Al2O3对低品位菱镁矿与天然硅石合成制备镁橄榄石的影响

以低品位菱镁矿与天然硅石为原料,以Al2O3为添加剂,通过反应烧结制备镁橄榄石。研究讨论Al2O3对镁橄榄石材料相组成、晶胞参数、微观结构及常温性能的影响。用XRD和SEM对烧后试样的相组成和显微结构进行表征。利用X’pert plus软件对试样中镁橄榄石相的晶胞参数进行计算。结果表明:以低品位菱镁矿轻烧氧化镁和天然硅石为原料,经1500℃煅烧合成制备的镁橄榄石中,由于Al2O3的加入,促进了系统中顽火辉石相的形成。Al2O3的加入导致镁橄榄石相的晶胞参数和晶胞体积的增大。随着Al2O3加入量增加,镁橄榄石的相对密度和常温耐压强度逐渐增加,说明了Al2O3对镁橄榄石的促烧结作用。     

基于带隙分析的三维反蛋白石光子晶体的非理想态结构参数的求解

应用平面波展开法分析了三维反蛋白石结构光子晶体的带隙性质;计算了沿[111]方向入射时其赝带隙(第一、第三赝带)中心频率分别与填隙材料在模板中填充率ff、模板煅烧因子sf的关系曲线:随ff的减小,v增大;随sf的增大,v随之增大,非理想状态下,ff＜100;、sf＞1,因此较理想态发生蓝移;由此提出了求解平均填充率ffev与平均煅烧因子sfev的计算框图.     

白云石制备碳酸钙晶须及其机理的研究

以白云石为原料,采用气液接触法制备碳酸钙晶须.研究了煅烧条件对白云石分解的影响;同时对碳酸钙晶须的制备以及机理进行了研究,采用XRD、SEM等分析手段对产品进行表征.结果 表明,白云石在煅烧温度850℃,升温速率10℃/min,煅烧时间4h的情况下,分解效果最佳;反应温度、通气速率和搅拌速率对碳酸钙晶须的生成具有显著作用,通过对结晶过程以及晶体的生长理论来解释碳酸钙晶须的生成.     

块状菱镁矿热分解机理及动力学方程的建立

采用TG法对块度为20 mm、30 mm 、40 mm和50 mm的立方体状菱镁矿的热分解进行了研究.结果表明:在相同转化率条件下,块状菱镁矿的分解活化能随块度增加而增大,块度(L =20 ～50 mm)与活化能的关系为:E=4.795×L+34.070(kJ·mol-).块状菱镁矿在不同的分解阶段,受不同的机理函数控制:分解前期,Anti-Jander方程控制的n=2的3D模型为最概然机理函数,动力学方程为:dα/dT=6.111×1010 ×β-1 exp[(4.098-0.577 × L)×T-1](1+α)2/3[(1+α)1/3-1]-1;分解中期,Avrami-Erofeev方程控制的n=3(Code:AE3)的随机成核和随后长大模型为最概然机理函数,动力学方程为:dα/dT=1.422×109×β-exp[(4.098-0.577×L)×T-1](1-α)[-ln(1-α)]-2;分解后期,Avrami-Erofeev方程控制的n=3/2的随机成核和随后长大模型为最概然机理函数,动力学方程为:dα/dT =2.477×109 ×β-1exp[(4.098-0.577L)×T-1](1-α)[-ln(1-α)]-2.本项研究为制定块状菱镁矿生产MgO工艺提供了理论依据.     

水热合成钛酸盐纳米管的晶型结构及光催化活性

以锐钛矿相为主的氧化钛粉体为原料,在强碱条件下采用水热合成法制备出外径约10nm的钛酸盐纳米管.采用TEM、XRD和EDS对产物进行表征,并对其热稳定性、光催化活性进行测试,研究结果表明:制得的纳米管的结晶程度很低,主要成分为钛酸钠,含少量锐钛矿二氧化钛;煅烧温度对钛酸盐纳米管的晶型结构和光催化活性有显著影响.未煅烧及400℃煅烧的纳米管光催化活性较低, 500℃煅烧后具有较高的光催化活性,但煅烧温度高于600℃后,由于锐钛矿晶体减少,纳米管的光催化活性降低.     

