液相非稳态共沉淀法合成了Zn Al类水滑石(HTlc),研究了样品中n(Al)/n(Zn+Al)(x)和层间阴离子CO2-3对Zn Al HTlc化学组成、晶体结构和粒子形貌的影响。结果表明,当0 31≤x≤0 52时可得到单一的Zn Al Cl HTlc相;x≤0 25时有ZnO杂质相出现;x>0 52时样品主要以无定形物存在。x对晶胞参数a和c影响不大;与Cl-相比,层间CO2-3对a影响不大,使c值略有降低。透射电镜(TEM)结果表明,随每摩尔HTlc样品n(Zn)增加,Zn Al ClHTlc粒子六角形片状结构规则度增加。电子衍射图谱表明,所合成的HTlc样品均为六方晶系多晶结构物质。     

络合溶胶-凝胶法制备Al_2O_3纳米晶及其表征(英文)

以异丙醇铝为原料,用聚乙二醇(PEG1000)络合溶胶-凝胶法合成了Al2O3纳米晶,并采用差热-热重分析、X射线衍射、透射电子显微镜等对络合前驱体及粉体进行表征;探讨了PEG1000及煅烧温度对纳米Al2O3相结构、粒子尺寸、形貌及分散性的影响规律.结果表明:PEG1000增强了纳米Al2O3粒子的分散性.干凝胶在600～900℃煅烧后得到γ-Al2O3相;在600℃煅烧条件下,得到γ-Al2O3粒子形貌为针状结构,长度约为50～60nm.随着煅烧温度的升高,γ-Al2O3针状粒子长度逐渐减小,在750℃煅烧后,得到γ-Al2O3粒子长度为20～30nm;在900℃煅烧条件下,γ-Al2O3粒子形貌为颗粒状,平均粒径尺寸为10nm;当干凝胶在1 000℃煅烧后得到θ-Al2O3和α-Al2O3的混合相,所得粒子平均粒径尺寸为20 nm;当干凝胶在1 200℃煅烧后,得到的Al2O3全部转化α-Al2O3相,制得的纳米Al2O3粒子尺寸均一且分散性良好.     

含钛水滑石的制备表征及其光催化活性的验证

通过动态尿素法制备了不同二价金属的系列类水滑石M(Ni、Zn、Co)-Ti LDHs。通过XRD、SEM对产物进行表征,显示M(Ni、Zn、Co)-Ti LDHs均生成且具有较好的结晶度和晶型。通过紫外-可见漫反射光谱研究了样品的光吸收特性,显示3类水滑石在紫外可见区均具有吸收。在500 W氙灯(模拟太阳光)照射降解亚甲基蓝(5 mg/L)实验中验证催化剂的可见光催化活性,结果表明,3类水滑石相比市售TiO2均表现出较强的催化活性,3类水滑石具有一定的可见光催化活性,其中Zn-TiLDHs活性最高。在催化剂用量为20 mg,照射时间为4 h时,亚甲基蓝降解率达99.8%。     

高含量高透明度PS/TiO2纳米复合材料膜的紫外防护性能研究

采用溶剂热法非水合成了粒径小于20 nm的二氧化钛（TiO2）纳米粒子,并用硅烷偶联剂（KH 570）对纳米粒子进行原位修饰以提高粒子在聚苯乙烯（PS）的对二甲苯溶液中的分散性。采用旋涂法制备不同纳米TiO2粒子含量的PS复合材料膜,用紫外可见光光谱仪检测了薄膜的紫外防护性能。结果表明,纳米TiO2的最高含量达到95 %（质量分数,下同）;随着纳米TiO2粒子含量的增加,薄膜的紫外屏蔽性能逐渐增强,同时可见光区的透明度不会线性减少,而是趋于饱和,当纳米TiO2粒子含量达到95 %时,在人眼最敏感的550 nm波长处,依然可以获得82 %的透明度。     

