Fe_3O_4/PANI抗氧化水基磁流体的制备与表征

在无氮气保护条件下,用化学共沉淀法制备了四氧化三铁(Fe3O4)纳米颗粒,并通过表面原位合成法将颗粒用聚苯胺(PANI)包裹,由此获得兼具磁性和导电性能的纳米四氧化三铁/聚苯胺(Fe3O4/PANI)材料。作者称其为Fe3O4/PANI抗氧化水基磁流体。透射电子显微镜(TEM)分析表明,该法制备的Fe3O4/PANI复合粒子的粒径在30~50 nm,其分散性能比包裹前的Fe3O4粒子明显改善。红外光谱(FTIR)和X射线衍射(XRD)测试结果发现,Fe3O4粒子及Fe3O4/PANI复合粒子具有不同的物态和晶相结构。对纳米复合粒子的抗氧化性能和磁性能的检测证实,原位合成的Fe3O4/PANI复合粒子不仅能有效防止在空气中被氧化,还可在磁场环境中实现快速富集、定位,为Fe3O4/PANI纳米复合粒子在生物医学领域的应用提供了可能。     

GO/CaCO_3复合材料的制备及其药物缓释性能

以经氨基修饰的CaCO_3(CaCO_3-NH_2)和氧化石墨烯(GO)为反应物制备了复合材料(GO/CaCO_3-NH_2)。通过透射电镜(TEM)和傅里叶红外(FT-IR)对材料进行表征,发现GO成功地包裹在CaCO_3的表面,二者通过静电作用结合。对GO/CaCO_3-NH_2复合材料进行了药物布洛芬的载药和缓释性能的研究,结果表明:与CaCO_3相比,GO/CaCO_3-NH_2复合材料具有更高的载药量和更好的缓释性能。载药量从19.56%增加到39.70%,药物连续释药72 h时累积释放量达到53.49%,明显延长了药物作用时间。当质量浓度为75μg/m L时,复合材料的细胞增值率降至73%。GO/CaCO_3-NH_2复合材料在药物缓释体系中有潜在应用。     

希夫碱改性Fe3O4杂化材料的制备与表征

将制备的Fe3O4@SiO2-NH2磁性杂化材料依次经过丙烯酸甲酯(MA)、乙二胺(EDA)和水杨醛(SA)的接枝,得到希夫碱改性的Fe3O4杂化材料(Fe3O4@SiO2-S2),并通过FTIR、XRD、SEM、TEM、VSM对杂化材料的结构进行表征.结果表明,Fe3O4@SiO2-S2材料核壳结构明显,饱和磁化强度为45.9 emu/g.对水溶液中重金属离子的吸附实验结果表明,Fe3O4@SiO2-S2对Hg2+具有选择吸附性,pH=6、45℃条件下,饱和吸附量可达到362 mg/g(1.12 mmol/g),优于Fe3O4@SiO2-NH2、均相体系制备的希夫碱改性的Fe3O4@SiO2复合材料(Fe3O4@SiO2-HO-S)等吸附剂,且在5次循环使用后吸附性能仍能保持89％以上,吸附时间约300 min达到吸附平衡,吸附等温线符合Langmuir等温吸附模型.     

铁氧化物/铝体系绝热温度数值计算与分析

基于热力学基本原理,对铁氧化物/铝体系绝热温度进行计算机数值计算与分析。结果表明:不同铁氧化物/铝体系(FeO/Al、Fe2O3/Al及Fe3O4/Al)常温下发生燃烧合成反应的绝热温度均为产物Fe的沸点温度(3 148.2 K),且Fe的气相转变率(摩尔比)各不相同,分别为20.6%FeO/Al,21.3%Fe2O3/Al,2%Fe3O4/Al。通过在体系中添加不同含量的铁合金,可以降低体系的绝热温度及产物的相转变率,对于Fe2O3/Al体系,铁合金添加量为0～1.35 mol及3.75～5.1 mol时,可以控制产物Fe气相及Al2O3液相的转变率。当添加铁合金含量使得体系绝热温度低于1 800 K时,燃烧波不能自维持反应,通过对体系进行预热,可以实现燃烧合成反应燃烧波的自维持,预热温度越高,铁合金可添加量越大。     

