化学沉淀法制备纳米氧化铝过程中的防团聚研究

分别以无水乙醇、去离子水为溶剂，以NH3·H2O、NH4HCO3为沉淀剂，采用化学沉淀法制备了纳米Al2O3粉体。利用TEM、XRD、nIR和激光粒度仪研究了溶剂、沉淀剂、浓度、前驱体等因素对纳米Al2O3粉体制备过程中的团聚程度的影响。结果表明：当NHaHCO3和Al（NO3）3水溶液浓度分别为3．0mol／L和0．3mol／L时，借助超声分散和微波干燥，得到的纳米Al2O3粉体粒度均匀、分散良好，1100℃煅烧所得粉体平均粒径为20nm。     

以茂名高岭土为原料制备亚微米级α-Al_2O_3粉体

研制粒度分布集中、颗粒圆度好的亚微米α-Al2O3粉体材料是超细氧化铝材料研究领域的一个重要课题。分析了以茂名水洗高岭土的化学组成,并以此高岭土为原料,以酸法制备氧化铝的中间产物硫酸铝铵为铝源,采用尿素沉淀法,进行超细α-Al2O3粉体的制备研究。结果表明,茂名水洗土Al2O3含量高达40%,可用该原料制备出硫酸铝铵;该硫酸铝铵经尿素水解法沉淀,得到前驱体Al(OH)3,前驱体经分散干燥和高温焙烧,得到粒径分布范围在50~170nm之间、粒子形状为球形的亚微米级粉体材料。     

化学共沉淀法制备纯相BiFeO_3粉体

以Bi(NO_3)_3·5H_2O和Fe(NO_3)_3·9H_2O为原料,稀硝酸为溶剂,氢氧化钠作为沉淀剂,采用化学共沉淀法制备铁酸铋前驱体,对前驱体进行煅烧处理得到BiFeO_3粉体。研究了沉淀体系pH值和煅烧工艺对BFO结构及光催化性能的影响。采用XRD、SEM对所制备的BFO粉体进行了表征。结果表明,沉淀体系pH值为8~11范围内,并于600℃下煅烧2h可得到纯相BFO粉体。该粉体具有优异的可见光催化性能,且随BFO的晶粒尺寸增大,其可见光催化降解率提高。     

Ni包裹Al2O3复合粉体的制备

采用非均相沉淀工艺在Al2O3颗粒表面均匀地包裹上镍盐前驱体，经煅烧，还原后得到纳米晶Ni包裹Al2O3复合粉体，相分析表明，非晶态的镍盐前驱体在550℃已转变为NiO，再经700℃氢气处理后，NiO还原为Ni，其晶粒尺寸约为20nm。结果分析表明，复合粉体在热处理过程中，包裹层由连续态变为非连续态。     

沉淀剂对共沉淀法制备Lu2O3发光粉体形貌的影响

研究了共沉淀法制备Eu3 掺杂氧化镥(Lu2O3)发光粉体过程中三种不同的沉淀剂(氨水、碳酸氢铵以及NH3·H2O NH4HCO3两者的混合溶液)对所得粉体形貌的影响.通过差热热重质谱联用(DTA-TG-MS)和红外光谱研究了不同沉淀剂所得沉淀前驱体的热分解行为,结合显微结构观察、粒度分布和比表而积测试,对i种沉淀剂影响Lu2O3晶粒尺寸和团聚状态的规律进行了探讨.研究发现:采用NH3·H2O NH4HCO3混合沉淀剂得到的Lu2O3粉体具有最佳的显微结构和粒径分布状态,沉淀前驱体经1000°C煅烧2h,粉体的平均晶粒尺寸为35nm,中位粒径(D50)为0.48μm.     

部分草酸铅法共沉淀合成Pb(Zr0.52Ti0.48)O3(PZT)粉体

结合部分草酸铅固相反应法的优点对共沉淀法进行改进,发展了一种合成锆钛酸铅(PZT)粉体新工艺.在该工艺中,首先利用共沉淀法制备Zr、Ti的羟基氧化物共沉淀((Zr0.52Ti0.48)O(OH)2,ZTOH),然后以草酸为沉淀剂,在含有ZTOH沉淀物的悬浮液中沉淀铅离子,得到合成PZT粉体的前驱体粉体.利用DTA、TG和XRD对前驱体的热分解行为和相转化过程进行了研究,利用场发射扫描电镜(FESEM)对前驱体的形貌演化进行了观察.前驱体粉体经过700℃煅烧2h,转化为晶化良好的纯相钙钛矿PZT粉体.     