蓝宝石衬底上透明Mg_xZn_(1-x)O薄膜的制备及表征

采用射频磁控溅射法在Al_2O_3(001)衬底上制备了高Mg含量的Mg_xZn_(1-x)O薄膜,研究了Mg_xZn_(1-x)O薄膜的结构和光学性能。结果表明:Al_2O_3(001)衬底上Mg_xZn_(1-x)O薄膜的组分为Mg_(0.47)Zn_(0.53)O,薄膜呈六方纤锌矿结构,薄膜沿c轴方向取向生长,且c轴方向晶格增大0.0029 nm。薄膜的吸收边峰值位于292nm,对应的禁带宽度为4.24ev。薄膜平均粒径约为10～20nm,在深紫外-可见光激发下的荧光发射峰分别位于320nm和400nm附近。     

以钢渣为原料合成层状双氢氧化物及其结构表征

以钢渣为原料,醋酸为浸出介质,在一定条件下得到浸出液,利用共沉淀法合成了Ca-Mg-Al-Fe四元层状双金属氢氧化物(LDHs),探讨了pH、晶化温度和晶化时间对Ca-Mg-Al-Fe四元LDHs层状材料合成的影响,采用XRD、XRF、SEM、FT-IR、TEM、DTA/TG和BET对样品进行了表征。研究表明,pH对层状材料合成的影响最大,pH在10.5～11.8可形成纯相水滑石;晶化温度和晶化时间是影响晶格参数和层间距的重要因素,随温度及时间的增加,其晶格参数a、c及层间距均先减小后增大;LDHs的晶粒尺寸沿a轴方向比沿c轴方向大。当pH 11.8,晶化温度150℃,晶化时间16 h时,合成的LDHs层状材料结构规整、晶型良好、层状结构明显、孔径较大且热稳定性良好。     

Mg-Al水滑石的水热合成及晶面选择性生长

以MgO、Al(OH)3为镁源和铝源,采用一步水热法合成了镁铝水滑石(Mg-Al LDHs),考察了水热时间及水热温度对水滑石晶粒度和晶面选择性生长的影响规律.用XRD、SEM等对合成产物进行了表征.结果发现水热时间不变,升高水热温度,或水热温度不变,延长水热时间,LDHs的晶体结构均趋于完整,径厚比呈增大趋势;并且晶体沿a轴方向的生长速率比沿c轴方向的生长速率大,即[110]晶面的生长速率比[003]晶面的生长速率快.     

TiO2纳米复合抗菌剂粉体的制备及耐热性

以TiCl4,Al2(SO4)3为原料,采用液相共沉淀法制备了TiO2纳米复合抗菌剂,并对其耐热性能及抗菌性能进行了研究,同时对其复合结构进行了初步分析.结果表明:复合Al2O3后的TiO2纳米抗菌剂在900℃煅烧后完全为锐钛矿;950℃煅烧后为锐钛矿(相对质量含量为77%)占主要含量的混晶结构,平均粒径为20～30 nm.在950℃时,其紫外-可见光吸收特性较纯纳米TiO2在700℃有较大提高,且抗菌效果优于纯TiO2纳米抗菌剂的.Al2O3在TiO2表面形成的均匀包覆和键合约束机制是抑制纳米TiO2晶型转化和晶粒生长原因.     

TiO2纳米粒子的制备及表征

利用溶胶-凝胶法制备了TiO2纳米粒子,并利用透射电子显微镜、扫描电子显微镜、紫外-可见吸收光谱仪和傅立叶转换红外光谱仪对TiO2纳米粒子的形貌、结构和尺寸进行了表征。结果表明:TiO2纳米粒子为近球形,粒径为12~15nm左右的锐钛矿型纳米晶;TiO2溶胶薄膜中粒子均匀分散,有较好的均一性;TiO2纳米粒子表面富氧,含有较多的TiOH基团;TiO2纳米粒子尺寸对反应体系的pH值很敏感;不同尺寸的纳米粒子在紫外区均有较强吸收,并表现出吸收带边蓝移效应。     