Fe_2O_3对天然原料合成Al_4SiC_4/Al_4O_4C复合耐火材料的影响(英文)

以焦宝石、活性炭和铝粉为原料并添加Fe2O3后制备了Al4SiC4/Al4O4C复合耐火材料。利用化学分析、X射线衍射和扫描电镜研究了Fe2O3对所制备复合材料的物相组成和显微结构的影响。结果表明:在烧结过程中,从1400℃开始,Fe2O3转变为低熔点物相Fe3Si,产生液相促进Al4SiC4成核、细化晶粒,同时包裹Al4SiC4。此外,未添加Fe2O3的样品中生成的Al4O4C短纤维,Fe2O3的加入使得Al4O4C相变为细小的晶粒。     

铁氧化物/铝体系绝热温度数值计算与分析EI北大核心CSCD

基于热力学基本原理,对铁氧化物/铝体系绝热温度进行计算机数值计算与分析。结果表明:不同铁氧化物/铝体系(FeO/Al、Fe2O3/Al及Fe3O4/Al)常温下发生燃烧合成反应的绝热温度均为产物Fe的沸点温度(3148.2 K),且Fe的气相转变率(摩尔比)各不相同,分别为20.6%FeO/Al,21.3%Fe2O3/Al,2%Fe3O4/Al。通过在体系中添加不同含量的铁合金,可以降低体系的绝热温度及产物的相转变率,对于Fe2O3/Al体系,铁合金添加量为0~1.35 mol及3.75~5.1 mol时,可以控制产物Fe气相及Al2O3液相的转变率。当添加铁合金含量使得体系绝热温度低于1800 K时,燃烧波不能自维持反应,通过对体系进行预热,可以实现燃烧合成反应燃烧波的自维持,预热温度越高,铁合金可添加量越大。     

聚丙烯酸/氧化石墨烯自修复水凝胶的合成及性能

通过改进的Hummers方法成功制备了氧化石墨烯(GO)。以Fe3+为交联剂、丙烯酸(AA)为单体、GO为增强剂,采用原位聚合法制备了聚丙烯酸(PAA)/GO自修复水凝胶。考查了不同GO含量下,PAA/GO自修复水凝胶的溶胀性能,并探讨了GO含量、Fe3+含量和H2O含量对PAA/GO自修复水凝胶力学性能的影响,研究了PAA/GO自修复水凝胶的自修复性能。结果表明,Fe3+含量、GO含量和H2O单体含量分别为0.5 %（摩尔分数）、0.5 %（质量分数,下同）、80 %时,具有最佳力学性能（其拉伸强度为743.5 kPa,断裂伸长率为2940.5 %）;GO含量为0.25 %时,PAA/GO自修复水凝胶的吸水性能最大;PAA/GO自修复水凝胶具有优异的自修复性能。     

微孔金属有机框架担载多酸型催化剂的合成及应用

多金属氧酸盐化合物是指一类具有纳米尺寸的金属-氧簇化合物。本实验根据文献资料以磷钨酸盐为模板,合成了具有特殊结构的一种POMs/MOFs杂化化合物,可作为担载多酸型催化剂用于催化甲醇生成二甲醚,化学式为H_3[( Cu_4Cl)_3( BTC) ]_2[PW_(12)O_(40)]·( C_4H_(12)N)_6·3H_2O,并对这一种化合物进行催化分析、结构分析和热重分析。实验结果表明:这类杂化物具有较强的催化性能和热稳定性,是一类具有较强的催化应用前景的无机-有机杂化材料。     