Ni包裹Al2O3复合粉体的制备

采用非均相沉淀工艺在Al2O3颗粒表面均匀地包裹上镍盐前驱体,经煅烧、还原后得到纳米晶Ni包裹Al2O3复合粉体.相分析表明,非晶态的镍盐前驱体在550℃已转变为NiO,再经700℃氢气处理后,NiO还原为Ni,其晶粒尺寸约为20nm.结构分析表明,复合粉体在热处理过程中,包裹层由连续态变为非连续态.     

聚乙二醇在MgAl_2O_4前驱体表面的吸附及改性作用

借助IR光谱、SEM及粒度分析、Zeta电位等测试手段,研究了非离子型表面活性剂聚乙二醇(PEG)大分子对MgAl2O4前驱体表面上的吸附状态和表面性能的影响。结果表明,在沉淀过程中引入PEG1000,并用含有少量PEG1000的溶液洗涤前驱体,可以改变前驱体表面特性,增强空间位阻效应,避免干燥和焙烧过程中形成硬团聚体以及改善粉体的分散性。     

沉淀-氨解法制备超细高纯氮化铬粉体

以氨水直接沉淀法制备的纳米Cr2O3为前驱体,采用氨解法制备了纯度99%以上的高纯超细CrN粉体。对不同氨解温度、氨解时间和不同前驱体合成的CrN粉体用XRD、SEM和氮/氧分析等方法进行了表征。对CrN粉体合成的原理及其主要影响因素进行了分析,并研究了不同前驱体、不同氮化温度和不同氮化时间对CrN粉体性能的影响。结果表明,将氨水直接沉淀法制备的Cr2O3粉体在800℃下利用氨气氮化12h可得到纯度99.15%高纯超细氮化铬粉体,粒径大小约为0.2μm左右。     

尿素法制备纳米氮化锆粉体

利用尿素为固体氮源, 通过尿素分子与ZrCl₄、ZrOCl₂·8H₂O无机锆盐发生络合反应得到Z-U和ZO-U两种ZrN陶瓷的前驱体, 两种前驱体在较低温度下热裂解都可以得到ZrN陶瓷粉体。使用FT-IR对前驱体分子进行了结构分析, 采用TG-DTA跟踪了前驱体的热裂解过程, 并通过XRD和SEM对最终热裂解获得的ZrN产物进行了表征, 探讨了不同锆源制备前驱体的热裂解反应历程及其对产物ZrN的影响。结果显示: 结晶水的存在对络合反应有较大影响, 从而造成两种前驱体分子结构上存在较大差异; 尽管热裂解反应历程相似, 由于前驱体分子结构不同, 获得的ZrN粉体在纯度和形貌上存在较大差异; Z-U前驱体更容易得到纯度高的ZrN纳米粉体。     

电喷雾和二步热处理制备无硬团聚纳米氧化锌

通过电喷雾和二步热处理法制备得到无硬团聚的ZnO纳米微粒, 为制备无硬团聚氧化物纳米粉体提供了一种新方法. 试验采用添加适量PVP的Zn(CH₃COO)₂·2H2O的乙醇溶液作为电喷雾液体, 经过锥形喷雾得到均匀的微米级小液滴. 干燥后的喷雾产物先后在氮气炉和空气炉中分别600℃和400℃保温1h进行二步热处理. SEM、XRD测试结果表明, 使用该方法制备得到的ZnO纳米微粒粒度均匀, 结晶完整, 无硬团聚, 具有六角纤锌矿结构.     

Modified oxide sol-gel (MOSG) synthesis of borophosphosilicate glasses and glass-ceramics

A modified oxide sol-gel (MOSG) process was used to synthesize borophosphosilicate glasses and glass-ceramics using boron oxide and phosphorous pentoxide as starting precursors. The oxide precursors were used to form alkoxidesin situ, which were then hydrolysed and condensed to form borophosphosilicate gels. The dried gels were analysed for their thermal properties and were heat treated accordingly, at a temperature of 800 °C, to crystallize the boron phosphate phase. The resultant xerogels were then analysed for their microstructure. Both pressureless and hot-pressing techniques were used to sinter the calcined gels to form glass-ceramics. The sintered samples were characterized for their microstructure using electron microscopy and evaluated for their dielectric properties. Dielectric measurements indicate that the sintered glass-ceramics possess dielectric constants less than 5 and dissipation factors less than 0.001 at a frequency of 1 MHz. The results of these studies show the potential of the oxide sol-gel-derived borophosphosilicate glass-ceramics for use as substrate materials in microelectronic packaging.     

