离子液体辅助制备粒度均匀的铁酸锌纳米粉体

以离子液体作为辅助反应介质,采用水热合成法制备了铁酸锌纳米粉体,并利用XRD和TEM研究了反应温度、压力和反应环境对铁酸锌晶相组成、粒度大小的影响.结果表明：制备的样品为纳米结构的单相铁酸锌,随着反应温度和反应环境的变化,半峰宽明显的不同;适当提高反应温度,能够明显地细化晶粒,促进晶粒形成;改变反应压力,对铁酸锌纳米晶粒形成有影响;在反应过程中添加适量的离子液体[EMIM]PF6,能够加速晶粒细化,有效促进铁酸锌纳米晶粒形成.     

Effect of sintering temperature on phase evolution of Al_(86)Ni_6Y_(4.5)Co_2La_(1.5) bulk amorphous composites synthesized via mechanical alloying and spark plasma sintering

Al_(86)Ni_6Y_(4.5)Co_2La_(1.5) amorphous powders were synthesized by mechanical alloying for 200 h. Subsequent consolidation was performed via spark plasma sintering in the temperature range of 250 ℃ to 500 ℃ at the pressure of 500 MPa. The role of viscous flow on densification was investigated by studying the viscosity change of the amorphous phase at different consolidation temperatures. The decrease in viscosity at higher sintering temperatures resulted in better particle bonding and densification of consolidated samples. The formation of only FCC Al was observed in the consolidated samples at sintering temperatures ≤ 300 ℃ and the intermetallic phases formed at temperatures ≥ 400 ℃. The mechanical properties of the bulk samples were measured by Vickers microhardness and nanoindentation tests. The testing results showed that the average values of microhardness, nanohardness and elastic modulus of the sample consolidated at 500 ℃ were 3.06 ± 0.14 GPa,4.85 ± 1.14 GPa and 89.53 ± 9.25 GPa, respectively. The increase in hardness and elastic modulus of the higher temperature consolidated samples is attributed to the improvement in particle bonding, densification and distribution of various hard intermetallic phases in the amorphous matrix.     

保温时间对铝厂废渣研制的氧化铝磨介微观结构及性能影响

以铝型材厂废渣为主要原料,通过添加少量粘土,滑石及碳酸钡复合助烧剂研制刚玉耐磨瓷球.探讨不同保温时间对瓷球微观结构及各项性能指标的影响.采用XRD和SEM等测试手段探讨其晶相结构和显微结构并测试抗弯强度、硬度、磨损率和气孔率等性能指标.结果表明:最佳保温时间为3 h,此时样品由4种晶相组成,其中刚玉为主晶相,含量约75%,其各项性能分别为:吸水率为0.032%,气孔率为0.105%,体积密度为3.289 g/cm3,抗弯强度为136 MPa,显微硬度为8.25 GPa,磨损率为0.044 1%/h.     

不同表面活性剂对CoSb_3纳米粉体的影响及其非晶化研究

分别选用不同的表面活性剂(SDBS、CTAB、EDTA、PVP),采用水热法成功制备CoSb_3纳米粉体.对制备的纳米粉体分别进行XRD和SEM表征,研究了不同表面活性剂对制备的CoSb_3纳米粉体的影响.结果表明不同表面活性剂对制备的CoSb_3纳米粉体形貌有显著的影响.并将水热法制备的CoSb_3纳米粉体,采用脉冲激光非晶化技术进行处理,结果表明纳米粉体实现了部分非晶化.通过样品的XRD分析研究了影响CoSb_3纳米粉体部分非晶化的条件,结果表明扫描重复次数的增加可以提高CoSb_3基方钴矿热电材料的非晶化能力,适当提高扫描速度有利于CoSb_3基方钴矿热电材料的非晶化.     