冻融法制备微米级Fe3O4/聚乙烯醇磁性水凝胶及其磁力学性能研究

以微米级Fe3O4粉末和聚乙烯醇(PVA)为原料,采用反复冷冻-融化技术(冻融)制备了Fe3O4/PVA磁性水凝胶,研究了磁性水凝胶的力学性能、磁场阈值,磁性能等随Fe3O4的含量及冻融次数的变化行为,并使用扫描电子显微镜(SEM)以及X射线衍射(XRD)分别研究了Fe3O4/PVA磁性水凝胶的微观形貌和结晶性能.结果表明随冻融循环次数的增加,Fe3O4/PVA磁性水凝胶的力学性能、磁场阈值,及磁性能等均随Fe3O4的含量及冻融次数显著变化;Fe3O4在磁性水凝胶中分布均匀,PVA水凝胶经反复冷冻-融化后结晶性能有所提高.     

以铁泥为原料合成Fe_2O_3并制备LiFePO_4/C

采用溶解还原、沉淀、球磨、灼烧、稀HNO3处理等工艺过程,将铁泥中的Fe以Fe2O3的形式回收。以得到的Fe2O3为原料经过高温固相法合成Li Fe PO4/C作为锂离子电池的正极材料。分别研究了"球磨"和"稀HNO3处理"两个工艺步骤对产品性能的影响。XRD分析结果表明Li Fe PO4/C属橄榄石型晶系纯相。SEM图片显示Li Fe PO4/C颗粒均匀,尺寸分布在100~150 nm之间。通过电池充放电测试表征了Li Fe PO4/C的电化学性能,实验结果表明,由于采用优化的工艺过程制备的Fe2O3中适量保留了铁泥中的Co、Cr和Ni元素,所合成的Li Fe PO4/C表现出较好的循环稳定性和倍率性能。     

Polymorphism of LiGa5O8 and of LiGa5O8-MgGa2O4Solid Solutions

High-temperature X-ray diffraction and differential thermal analyses showed that LiGa₅O₈ exists in two polymorphs related by the first-order transition at 1138°±3°C of the low-temperature simple-cubic form, space group (probably) O⁷, to the high-temperature spinel (fcc) form, space group O _h ⁷. The transition is rapid, and the high-temperature form in pure LiGa₅O₈ could not be quenched to room temperature under the conditions used. However, the high-temperature polymorph can be quenched under equilibrium conditions when 40 mol% or more MgGa₂O₄ is present. The subsolidus equilibrium relations in the system MgGa₂O₄-LiGa₅O₈ are discussed.     

Magnetoresistance of CuxCo1-xFe2O4 Ferrites

Magnetoresistance measurements (Δ/R) were carried out on Cu _x Co_{1- x} Fe₂O₄ samples with x =1, 0.75, 0.50, 0.25 and cobalt ferrite in the range of magnetic intensity (H) from 1.0 to 4.5 kG. Linear plots were obtained between log (Δ/R) and log H for all compositions except that of cobalt ferrite. The values of n at x =0.5 do not agree with the results of some authors. The discrepancy may be attributed to the value of magnetic field intensity at which such measurements were carried out. The similarity of features of n and μ_D with composition leads us to believe that the magnetoresistance may arise from the scattering of conduction electrons by localized electrons involving the s-d exchange interaction.     

Sintering of Si3N4-Y2O3-Al2O3

Sintering kinetics of the system Si₃N4-Y2O₃-Al₂O3 were determined from measurements of the linear shrinkage of pressed disks sintered isothermally at 1500° to 1700°C. Amorphous and crystalline Si₃N₄ were studied with additions of 4 to 17 wt% Y₂O₃ and 4 wt% A1₂O₃. Sintering occurs by a liquid-phase mechanism in which the kinetics exhibit the three stages predicted by Kingery's model. However, the rates during the second stage of the process are higher for all compositions than predicted by the model. X-ray data show the presence of several transient phases which, with sufficient heating, disappear leaving mixtures of β ' -Si₃N₄ and glass or β '-Si₃N₄, α '-Si₃N₄, and glass. The compositions and amounts of the residual glassy phases are estimated.     