改性多省并醌的合成与性能研究

合成了两种新型蒽醌单体:1,4-二(辛氧基)蒽-9,10-二酮和1,4-二(丁氧基)蒽-9,10-二酮。通过红外、核磁和元素分析确证了单体的结构。DSC、TG结果显示两种新型单体的5%质量损失温度最高可达266.4℃。将新型蒽醌单体与均苯四甲酸酐在硝基苯中预聚,再将预聚产物在NaCl/AlCl3熔盐中继续反应得到改性多省并醌聚合物。通过红外光谱、热分析等方法表征改性聚合物的结构并研究了改性聚合物的介电性能。研究结果表明改性聚合物仍有较好的热稳定性,5%质量损失温度>387℃;20Hz下改性聚合物的最大介电常数值为100,比改性前低。同时合成了乙醇可溶的改性多省并醌聚合物,20Hz下最大介电常数为19997。     

Electrophoretic deposition of nano-sized BaTiO3

In this study, a non-aqueous method in a simple one pot reaction process was employed to synthesize nano-sized BaTiO₃ particles and then electrophoretic deposition technique was employed for thin film coatings. In the first step of the preparation, metallic barium is directly dissolved in benzyl alcohol at slightly elevated temperatures. Then titanium isopropoxide was added following by a solvothermal treatment. At the end of the reaction, nearly spherical BaTiO₃ nanoparticles were obtained typically 5 nm in diameter. After establishing the stability of the BaTiO₃ suspension in ethanol, electrophoretic deposition process was performed without any additional operation. Alumina with platinum plating was used as substrate. To achieve the optimal process parameters, various voltages were applied by altering the cathode to anode distance as well as deposition time. High voltages application was possible without causing hydrolysis, because of the non-aqueous ethanol medium with higher surface charge of the nanoparticles. The deposited surface coatings were dried in air and sintered at various temperatures. SEM, EDX and XRD analysis were employed for the investigation of the coating.     

The control of paracetamol particle size and surface morphology through crystallisation in a spray dryer

The parameters governing the crystallisation of paracetamol using various conventional techniques has been extensively studied, however the factors influencing the drug crystallisation using spray drying is not as well understood. The aim of this work was to investigate the crystallisation of an active pharmaceutical ingredient through evaporative crystallisation using a spray dryer to study the physicochemical properties of the drug and to use semi-empirical equations to gain insight into the morphology and particle size of the dried powder. Paracetamol solutions were spray dried at various inlet temperatures ranging from 60 °C to 120 °C and also from a series of inlet feed solvent compositions ranging from 50/50% v/v ethanol/water to 100% ethanol and solid-state characterisation was done. The size and morphology of the dried materials were altered with a change in spray drying parameters, with an increase in inlet temperature leading to an increase in particle Sauter mean diameter (from 3.0 to 4.4 µm) and a decrease in the particle size with an increase in ethanol concentration in the feed (from 4.6 to 4.4 µm) as a result of changes in particle density and atomised droplet size. The morphology of the dried particles consisted of agglomerates of individual crystallites bound together into larger semi-spherical agglomerates with a higher tendency for particles having crystalline ridges to form at higher ethanol concentrations of the feed.     

Silica Glass from Aerosil by Sol-Gel Process: Densification and Textural Properties

Sol-gel processes allow the synthesis of inorganic materials from solutions of molecular precursors. These precursors can be either organic, inorganic, or a mixture of the two. The aim of this work is the preparation of aqueous solutions consisting of Aerosil OX 50 (fumed silica) using small amount of additives like ammonium fluoride NH₄F (less than 2%), which are dried at room temperature in order to obtain monolithic gels. These are then densified at temperatures below 1200°C and sintered at 1300°C in order to obtain pure silica glass. The textural properties evolution of these gels is investigated as a function of temperature by thermal analysis (mass loss, shrinkage, and density) and scanning electron microscopy.     