Efficient inactivation of Staphylococcus aureus by silver and copper loaded photocatalytic titanate nanotubes

One dimensional titanate nanotubes(TNTs) were synthesized by microwave assisted alkaline hydrothermal process. The process was followed by UV-photodeposition of Ag and Cu on the surface of TNTs to enhance the photocatalytic activity in visible light spectrum. The loading of Ag and Cu(single and combination mode)offered a new insight to inactivate multi-drug resistant micro-organisms. The antibacterial properties of these samples were studied on Gram positive bacteria, Staphylococcus aureus(S. aureus) using well diffusion method.The TNTs with Ag and Cu loading showed a clear zone of inhibition after overnight incubation of S. aureus. The bacterial inactivation efficiency of nanoparticles in the visible light was further analyzed by kill kinetics. TNTs with Ag and/or Cu loading showed a significant reduction in bacterial growth. Cu co-loaded with Ag sample showed the highest inactivation efficiency within 90 min of visible light irradiation. To elucidate the mechanism of bactericidal properties of samples under visible light irradiation, the formation of reactive oxygen species(ROS), particularly, superoxide radical anion was determined by nitro blue tetrazolium(NBT) assay and the protein degradation by each samples were measured. Based on overall results, it was observed that the Cu coloaded with Ag on TNTs samples were found to be more effective as compared to either Ag or Cu loaded TNTs. It provides new avenues for utilizing the combination of Cu and Ag for enhancing the antimicrobial efficacies for different nanoparticles.     

两种加热法合成乙酰苯胺的对比实验研究及其教学效果探讨

分别用常规加热法和微波辐射法合成了乙酰苯胺.结果表明:常规加热法合成的最佳时间为45min,微波辐射法为4min,反应时间比常规加热法缩短了约11倍.微波辐射法的转化率比实验教材给定反应30min的转化率提高了约30%.与学生用常规加热法所得的实验数据比较,微波辐射法得到的收率高,产物纯度高.因此,微波辐射法具有反应速度快、转化率高、产物纯度高等优点.用微波辐射法合成乙酰苯胺既能很好地解决目前学生实验学时紧张的教学问题,又能达到很好的实验效果.     

K0.5Na0.5(TaxNb1-x)O3纳米粉体的合成及其光吸收特性研究

采用水热法在一定条件下合成K0.5Na0.5(TaxNb1-x)O3 (x=0.09,0.23,0.49,0.69,0.89)纳米粉体,利用XRD、SEM和UV-vis吸收光谱等手段分别对产物的物相、形貌和光吸收等特性进行表征.结果表明,随着Ta含量的增加,产物由正交相结构转变为四方相结构,再由四方相结构转变为立方相结...     

微波合成非晶形ZrO_2纳米粒子

在Zr(NO3) 4·5H2 O、聚乙二醇 (PEG)和脲的水溶液中 ,通过微波加热合成了约 8nm的非晶形ZrO2 纳米粒子 ,并用XRD、TEM进行了表征。     

热敏材料聚N-异丙基丙烯酰胺的结构对其溶胀性能影响

本文主要研究热敏材料聚N-异丙基丙烯酰胺 (PNIPAAm) 的结构对其溶胀性能影响。分别采用水热法和微波辐射法合成PNIPAAm热敏水凝胶，应用扫描电镜观察了两种合成方法制得的水凝胶的表面结构，测定了水凝胶随温度变化的溶胀率曲线及其溶胀和退溶胀动力学，并讨论了水凝胶的结构对其溶胀率的影响。结果表明：与水浴法制备的水凝胶相比，微波辐射法所得到的水凝胶无论是在干燥状态下还是溶胀状态下都具有更为丰富发达且较大的孔隙结构，在溶胀过程中，微波辐射法合成的水凝胶在临界溶解温度(LCST)以下具更高的溶胀率，而在LCST以上时，能更多地释放水而具有更低的溶胀率。此外，微波辐射所合成的水凝胶由于具有较为发达的孔隙结构，使其比水浴法制备的水凝胶具有更快的溶胀速度和退溶胀速度。     

微波合成LiCoO2及其结构表征

以Co2O3和LiOH·H2O为原料,微波加热合成锂离子电池正极材料LiCoO2·考察了微波输出功率、微波加热时间及保温时间对产物结构和组成的影响,用XRD实验对所得产品进行表征·结果表明,当微波输入功率为360W,加热时间为10min,保温时间为10min时,产品是单一相层状结构LiCoO2,晶格常数和标准值一致·SEM实验显示,该反应条件下制备LiCoO2样品颗粒边缘清晰、光滑,颗粒度约为5μm,粒度分布较均匀·对LiCoO2的微波合成机理进行了探讨,结合XRD实验,说明Co2O3和LiOH·H2O反应生成LiCoO2分两步完成·     