Expansive properties of the mixture C4ASH12 − 2CS III. Effects of temperature and restraint

The effects of temperature and restraint upon the hydration and the expansion of $\text{C}{}_4\text{A}\text{S}\text{H}{}_{12}\text{? 2}\text{C}\text{S}$ mixture compacts in different contact solutions have been investigated. Temperatures above 20°C do apparently hinder the formation of an impervious felt-like layer of ettringite around the $\text{C}{}_4\text{A}\text{S}\text{H}{}_{12}$ particles, thus greatly reducing the retarding effect of the lime. An uniaxial restraint of 1 Kg/cm² is enough to reduce sensibly the expansions which remain however high (about 100%). The results can be satisfactorily interpreted by the reaction and expansion mechanism hypothesized in our previous papers.     

Raman Study of Glasses of Ba2TiSi2O8 and Ba2TiGe2O8

Raman spectra are reported for fresnoite (Ba₂Ti(Si,Ge)₂O₈ glasses, and comparison is made between the Raman spectra of the corresponding crystalline powders and glasses of Ba₂TiSi₂O₈ and Ba₂TiGe₂O₈. The Ba₂TiGe₂O₈ glass spectra show correspondence with the Ba₂TiGe₂O₈ crystalline Raman spectra; the v _s(Ge–O–Ge) mode occurs at 518 cm⁻¹ in the glass and at 521 cm⁻¹ in the crystalline material. Five-fold coordinated titanium is the majority species present in the Ba₂TiGe₂O₈ glass as revealed by a strong band at 824 cm⁻¹ in the I glass spectrum. The Ba₂TiSi₂O₈ glass spectra are similar to the Ba₂TiSi₂O₈ crystalline spectrum; the strongest band is found at 836 cm⁻¹ in the I glass spectrum. Through comparison with the previous Raman data of other titania silicate glasses, we conclude that the Ba₂TiSi₂O₈ glass has a structure similar to the crystalline phase.     

Preparation and properties of poly(Nε,Nε-dicarboxymethyl-l-lysine)

A new ampholytic homopolypeptide, $\text{poly}\text{(N}{}^{\mathrm{\epsilon }}\text{,N}{}^{\mathrm{\epsilon }}\text{-}\text{dicarboxy-methyl-}\text{l}\text{-lysine}\text{)}$, which has one tertiary amino and two carboxyl groups in the side chain has been derived from a hydrochloride salt of poly(L-lysine). The polymer in aqueous solution seems to be in the coil form with locally extended structure (LES) at neutral pH. In both the acidic and alkaline regions, the molar ellipticity of the polymer changes as a result of change in net charge on the side chain. The conformational changes may be from the coil with LES to other coiled forms. 5–7 M NaClO₄ and 80% aqueous methanol induce the α-helix in the polymer at neutral pH. Divalent cations, Cu²⁺ and Ca²⁺, do not induce any remarkably ordered structures such as α-helix or β-structure in the polymer in aqueous solution at any pH. Ultraviolet absorption studies show an absorption peak of the polymer-Cu²⁺ complex near 240 nm. Dependence of the peak intensity on pH at various q values ($\text{q =}\text{[}\text{Cu}{}^{\mathrm{2+}}\text{]}\text{[}\text{residue}\text{]}$) indicates the two steps of the complex formation. At q less than 0.64, the formation is described only with the first step. An average coordination number for Cu²⁺ at the first step was calculated to be about 2 by the method of Mandel and Leyte. The association constant of Cu²⁺ with the residue at the step was determined from the absorption data to be far smaller than that for the Cu²⁺-EDTA complex. The second step of the formation occurs in the case of large q but the absorption data for the second step cannot be obtained exactly due to precipitation.     