乙酸异戊酯共沸干燥法制备低团聚掺锑氧化锡纳米微粉

以SnCl4·5H2O和SbCl3乙醇溶液为原料,用阴离子树脂交换除氯水解法制备得到无氯离子的前驱体掺锑氢氧化锡胶体沉淀。首次对以含氧官能团为主的系列憎水有机溶剂进行了共沸干燥脱水研究,并对所得粉体团聚程度进行比较。实验发现掺锑氧化锡共沸脱水干燥效果与有机溶剂分子结构之间有密切关系,提出了选择共沸有机溶剂的3个原则,在一系列有机溶剂中选择了最符合的乙酸异戊酯进行干燥实验,与常用的正丁醇共沸溶剂进行了消除粉体团聚效果的比较。运用IR、BET、TEM、XRD等方法对掺锑氢氧化锡粉体的结构、比表面积、形貌、物相进行表征。结果表明,乙酸异戊酯溶剂是理想的共沸干燥有机溶剂,其干燥所得掺锑氢氧化锡蓬松粉体的比表面积为284.44m2/g,比用正丁醇处理的增大了22%。将乙酸异戊酯干燥所得的掺锑氢氧化锡微粉经热处理后得到了低团聚的掺锑氧化锡纳米微粉。     

The effect of ethanol on the formation and physico-chemical properties of particles generated from budesonide solution-based pressurized metered-dose inhalers

The aerosol performance of budesonide solution-based pressurized metered-dose inhalers (HFA 134a), with various amounts of ethanol (5–30%, w/w) as co-solvents, was evaluated using impaction and laser diffraction techniques. With the increase of ethanol concentration in a formulation, the mass median aerodynamic diameter was increased and the fine particle fraction showed a significant decline. Although data obtained from laser diffraction oversized that of the impaction measurements, good correlations were established between the two sets of data. Particles emitted from all the five formulations in this study were amorphous, with two different types of morphology – the majority had a smooth surface with a solid core and the others were internally porous with coral-like surface morphology. The addition of ethanol in the formulation decreased the percentage of such irregular-shape particles from 52% to 2.5% approximately, when the ethanol concentration was increased from 5% to 30%, respectively. A hypothesis regarding the possible particle formation mechanisms was also established. Due to the difference of droplet composition from the designed formulation during the atomization process, the two types of particle may have gone through distinct drying processes: both droplets will have a very short period of co-evaporation, droplets with less ethanol may be dried during such period; while the droplets containing more ethanol will undergo an extra condensation stage before the final particle formation.     

Effects of ethanol to water ratio in feed solution on the crystallinity of spray-dried lactose

In the present study, the effects of ethanol to water ratio in feed solution on the physical properties of spray-dried alpha-lactose monohydrate were evaluated. Crystallinity of the spray-dried lactose was determined by isothermal microcalorimetry (IMC) and by differential scanning calorimetry (DSC). Water content of the spray-dried lactose was determined by thermogravimetric analysis and the surface area was evaluated by Brunauer, Emmett, and Teller (BET) method. The crystallinity of spray-dried lactose varied from 0% to 100%, depending on the ratio of ethanol to water in the feed solution. Lactose spray dried from pure ethanol was 100% crystalline and contained hydrate water. Lactose spray dried from pure water was 100% amorphous. The feed solution substantially affected the ratio of surface water to hydrate water, as the content of surface water increased and hydrate water decreased, while the crystallinity of spray-dried lactose decreased. Surface area of the spray-dried lactose increased as a function of amorphous content.     

Effects of Ethanol to Water Ratio in Feed Solution on the Crystallinity of Spray-Dried Lactose

ABSTRACT

In the present study, the effects of ethanol to water ratio in feed solution on the physical properties of spray-dried α-lactose monohydrate were evaluated. Crystallinity of the spray-dried lactose was determined by isothermal microcalorimetry (IMC) and by differential scanning calorimetry (DSC). Water content of the spray-dried lactose was determined by thermogravimetric analysis and the surface area was evaluated by Brunauer, Emmett, and Teller (BET) method. The crystallinity of spray-dried lactose varied from 0% to 100%, depending on the ratio of ethanol to water in the feed solution. Lactose spray dried from pure ethanol was 100% crystalline and contained hydrate water. Lactose spray dried from pure water was 100% amorphous. The feed solution substantially affected the ratio of surface water to hydrate water, as the content of surface water increased and hydrate water decreased, while the crystallinity of spray-dried lactose decreased. Surface area of the spray-dried lactose increased as a function of amorphous content.