微波水热法用于制备纳米氧化锌粉体的研究

以氯化锌和氢氧化钠为原料,采用微波水热法制备了纳米氧化锌粉体,并采用X射线衍射（XRD）和透射电镜（TEM）对粉体的粒度、形貌、纯度进行了表征。通过单因素实验考察了反应温度、微波反应时间、微波功率、锌离子与氢氧根的浓度比等因素对氧化锌粉体的产率和粒径的影响,再通过正交试验得到最优制备条件。最佳制备工艺条件：锌离子与氢氧根的浓度比为1∶1.2、反应温度为 120 ℃、反应时间为 10 min、微波功率为500 W。在此条件下所得氧化锌粉体的晶型为六方晶相,产率达到93.5%,平均粒度约70 nm,粒径分布较窄,结晶完整。     

橡胶粒子尺寸对ABS树脂性能的影响

通过乳液聚合制备了橡胶粒子尺寸为64～420 nm的丙烯腈-丁二烯-苯乙烯(ABS)共聚物.然后将其与SAN-T树脂熔融共混制备橡胶质量分数为15%的ABS树脂.研究了橡胶粒子尺寸对ABS树脂力学性能影响和材料内部形态结构.结果表明:随着橡胶粒子尺寸的增加ABS树脂的冲击韧性提高.当橡胶粒子尺寸在320 nm时,拉伸强度达到最大,ABS树脂的综合性能达到最好.粒子尺寸在64～110 nm时,橡胶粒子在基体内部发生团聚,材料发生脆性断裂.当橡胶粒子尺寸在216～420 nm时,材料主要以韧性断裂为主,发生脆韧转变.具有双峰分布ABS-110nm/ABS-275 nm共混物大、小橡胶粒子间发生明显的协同作用.     

Particle Size and Optical Properties of Montmorillonite in Suspension

The light absorption spectra of monoionic montmorillonite suspensions with Li, Na, K, Rb, NH₄, Cs, Mg, Ca and Ba as adsorbed ions were studied in the wavelength range 200–800 mμ. Theoretical analysis of the spectra showed that in the visible range, only scattering is responsible for light intensity attenuation. The scattering was found to depend on the type of adsorbed ion and to increase systematically along the series from Li to Ba. This was attributed to increased particle size of the clay caused by parallel plate condensation to form tactoids. A geometrical model of a montmorillonite tactoid was assumed. The general dependence of the properties of such tactoids, and of their suspensions, on the number of plates per tactoid was formulated. Using the measured values of light absorbance index, and the theoretical model, the relative sizes, measured by the number of plates per tactoid, in the different ionic forms were calculated. The relative sizes thus estimated were found to agree favorably with relative sizes calculated from negative adsorption surface area measurements. A typical peak of specific light absorption was observed at 240–245 mμ, for both the suspensions and their clay-free supernatant solutions. Though the compound responsible for this peak is unidentified yet, its quantity in the various suspensions could be roughly estimated. The quantity was found to be negatively correlated with the relative size of the tactoid. It was concluded that the average particle size of montmorillonite in suspension markedly and systematically depends on the type of adsorbed ion. The implications of this finding are discussed.     

Preparation and characterization of nanocrystalline and mesoporous strontium titanate thin films at room temperature

The low temperature perovskite-type strontium titanate (SrTiO₃) thin films and powders with nanocrystalline and mesoporous structure were prepared by a straightforward particulate sol–gel route. The prepared sol had a narrow particle size distribution with hydrodynamic diameter of about 17 nm. X-ray diffraction (XRD) revealed that the synthesized powders had a perovskite-SrTiO₃ structure with preferable orientation growth along the (1 0 0) direction. TEM images showed that the average crystallite size of the powders annealed in the range 300–800°C was around 8 nm. FE-SEM analysis and AFM images revealed that the deposited thin films had mesoporous and nanocrystalline structure with the average grain size of 25 nm at 600°C. Based on Brunauer–Emmett–Taylor (BET) analysis, the synthesized powders showed mesoporous structure with BET surface area in the range 92–75 m²/g at 400–600°C. One of the smallest crystallite sizes and one of the highest surface areas reported in the literature were obtained, which can be used in many applications, such as photocatalysts.     

