模拟体液中纳米羟基磷灰石/壳聚糖的制备及表征

从仿生合成的思路出发,分别以模拟体液和含有壳聚糖的模拟体液为反应介质,通过磷酸和硝酸钙反应合成了羟基磷灰石(HAp)和HAp/壳聚糖复合粉体,利用TG-DTA、XRD、FT-IR和TEM等对HAp和HAp/壳聚糖的形成过程、结构及其微观形貌进行了研究.结果表明,在模拟体液中合成的HAp粉体呈现出球状和短棒状形态;HAp/壳聚糖复合粉体呈现出不规则形状,粒度<100 nm,主要晶相为羟基磷灰石.体外生物活性实验结果表明,HAp/壳聚糖复合材料比纯HAp具有更好的生物活性,具有较强的诱导磷灰石沉积能力.     

超声波合成技术在纳米羟基磷灰石制备中的应用

采用超声波合成技术,以硝酸钙和磷酸氢二铵为原料,在恒温、常压下,通过控制合成过程中的超声时间、超声功率,成功合成了粒子尺寸为20nm×50nm、粒度分布窄、分散性好的针状晶体纳米羟基磷灰石．利用扫描电镜（SEM）和X衍射（XRO）来表征粒子的表面形貌和相组成,透射电镜来表征粒子尺寸．讨论了不同合成条件对纳米羟基磷灰石晶体的形态、尺寸及其分散性的影响．结果表明,最佳超声功率为80W、超声时间为1．5h合成出的纳米羟基磷灰石粉末的分散性最好．     

固相反应合成4,4′-硫代双(5-甲基-2-叔丁基苯酚)低聚物抗氧剂

以４,４′－硫代双（５－甲基－２－叔丁基苯酚）为原料,氯化铁作氧化偶联剂,在碳酸钠的存在下应用超声波辐射进行固相反应合成了４,４′－硫代双（５－甲基－２－叔丁基苯酚）低聚物抗氧剂（ＰＴＢＰ）,收率为９８．５％。ＰＴＢＰ合成条件为：４,４′－硫代双（５－甲基－２－叔丁基苯酚）：三氯化铁：碳酸钠（摩尔比）＝１：２：１,超声波频率３３ｋＨｚ,功率１５０Ｗ,反应时间３ｈ,反应温度２５～５０℃。以核磁共振谱（１３Ｃ－ＮＭＲ）、场解吸质谱（ＦＤ／ＭＳ）和元素分析对低聚物结构进行了表征。该方法无反应溶剂,设备空间利用率高,副产物少,产品颜色浅且无需精制     

水热法制备YSZ粉体的转化率和团聚特性研究

将反向共沉淀法制备的Zr（OH）4-Y（OH）3前躯体,分别在160、170、180、190、200℃的温度下水热反应1、2、4h,对粉体的水热转化率、一次粒度和团聚状态进行研究。结果表明,在200℃的温度下,添加一定量的三乙醇胺．水热反应4h可以制得转化率高、团聚少、颗粒大小均匀、形貌接近于球形的氧化钇掺杂的氧化锆粉体。     

纳米碳酸钙干燥方式的研究

以汉白玉废料为起始原料,利用化学方法合成纳米碳酸钙粉体,为了获得无团聚、特性好的碳酸钙粉体,探讨了4种干燥方式:冷冻干燥、真空干燥、喷雾干燥、普通烘箱干燥对纳米碳酸钙粉体形成硬团聚的影响;并用平均粒度、BET和TEM法对制得的纳米碳酸钙粉体进行表征,实验结果表明:冷冻干燥和真空干燥都能防止纳米碳酸钙粉体形成硬团聚,其中冷冻干燥效果更显著,得到的碳酸钙粉体平均粒径为70nm,且分布均匀,比表面积大,冷冻干燥是最好的沉淀干燥方式;经喷雾干燥和烘箱干燥的碳酸钙粉体团聚现象严重,不适宜纳米碳酸钙干燥。同时分析了4种干燥方式中纳米碳酸钙粉体硬团聚形成的原理。     

超声波法制备球形Li3PO4粉末

为了制备锂离子电池正极材料球形LiFePO4,以曲拉通-100(Tx-100)作表面活性剂,用超声波法制备了LiFePO4的前驱体材料μm级球形Li3PO4粉末,并用X射线衍射进行了表征.研究了各种因素对Li3PO4颗粒形态的影响,得到了超声波法制备球形Li3PO4粉末的适宜条件:反应温度为35℃,Li+的浓度为0.6 mol/L,Tx-100的质量百分数为10%,超声波作用时间为5 min.     