Effects of metal-support interactions on the hydrogenation of CO over PdSiO2 and PdLa2O3

A study of CO hydrogenation over $\text{Pd}\text{SiO}{}_2$ and $\text{Pd}\text{La}{}_2\text{O}{}_3$ has been carried out for the purpose of identifying the effects of Pd dispersion, Pd morphology, and support composition on the catalytic activity of supported Pd. The specific activity of each catalyst for methanol and methane synthesis was determined from microreactor studies carried out at a fixed set of reaction conditions. Palladium dispersion was measured by H₂O₂ titration, and the morphology of the Pd crystallites, as expressed by the distribution of Pd(100) and Pd(111) planes, was determined from in situ infrared spectra of adsorbed CO. The crystallite morphology of the $\text{Pd}\text{SiO}{}_2$ catalysts is the same, independent of Pd weight loading: 90% of the surface is comprised of Pd(100) planes and 10% of the surface is comprised of Pd(111) planes. By contrast, the crystallite morphology of the $\text{Pd}\text{La}{}_2\text{O}{}_3$ catalysts changes with Pd loading. Primarily Pd(100) planes are exposed at low-weight loadings while Pd(111) planes are exposed at high-weight loadings. The Pd dispersion has little effect on the methanol turnover frequency over both $\text{Pd}\text{SiO}{}_2$ and $\text{Pd}\text{La}{}_2\text{O}{}_3$, for dispersions between 10 and 20%. On the other hand, the methane turnover frequency is independent of Pd dispersion over $\text{Pd}\text{SiO}{}_2$, but increases with decreasing dispersion over $\text{Pd}\text{La}{}_2\text{O}{}_3$. It is further observed that the Pd morphology influences the specific activity of $\text{Pd}\text{La}{}_2\text{O}{}_3$ for methanol synthesis: Pd(100) is nearly threefold more active than Pd(111). For a fixed morphology, the specific methanol synthesis activity of $\text{Pd}\text{La}{}_2\text{O}{}_3$ is a factor of 7.5 greater than that of $\text{Pd}\text{SiO}{}_2$.     

In situ laser raman spectroscopy of the sulfiding of Moγ-Al2O3 catalysts

Raman spectra of sulfided $\text{Mo}\text{γ-}\text{Al}{}_2\text{O}{}_3$ catalysts were obtained using in situ techniques for two sulfiding methods. For samples sulfided by 10% $\text{H}{}_2\text{S}\text{H}{}_2$ at 400 °C, MoS₂ structures were observed. A stepwise sulfiding using 10% $\text{H}{}_2\text{S}\text{H}{}_2$, with spectra recorded at 150, 250, and 350 °C, resulted in observation of molybdenum oxysulfide, reduced molybdate, and surface “MoS₂” phases. Reexposure of these samples to air led to radical modification of the oxysulfide structures as well as transformation of some sulfide phases. A model incorporating terminal and bridging MoS bonding and anion vacancies is proposed. This model is based on the conversion of isolated and aggregated molybdate and MoO₃ species to oxysulfide and reduced molybdenum phases. Conversion of reduced molybdenum phases to sulfides is observed to be slow.     

Wet Milling of Fe/Al/Al2O3 and Fe2O3/Al/Al2O3 Powder Mixtures

Wet milling of Al₂O₃-aluminide alloy (3A) precursor powders in acetone has been investigated by milling Fe/Al/Al₂O₃ and Fe₂O₃/Al/Al₂O₃ powder mixtures. The influence of the milling process on the physical and chemical properties of the milled powders has been studied. Particle refinement and homogenization were found not to play a dominant role, whereas plastic deformation of the metal particles leads to the formation of dislocations and a highly disarranged polycrystalline structure. Although no chemical reactions among the powder components in Fe₂O₃/Al/Al₂O₃ powder mixtures were observed, the formation of a nanocrystalline, ordered intermetallic FeAl phase in Fe/Al/Al₂O₃ powder mixtures caused by mechanical alloying was detected. Chemical reactions of Fe and Al particle surfaces with the atmosphere and the milling media lead to the formation of highly porous hydroxides on the particle surfaces. Hence the specific surface area of the powders increases, while the powder density decreases during milling. The fraction of Fe oxidized during milling was determined to be 0.13. The fraction of Al oxidized during milling strongly depends on the metal content of the powder mixture. It ranges between 0.4 and 0.8.