Ni2+/TiO2纳米管的光催化活性

以Ni2+/TiO2粉体和NaOH为原料,采用水热法制备了Ni2 +/TiO2纳米管,通过XRD、UV-Vis、SEM等技术对Ni2+-TiO2纳米管的结构、形貌等进行表征,并以罗丹明B为目标降解物,对样品光催化活性进行评价.结果表明:煅烧前,样品主要以钛酸盐的形式存在,有很好的管状结构,管壁较薄,管径为50 ～ 100 nm,管长约为12μm,长径比较大.UV-Vis谱显示约为在284 nm处有一个较弱的吸收峰;500℃煅烧后,钛酸盐的衍射峰强度明显降低,TiO2衍射峰强度增强,纳米管出现坍塌、断裂,锐钛矿相显著,对光的吸收范围也拓展到可见光区,且煅烧后样品的光催化活性显著提高,60 min降解率可达95;.     

V2O5/g-C3N4复合物的制备及可见光催化性能研究

以偏钒酸铵和尿素混合物为前驱体,混合煅烧制备了V2O5/g-C3N4复合物催化剂.用X射线衍射(XRD)、傅里叶红外光谱(FT-IR)、扫描电镜(SEM)、透射电镜(TEM)、紫外-可见光漫反射吸收光谱(UV-vis)、比表面积测试(BET)、光致发光谱(PL)等对其结构进行了表征.结果表明复合物中存在V2O5和g-C3N4形成异质结构,其禁带宽度减小、吸收带边红移,光催化效率有显著提高.以亚甲基蓝(MB)为目标化合物,评价了样品的光催化活性,当前躯体中尿素与NH4VO3质量比为10∶1,煅烧温度为500℃,煅烧时间为0.5h,催化剂活性最高.在60W日光灯照射40 min,对亚甲基蓝得降解率达到97.52;.     

块状菱镁矿热压烧结方镁石晶粒结晶度的表征

采用热压烧结法对块状菱镁矿进行煅烧,研究了温度为1400 ℃,压力P分别为1 MPa、5 MPa和9 MPa,热压时间为2h条件下煅烧后试样的结晶度.结果表明,压力P=1 MPa时,方镁石晶粒间间隙较大,液相分布不均匀,晶粒各个方向晶界移动速率不均匀,晶粒多为半自形晶,结晶程度较差;压力P=5 MPa时,方镁石晶粒紧密排布,液相分布均匀,晶粒的结晶度最高,晶粒发育最好;压力P=9 MPa时,试样组织结构产生应力和应变,晶粒发生形变、损毁和晶面断裂,试样中方镁石晶粒结晶程度最低,晶粒发育最差.     

以偏钛酸浆料制备氮掺杂纳米二氧化钛及其可见光催化性能研究

以工业偏钛酸为前驱体、尿素为氮源,混合煅烧制备了不同氮含量的TiO2光催化剂(记为TiO2-xN-温度).用傅里叶红外光谱(FT-IR)、X射线光电子能谱(XPS)、X射线衍射(XRD)、透射电子显微镜(TEM)、荧光光谱和紫外-可见光漫反射吸收光谱(UV-Vis/DRS)等对催化剂进行了表征.以亚甲基蓝为目标污染物,评价了样品的可见光光催化活性.结果表明,当催化剂中尿素与TiO2质量比为3∶1,煅烧温度为400℃(即TiO2-3N-400℃)时制得的样品活性最高.500 W的长弧氙灯照射4h,对亚甲基蓝降解率达到93.9;.     

不同煅烧方式对粉煤灰水热合成沸石的影响

针对粉煤灰中含有活性较差的莫来石和石英晶体,在不同条件下对粉煤灰进行活化处理,水热晶化合成出不同种类的沸石样品.试验结果证明加碱煅烧活化效果较好,并对其活化机理、煅烧温度和结块现象等进行了研究.     

轻烧MgO的活性对合成镁铝尖晶石晶体结构及性能的影响

以不同活性的轻烧MgO和α-Al2 O3微粉为原料,通过固相烧结法合成镁铝尖晶石,研究轻烧氧化镁的活性对镁铝尖晶石物相组成、晶胞参数、微观结构及烧结性能的影响并探讨其机理.利用XRD和HighScore Plus分析合成试样的物相组成和晶胞参数,利用SEM表征合成试样的微观结构.结果表明:高活性轻烧MgO具有更高的缺陷能,可以加快烧结反应的进行,降低MgAl2 O4的合成温度;高活性轻烧MgO可以促进MgAl2 O4晶体发育,MgO活性越高,生成的MgAl2 O4晶胞参数和晶胞体积越大,晶粒发育更为完全.     