不同反应温度和原料对化学沉淀法制备纳米羟基磷灰石的影响

使用不同磷源与钙源制得纳米羟基磷灰石,并利用X射线衍射、红外光谱、透射电镜、热重分析等分析手段对产物进行表征,探究不同的反应温度、不同原料等实验条件对产物的组成、形貌及尺寸的影响。结果表明：升高温度有利于晶体生长;不同钙源对产物的影响不大,改变磷源对产物组成的影响较大;产物羟基磷灰石中的磷酸根会被磷酸氢根所取代,并且以磷酸氢二钠为原料时产物中磷酸氢根含量最高。     

微波镁热还原法制备ZrB2粉体及表征

以二氧化锆、硼酸和镁粉为原料,利用微波镁热还原法合成了纳米级的ZrB₂粉体。研究了镁粉含量与合成工艺对ZrB₂粉体的影响,通过TG-DTA分析了物相在不同温度下的反应过程,利用XRD、EDS和TEM考察了产物的组成和形貌。实验结果表明：采用微波镁热法,加热时间为20min就可得到ZrB₂粉体,杂相Zr₂O和Mg₃B₂O₆等为镁热反应中副反应生成的产物;当原料配比为n(Zr₂O)∶n(H₃BO₃)∶n(Mg)=1∶3∶4时,合成产物中ZrB₂的相对含量最高;合成的ZrB₂粉体为球状,平均粒径为80nm左右;加入NaCl有助于降低ZrB₂颗粒尺寸。     

Microwave sintering effects on the microstructure and mechanical properties of Ti-51at%Ni shape memory alloys

Ti-51at%Ni shape memory alloys (SMAs) were successfully produced via a powder metallurgy and microwave sintering technique. The influence of sintering parameters on porosity reduction, microstructure, phase transformation temperatures, and mechanical properties were investigated by optical microscopy, field-emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD), differential scanning calorimetry (DSC), compression tests, and microhardness tests. Varying the microwave temperature and holding time was found to strongly affect the density of porosity, presence of precipitates, transformation temperatures, and mechanical properties. The lowest density and smallest pore size were observed in the Ti-51at%Ni samples sintered at 900℃ for 5 min or at 900℃ for 30 min. The predominant martensite phases of β2 and β19' were observed in the microstructure of Ti-51at%Ni, and their existence varied in accordance with the sintering temperature and the holding time. In the DSC thermograms, multi-transformation peaks were observed during heating, whereas a single peak was observed during cooling; these peaks correspond to the presence of the β2, R, and β19' phases. The maximum strength and strain among the Ti-51at%Ni SMAs were 1376 MPa and 29%, respectively, for the sample sintered at 900℃ for 30 min because of this sample's minimal porosity.     

三氟化钐纳米圆盘的超声合成及表征

室温条件下,采用温和的超声液相沉淀法制备得到了三氟化钐纳米圆盘.产物的晶相、形貌和尺寸分别用X射线衍射(XRD)、场发射扫描电镜(FE-SEM)、透射电镜(TEM)进行了表征.结果表明,所得三氟化钐为高纯、结晶度好的六方晶系,纳米圆盘厚度约为50nm,直径为300～500 nm.进一步检测了SmF3:Tb3+纳米圆盘的荧光性质.     

微波辐射制备含铕荧光配合物及其性能表征

以苯甲酸（BA）为第一配体、邻菲罗啉（Phen）为第二配体、铕离子（Eu计）为中心离子,采用微波辐射的方法制备了含铕荧光配合物,通过元素分析、FT-IR和1HNMR确定配合物组成为Eu（BA）3Phen,采用TGA、XRD和荧光分光光度计对其性能进行测试分析：TGA结果表明配合物的起始分解温度为270℃,热稳定性良好;荧光分光光度计和XRD显示荧光性能优异且具有良好的结晶性能;与普通的制备方法相比,极大地缩短了反应时间,显著提高了反应效率．     