Critical Particle Size and Phase Transformation in Zirconia: Transmission Electron Microscopy and X-ray Diffraction Studies

A study was undertaken to examine the crystallite size effect on the low-temperature transformation of tettragonal zirconia. Zirconia weas prepared by precipitation from a solution of zirconium tetrachloride by adding ammonium hydroxide to produce a pH of 2.95. Portions of the sample, after drying, were calcined at 500°C for various time intervals. Phase transformation was followed by X-ray diffraction; the data show that the tetragonal phase was initially formed and it was transformed to the monoclinic phase at longer periods of calcination. It was observed by TEM particle size and XRD crystallite size that the transformation does not appear to be due to a critical particle size effect.     

纳米镁基储氢材料的粒度分布表征

用碱熔、酸洗、碳化处理制得的微晶碳做助磨剂,球磨金属镁3 h,制得储氢材料70Mg30C。用扫描电镜和原子力显微镜观测可见,颗粒的平均粒径约为100 nm,颗粒大小主要分布在50~100 nm之间,而透射电镜观测的颗粒大小主要集中在50 nm左右。扫描电镜图的粒度分布近似为对数正态分布,粒度分布范围为25~260 nm。     

不同粒度纳米TiO2的制备

不同粒度的纳米TiO2具有不同的用途。文章以硫酸钛为原料,尿素作沉淀剂,采用均匀沉淀法,研究了不同平均粒径纳米二氧化钛的制备工艺,讨论了工艺条件对其粒径的影响。研究结果表明：通过改变工艺条件,采用均匀沉淀法可制备出平均粒径范围为8～40nm的锐钛矿型纳米TiO2;在制备过程中,反应物浓度及配比、反应温度、煅烧温度等工艺参数对所制备粉体粒度都有不同程度的影响;纳米二氧化钛的粒度随反应物浓度的增加或反应温度的升高而减小,随煅烧温度的升高而增大。     

Preparation of Nanosized Hematite Particles by Mechanical Activation of Goethite Samples

Nanosized single crystals of hematite with a very narrow particle size distribution were prepared by mechanical activation of two different goethite samples. Both goethite samples transformed completely into hematite after 70 h grinding time. Transmission electron microscopy showed that the final particles were spherical in shape and of ∼17 nm average particle size. This particle size was coincident with that estimated from specific surface measurements, indicating that the hematite samples consisted of nonporous and nonaggregated particles. The crystallite size, calculated from the broadening of the XRD peaks, in the hematite samples indicated that particles consisted of single crystals. No influence of the precursor was observed in the products, so both goethite samples yielded identical rounded single crystals with a narrow particle size distribution.     

用激光粒度分析仪检测细粒径SiO2基相变调湿复合材料的粒度分布

以SiO2为载体、棕榈醇-棕榈酸-月桂酸为相变材料,采用溶胶-凝胶法制备细粒径SiO2基相变调湿复合材料,以中位径(d50)为评价指标,采用激光粒度分析仪研究了溶液溶质浓度、超声时间、超声频率及分散介质对材料粒度的影响. 结果表明,激光粒度分析仪可用于检测SiO2基相变调湿复合材料的粒度分布,水对材料的分散效果比乙醇好,以水为分散介质,材料最佳溶质浓度为5~10 g/L,最佳超声时间为15 min以上,最佳超声功率大于400 W.     

NiTiO3纳米棒的制备及表征

结合溶胶-凝胶法和微乳液化学剪裁技术,以钛酸丁酯和N iC l2制备凝胶,在SDS/正丁醇/正庚烷/水形成的微乳液体系中,对凝胶进行化学剪裁并与KBH4反应,经500℃煅烧30 m in,制备出直径40~100 nm,长度150~700 nm,长径比为4~7的N iTiO3纳米棒。用XRD、ED、EDS、IR、TEM、TGA和DSC等方法对产物的组成、结构及纳米棒的形成过程进行了研究。实验表明,凝胶的陈化时间、煅烧温度和煅烧时间对纳米N iTiO3的组成、粒径和形貌均有影响。研究认为,前驱物不均匀地吸附有机物,导致煅烧过程中,颗粒在不同方向上以不同的速度生长,是N iTiO3纳米棒形成的原因。