物理扰动对针状焦组织结构的影响

以煤焦油沥青为原料,在磁场诱导和超声波空化条件下制备针状焦,并通过扫描电镜SEM和X射线衍射XRD分析了外界物理扰动对针状焦组织结构的影响。结果表明,磁场诱导和超声波空化均能有效地提高针状焦的有序度、石墨化度和结晶度。与超声波空化相比,磁场诱导对针状焦的影响更大,磁场诱导作用下制备的针状焦经过高温煅烧后,其石墨化度达到45.35%。     

溶胶—凝胶法合成PLZT超细粉末

以金属氧化物、无机盐和一种金属醇盐－ 钛酸丁酯为原料, 用溶胶－ 凝胶法合成ＰＬＺＴ （Ｌａ／Ｚｒ／Ｔｉ 为８／６５／３５） 超细粉末, 并研究了ｐＨ 值、温度、干燥过程等工艺条件对溶胶时间和胶凝性能的影响, 通过Ｘ 射线衍射分析, 研究了焙烧温度对ＰＬＺＴ 粉末性能的影响。     

Ce0.9Gd0.1O19.5纳米粉的合成研究

分别采用柠檬酸一硝酸盐法,甘氨酸一硝酸盐法,碳酸盐共沉淀法制备了Ce0.9Gd0.1O19.5粉体。利用XRD、TG-DTA和FI-IR对粉体进行了表征,探讨了合成方法和烧结温度对掺杂CeO2米粉体粒径的影响。结果表明,烧结温度对粉体的粒径大小有较大的影响,采用碳酸盐共沉淀法合成的样品于500℃下焙烧2h后合成的掺杂CeO2粉体的颗粒最小。     

多孔超细碳酸钙微球的制备

采用乳状液膜与共沉淀结合法制备多孔超细碳酸钙微球,考察了不同反应条件对碳酸钙微球形貌的影响.通过X射线衍射、扫描电子显微镜及激光粒度仪对所得的碳酸钙微球的晶体组成、形貌以及粒度进行了表征.结果表明,超细碳酸钙微球生成的最佳工艺条件为:CaCl2溶液浓度0.1mol/L、吐温-80加量4mL、超声乳化5min、搅拌反应3h,此工艺条件下获得多孔碳酸钙微球粒径在2~10μm,球形圆整,且组成为球霰石与方解石的共混体.     

超声波辅助下纳米羟基磷灰石的制备

为有效控制纳米羟基磷灰石粉体的团聚,以硝酸钙和磷酸氢二铵为原料,超声波辅助下合成了纳米羟基磷灰石粉体,并对其进行了900℃的热处理。借助X射线衍射(XRD)、红外吸收光谱(FTIR)、扫描电子显微镜(SEM)、热重差热分析(TG-DTA)对合成的羟基磷灰石进行了物相组成、化学组成、微观形貌、热稳定性的研究。结果表明合成的羟基磷灰石为50nm左右均匀分散的等轴晶,超声处理有效控制了纳米粉体的团聚,热处理能显著提高羟基磷灰石晶粒的结晶度。     

Synthesis of Magnetic Manganese Ferrite

MnFe2O4 polycrystalline powders were prepared by the chemical coprecipitation method. When the reaction temperature is above 80 ℃, through depositing and washing, the MnFe2O4 can be obtained directly without calcining. However, when it is below 80 ℃, we have to calcine the precursor in order to obtain MnFe2O4, which does not result in pure spinal structure but a mixture of MnFe2O4 and α-Fe2O3. The powders＇ magnetic property was characterized with a Vibrating Sample Magnetometer. The phase structure, crystal size and lattice constant were presented by an X-ray diffractometer. In addition, the morphology of the powder was observed with a scan electron microscope and a transmission electron microscope.     

Effects of ultrasonic field on microstructures and properties of semi-solid AZ91D magnesium alloy

The microstructure distribution rule of semi-solid AZ91D alloy treated by ultrasonic was researched, and mechanical properies of specimens before and after ultrasonic treatment were investigated further.Semi-solid AZ91D melt specimens were processed by ultrasonic under different powers, and its microstructures and mechanical properties at different sampling points in specimens were obtained. The experimental results show that the microstructure of AZ91D alloy at different sampling points under the same ultrasonic power is different in grain size and shape, and there is also great difference among their microstructures at the same sampling point under different ultrasonic powers. AZ91D alloy treated by ultrasonic can obtain increment in both tensile strength and plasticity. Under same ultrasonic power, mechanical properties of specimen at different sampling points have obvious difference, and regularity for change of mechanical properties everywhere is similar to regularity for change of grain size and shape everywhere.     

The flowability of ground powders and the comminuting mechanism of mills

The ground powders with the same particle size distribulion and the sanw mean particle diameter were prepared by five different types of mills. The flowability index (FI) and the particle shape indices, namely. Wadell‘s working sphericity ψw and circularity ψc , of five kinds of test powders were nwasured. The effect of the comminuting mechanisms on the flowability of ground powders was investigated, and the relationship between the flowability of ground powders and the partticle shape indices was analyzed. The experimental restdts show that the ground turn,tiers obtained by collision have irregular particle shapes and smooth surfaces, showing a high flowability. On the other hand, though the particle obtained by grinding is close to a spherical particle, but it has a rugged suttee, and shows a bad flowability. Furthermore, the flowability index is more corrdated with the circularity titan the working sphericity is. This means that the surface roughness is more effective, in determining the flowability of powders than the roundtwss is.     