Studies on Wear and corrosion resistances of carbon nitride thin films on Ti alloy

0　IntroductionArtificialarthrosiseshavebeenwidelyusedintheoperatorsclinicalsurgeriesforthepatientswhosearthrosiseswerese riouslyseverelydamaged.Butmostofartificialarthrosisescanon lybeusedforabouttenyearslongduetotheseriousabrasion .Forthisreason ,theimprovementofthelongevityofartificialarthrosisbecomesanimportantsubjectofstudy .TheartificialarthrosisesbeingmadeupofTialloyTC4(Ti 6Al 4V)andthepolythenewithultrahighmolecularweighthavegreatpotentialitiesonim provinglongevitybecauseTC4canreac…     

Gd2Zr2O7烧绿石的高温高压快速合成

为了研究Gd₂Zr₂O₇烧绿石的合成条件,以Gd₂O₃,ZrO₂混合粉体为原料,在1 773 K的温度、3 GPa和5.2 GPa的压力及10～30 min的保温保压时间内,进行了高温高压实验。借助于XRD,SEM,IR等分析,对合成样品结构、形貌等进行表征,结果表明:在1 773 K的高温、5.2 GPa的高压和10 min的保温保压条件下可合成单一物相的Gd₂Zr₂O₇立方烧绿石。为固化锕系核素的陶瓷基材合成及其固化体的制备提供了一种快速高效的方法。     

钒钛磁铁矿微波助磨实验

针对我国复杂难处理钒钛磁铁矿资源特点,研究了微波加热对钒钛磁铁矿磨矿性能的影响,揭示了钒钛磁铁矿在微波作用下选择性破碎与界面破碎特性.结果表明:微波场中,矿石的温度随着矿石粒度的增大而增加,且微波功率对矿石升温性能的影响最显著;X射线衍射分析与SEM分析表明,微波预处理后矿石内部会产生大量的晶界裂纹,使更多的单体矿物解离出来;在微波功率为4 k W、加热时间100 s后的磨矿产物中,小于0.074 mm粒级的质量分数由原矿的72%提高到95%.     

Tb~(3+)掺杂β-Ga_2O_3纳米粉末的结构和光致发光性质的研究

采用溶胶-凝胶法制备Tb3+掺杂β-Ga2O3纳米粉末.用X-射线衍射(XRD)、拉曼(Raman)、光致发光激发谱(PLE)和发光谱(PL)对其进行了一系列的表征. XRD 和 Raman 的结果表明: Tb3+离子的掺入没有改变β-Ga2O3结构.用350 nm的激发光去激发Tb3+掺杂β-Ga2O3纳米粉末,样品的最强峰在543 nm (5D4-7F5)附近,对应着Tb3+离子的绿光发射.此外,还讨论了能量传递机制.     

Phosphorus partitioning and recovery of low-phosphorus iron-rich compounds through physical separation of Linz-Donawitz slag

The Linz-Donawitz (LD) steelmaking process produces LD slag at a rate of about 125 kg/t. After metallic scrap recovery, the non-metallic LD slag is rejected because its physical/chemical properties are unsuitable for recycling. X-ray diffraction (XRD) studies have indicated that non-metallic LD slag contains a substantial quantity of mineral phases such as di- and tricalcium silicates. The availability of these mineral phases indicates that LD slag can be recycled by iron (Fe)-ore sintering. However, the presence of 1.2wt% phosphorus (P) in the slag renders the material unsuitable for sintering operations. Electron probe microscopic analysis (EPMA) studies indicated concentration of phosphorus in dicalcium silicate phase as calcium phosphate. The Fe-bearing phases (i.e., wustite and dicalcium ferrite) showed comparatively lower concentrations of P compared with other phases in the slag. Attempts were made to lower the P content of LD slag by adopting various beneficiation techniques. Dry high-intensity magnetic separation and jigging were performed on as-received samples with particle sizes of 6 and 3 mm. Spiral separation was conducted using samples ground to sizes of less than 1 and 0.5 mm. Among these studies, grinding to 0.5 mm followed by spiral concentration demonstrated the best results, yielding a concentrate with about 0.75wt% P and 45wt% Fe.