ZnWO4-ZnO复合光催化剂的制备及光催化性能

以ZnO及WO3为前驱反应物,制备了一系列不同ZnWO4含量的ZnWO4-ZnO复合光催化剂.利用X射线衍射、扫描电子显微镜及X射线能谱仪等手段对催化剂进行表征,并以紫外光为光源,罗丹明B为模拟污染物,评价催化剂的活性.结果表明,热处理温度及ZnWO4与ZnO摩尔比对催化剂光催化降解罗丹明B的活性影响显著.当复合4mol;ZnWO4,并于850 ℃煅烧所制得的ZnWO4-ZnO催化剂活性最高,比纯ZnO高出25;.这是因为ZnWO4的复合可抑制ZnO晶粒长大,提高光生电子与空穴的分离效率,进而改善其光催化活性.     

电熔镁铝尖晶石和轻烧镁粉对合成镁铁铝系复合尖晶石的影响

本文研究电熔镁铝尖晶石和轻烧镁粉对合成镁铁铝复合尖晶石的影响.电熔镁铝尖晶石和轻烧镁粉分别与氢氧化铁、活性氧化铝混合均匀制得φ20 mm×10 mm的试样,在空气气氛烧结条件下,于1550℃×6 h高温烧成.采用XRD、SEM和EDS等手段对烧后试样的物相组成和显微结构进行表征.结果表明:加入电熔镁铝尖晶石的试样中存在刚玉相、赤铁矿、铁铝尖晶石相和镁铁铝复合尖晶石相四种矿物相,镁铁铝复合尖晶石的化学式为Mg796Al15.31Fe0.68O32;加入轻烧镁粉的试样中存在刚玉相、铁铝尖晶石相和镁铁铝复合尖晶石相三种矿物相,镁铁铝复合尖晶石的化学式为Al15.71Mg3.35Fe4.94O32;加入电熔镁铝尖晶石的试样中铁铝尖晶石的晶粒尺寸和镁铁铝复合尖晶石相差无几,加入轻烧镁粉的试样中铁铝尖晶石的晶粒尺寸明显大于镁铁铝复合尖晶石.     

Effects of ion exchange and calcinations on the structure and photocatalytic activity of hydrothermally prepared titanate nanotubes

Titanate nanotubes (TiNTs) were prepared by alkaline hydrothermal processing. The TiNTs are thermodynamically unstable and easily transformed to the titania phase by heat or acid treatment. These phase transformations are affected by the preparation conditions. In this study, we investigated the effects of using the washing process to modify the sodium content of the TiNTs. After an alkaline hydrothermal process was used to prepare the TiNTs, the resulting suspensions were washed with weak acid solution and distilled water until the pH value of the wash solution reached approximately 1 or 7, and the products were identified as H‐TiNTs or Na‐TiNTs, respectively. The characteristics and photocatalytic activities of the H‐TiNTs and Na‐TiNTs were compared for various calcination temperatures. The H‐TiNTs were transformed completely to anatase‐type TiO₂ by dehydration during calcination, while the crystallinity of the Na‐TiNTs increased with calcination temperature. However, the photocatalytic H₂ production rates on calcined H‐TiNTs were much higher than on Na‐TiNTs, which could be attributed to the crystalline anatase phase.     

微波固相反应前驱体热分解法制备纳米氧化铜粉体

将固体CuSO4·5H2O和Na2CO3混合均匀后溶于适量乙醇中,然后进行微波辐照,立即反应生成泥浆状固体,将该泥浆状固体洗涤后干燥即可得到粉状前驱体.然后在600 ℃加热1 h分解该前驱体,即可制得纳米氧化铜粉体.在加热速率为10 ℃/min的条件下,对该前驱体进行表征,发现其热分解和晶体化温度约为550 ℃.对制得的纳米氧化铜粉体进行XRD、SEM、TEM和IR分析,结果表明制得的产物为纳米氧化铜粉体,其粉体粒径在30～50 nm,平均粒径约为40 nm.     