Characterization of ultrafine copper powder prepared by novel electrodeposition method

The auto-evolved ultrafine copper powders were synthesized via a novel electrodeposition route performed by ultrasonic dispersion of the electrolyte. The properties of the samples obtained were characterized by X-ray powder diffractometry (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and laser size distribution analyzer (SL) respectively. The formation mechanisms of the powders and the efficiency of the elctrodeposition were discussed. The results show that the as-prepared powders are high-purity copper nanoparticles with the fcc structure taking a mixture of fishbone-like and irregular shapes. When the concentration of Cu²⁺ increases from 0.03 to 0.09 mol/L, the average size of copper particles increases from 0.92 to 1.80 μm, and current efficiency of electrodeposition linearly changes from 66.5% to 91.3%.     

生石灰粉磨段收尘灰制备轻质碳酸钙工艺

为充分利用石灰石矿的粉矿资源并减少二氧化碳尾气排放,以生石灰粉磨工段收尘灰为原料,利用立窑尾气通过碳化法制备了轻质碳酸钙.首先使用x-射线电子能谱及筛分法对收尘灰的成分及粒度分布进行了测定,然后探讨了水化温度和水化时间对水化过程的影响,并使用扫描电镜对水化产物的形貌进行了研究,最后研究了碳化温度和碳化时间对水化产物碳化过程的影响,并研究了产物形貌.结果表明,其最佳工艺条件为:将收尘灰于100℃条件下水化5~8h,然后使用立窑尾气碳化10~20min,可得到粒度分布均匀的轻质碳酸钙粉体,部分碳酸钙结晶为针状,可用于塑料制品的补强.通过该方法的制备的碳酸钙产品可达到化工行业标准《HG/T 2226-2000》所规定的质量要求.     

从铅阳极泥中制备纳米三氧化二锑粉体的研究

以铅电解精炼过程中的副产物——铅阳极为原料，通过加入碳粉，使铅阳极泥中的高价锑还原成三氧化二锑；在低压下，用直接蒸发冷凝的方法制备了纳米三氧化二锑。此方法无需对铅阳极泥中所含其它成份进行分离，生产成本低。经XRD分析，产品为立方晶型三氧化二锑。SEM分析表明，产品为球形；粒度分布测定表明：平均粒度为66nm，标准差（GSD）为1．67，粒度分布均匀；化学分析表明，产品中所舍三氧化二锑大于97．5％。     

Effects of HIPing pressure on microstructures and properties of TiAl alloy

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Preparation of diamond/Cu microchannel heat sink by chemical vapor deposition

A Ti interlayer with thickness about 300 nm was sputtered on Cu microchannels, followed by an ultrasonic seeding with nanodiamond powders. Adherent diamond film with crystalline grains close to thermal equilibrium shape was tightly deposited by hot-filament chemical vapor deposition(HF-CVD). The nucleation and growth of diamond were investigated with micro-Raman spectroscope and field emission scanning electron microscope(FE-SEM) with energy dispersive X-ray detector(EDX). Results show that the nucleation density is found to be up to 1010 cm-2. The enhancement of the nucleation kinetics can be attributed to the nanometer rough Ti interlayer surface. An improved absorption of nanodiamond particles is found, which act as starting points for the diamond nucleation during HF-CVD process. Furthermore, finite element simulation was conducted to understand the thermal management properties of prepared diamond/Cu microchannel heat sink.     

生蚝壳作为微生物固化砂土钙源的试验研究

微生物诱导碳酸钙沉淀（microbial induced calcium carbonate precipitation,MICP）是一种新兴的环保地基加固技术,使用该技术需消耗大量化学分析级试剂,如尿素、钙盐等,对环境等造成一定的不良影响。基于利用废弃资源的理念,选取厨余垃圾生蚝壳作为MICP固化砂土钙源,并与用硝酸钙、氯化钙作为钙源进行对比。通过无侧限抗压强度试验、渗透试验、碳酸钙质量分数测试、干密度试验和扫描电镜试验（SEM）等探讨该方法的可行性。试验结果表明,以生蚝壳为钙源的MICP固化砂柱的平均孔径最大,但其表观孔隙率最低,无侧限抗压强度、渗透系数、碳酸钙质量分数、干密度等物理力学指标均优于化学钙。SEM试验结果显示,不同钙源固化砂柱砂颗粒表面均有碳酸钙沉淀生成,生蚝壳钙源获得的碳酸钙沉淀晶体形态是表面比较粗糙,伴有微小孔隙的球体形态;硝酸钙获得的碳酸钙沉淀是介于球状和棱柱体之间的多棱角的簇状;氯化钙获得的碳酸钙沉淀呈现颗粒相互交错堆积的簇状。