TiO_2纳米管阵列的制备及其光催化性能研究

采用阳极氧化法在钛箔上制备了TiO_2纳米管阵列,利用场发射扫描电子显微镜(FSEM)、X射线衍射仪(XRD)和紫外-可见分光光度计对TiO_2纳米管的形貌、结构和光学性能进行表征,详细考察了阳极氧化工艺参数对纳米管阵列形貌的影响,探讨了氧化钛纳米管阵列的形成机理,并对其光催化活性进行了测试,研究结果表明:在0.5 wt; HF和1 mol/L H3PO_4电解液中,控制氧化电压为20 V,反应60 min后,在钛箔表面可获得垂直导向的TiO_2纳米管阵列,管内径为60~80 nm,管壁厚约10 nm;600 ℃热处理后的TiO_2纳米管阵列薄膜对349.7 nm近紫外光和443.9 nm可见光有较强的吸收能力;煅烧温度对纳米管的晶型结构和光催化活性有显著影响.     

Effect of citric acid and starch as emulsifier on phase formation and crystallite size of lanthanum oxide nanoparticles

Lanthanum oxide nanoparticles were synthesized via thermal decomposition method of the lanthanum nitrate in the presence of citric acid or starch as emulsifier. The effects of emulsifier and calcination temperature were investigated on the phase transformation and particle size distribution of the products. La₂O₃ nanoparticles were synthesized by drying lanthanum precursor and emulsifier solution, followed by calcination process at 600 and 900°C, respectively. Products were characterized by Fourier Transform Infrared (FT‐IR) spectroscopy, X‐ray diffraction (XRD), thermal analysis (TG/DTA) and nitrogen adsorption method (porous characteristics). The morphology of the samples analyzed using scanning electron microscopy (SEM). Average crystallite size of the products was calculated by XRD data and average particle size was measured from the TEM micrographs. Lanthanum dioxycarbonate in different forms of the tetragonal and monoclinic is crystallized in the presence of citric acid and starch during the calcination at 600°C, respectively. The hexagonal structure, however, is detected as the only crystalline phase formed by calcination at 900°C.     

Silica nano-particles produced by worms through a bio-digestion process of rice husk

It is reported the production and characterization of silica nano-particles by Californian-red worms through a bio-digestion process of rice husk; the rice husk contains, naturally, high concentrations of silica (22%). The worms were fed gradually with rice husk and water during 5 months to clean the worm’s digestive system from other types of food. The humus was collected, dried at room temperature, pH neutralized and calcined at different temperatures (500, 600 and 700 °C) to remove the organic matter. The calcined humus was digested to remove traces of inorganic compounds. The size of the silica particles was in the range from 55 to 250 nm depending on calcination temperatures. The efficiency in the production of the particles was 88%. These results were compared with those obtained using other agro-industrial wastes that contain silica: coffee (12%) and cane (8%) husk. The samples were characterized by XRD, FTIR, EDS, DLS, SEM and TEM.     

Direct preparation of K0.5Na0.5NbO3 powders

K_0.5Na_0.5NbO₃ powders have been directly synthesized by an alternative solid–state method. Stoichimometric mixture of ammonium niobium oxalate and C₄H₄O₆KNa·4H₂O were calcined in temperature range from 500 to 800 °C for 3 h. The precursor and calcination products were characterized with respect to stoichiometry, purity, crystalline structure, particle size and powder morphology using X–ray diffraction (XRD), X‐ray fluorescence (XRF) spectrometer, scanning electron microscope (SEM), Fourier transform infrared (FTIR) spectra, thermogravimetric (TG) analysis, differential scanning calorimetry (DSC) and UV–Vis diffuse reflectance (UV–Vis) spectroscopy. XRD and XRF results reveal that stoichiometric K_0.5Na_0.5NbO₃ powders could be synthesized by the method. The particle size is about 68 nm for the precursor calcined at 500 °C according to XRD data, which is in good agreement with SEM data. The average band gap energy is estimated to be 3.18 eV by UV–vis diffuse reflectance spectra. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Characterization of chemosynthetic Al2O3-2SiO2 geopolymers

Pure chemosynthetic Al₂O₃-2SiO₂ geoploymers displaying positive alkali-activated polymerization properties and high compressive strength at room temperature were effectively fabricated utilizing a sol-gel method. The molecular structure of the precursor powder and resulting geopolymers were investigated by X-ray diffraction (XRD) and nuclear magnetic resonance (NMR) analysis. In addition, the mechanical and alkali-activated polymerization properties of these materials were also studied. NMR data revealed that the chemosynthetic powders began to contain 5-coordinated Al atoms when the calcination temperatures exceeded 200 °C. These calcined powders were capable of reacting with sodium silicate solutions at calcination temperatures exceeding 300 °C, which is, however, much lower than the temperature required to convert kaolin to Metakaolin.