双修饰Fe3O4/CdSe/CdS荧光磁性复合物的制备及其表征

采用共沉淀法制得Fe3O4溶胶,用γ-缩水甘油醚氧丙基三甲氧基硅烷(KH-560)对其表面进行改性,制得有机硅改性的纳米Fe3O4磁性粒子;用L-半胱氨酸盐酸盐(L-Cys)将油相的CdSe/CdS转成水相并带上氨基的CdSe/CdS纳米晶;将其复合制备了Fe3O4/CdSe/CdS荧光磁性双功能纳米复合物颗粒。该Fe3O4/CdSe/CdS复合物颗粒平均尺寸约为40nm,饱和磁化强度为21.287A.m2/kg,该纳米粒子既具有优异的荧光特性,也具有较强的超顺磁性。     

磁性Fe3O4纳米颗粒的可控制备及生长研究

采用热法合成磁性Fe3O4纳米颗粒,通过精细调控实验条件能对其形状和大小进行有效控制。采用X射线衍射仪、透射电镜、振动样品磁强计等对Fe3O4纳米颗粒的成分、形貌及磁性等进行了表征测试。结果表明,Fe3O4纳米颗粒的饱和磁化强度为62.5emu/g。最后探讨了Fe3O4纳米颗粒的合成机理。     

Fe_3O_4/Au复合磁性纳米颗粒的制备及其表征

首先通过化学共沉淀法制备出Fe3O4磁性纳米颗粒,考察了表面活性剂的用量、碱的用量、陈化时间以及三价铁与二价铁的摩尔比等因素对Fe3O4纳米颗粒性能的影响。制备出饱和磁化强度为73.85A.m2/kg、粒径大小为10nm以下的Fe3O4纳米颗粒。在此基础上,制备出Fe3O4/Au复合纳米颗粒,通过VSM、TEM、XRD、XPS对产物进行了表征,研究了HAuCl4的用量、还原剂的种类、硅烷偶联剂以及包金之前的Fe3O4纳米颗粒对复合颗粒的影响,结果表明所制得的Fe3O4/Au复合磁性纳米颗粒包覆良好,粒径大小为50～200nm,饱和磁化强度为10.08A.m2/kg。     

化学还原法制备Fe3O4纳米颗粒及其性能研究

采用化学还原法制备得到了Fe3O4纳米颗粒,并用XRD对制备条件:分散剂种类、分散剂用量、煅烧温度、煅烧时间进行了研究。研究结果表明,当选用PEG(6000)做分散剂,PEG用量为50g/L,煅烧温度为700℃,煅烧时间为120min时,制备得到的Fe3O4纳米颗粒已经具有晶型完整的反尖晶石结构。将该样品做VSM分析,分析结果表明样品饱和磁化强度可达85A.m2/kg,并且矫顽力趋近于0,呈现出良好的顺磁性。     

酸碱度对纳米Fe_3O_4磁性流体性能的影响

采用化学共沉淀法制备纳米Fe3O4磁性颗粒,并用油酸钠对其进行包覆改性,以煤油为基液制备出煤油基Fe3O4磁流体。对比分析了pH值=5和10.5条件下油酸钠包覆的Fe3O4磁性颗粒的性能差异,得出油酸钠在pH值=5时可以更好地包覆在Fe3O4磁性颗粒表面,其饱和磁化强度为58.0A·m2/kg,在此基础上制备出的磁流体的饱和磁化强度为20.2A·m2/kg,并且Fe3O4磁性颗粒分散较均匀。而油酸钠在pH值=10.5时包覆的Fe3O4磁性颗粒,其饱和磁化强度虽然高一些(67.8A·m2/kg),但制备出的磁流体稳定性较差,出现较为明显的沉降现象。     

聚乙二醇法在温和条件下制备不同结构的磁性Fe3O4纳米晶

以Fe（acac）3为原料,乙二醇、聚乙二醇1000和聚乙二醇5000为还原剂和溶剂,在温和的溶剂热的条件下制备了不同尺寸的顺磁性Fe3O4纳米颗粒.利用X射线衍射（XRD）、光电子能谱（XPS）、透射电子显微镜（TEM）和磁性测量技术对制备的Fe3O4纳米颗粒的结构、形貌、磁性能进行了表征测试.结果发现,聚乙二醇分子链的长度对Fe3O4纳米颗粒的平均粒径大小、结晶度和饱和磁化强度均有重要影响.以乙二醇、聚乙二醇1000和聚乙二醇5000为还原剂制备的Fe3O4纳米颗粒的尺寸分别为2～3nm、5nm和7～8nm;相应的纳米Fe3O4颗粒饱和磁化强度分别为55.2、61.5和81.3emu/g;同时结晶度也随分子链的增加而增加.随分子链长度的增加,还原剂还原性的逐渐增加是导致Fe3O4纳米颗粒平均粒径大小、结晶度和饱和磁化强度逐渐增大的重要因素.     

Fe3O4/CdTe磁性荧光纳米复合物的逐步杂凝聚法合成及其表征

采用逐步杂凝聚法合成了Fe3O4/CdTe磁性荧光纳米复合物.以化学共沉淀法制备Fe3O4纳米颗粒,经油酸修饰后分散在表面活性剂中形成磁流体.CdTe量子点以巯基乙酸为稳定剂制得.最后以聚乙烯亚胺(PEI)为联接剂,成功制备了Fe3 O4 /CdTe磁性荧光双功能纳米复合物颗粒.该复合物颗粒平均尺寸为(30±5)nm,荧光产率为0.186,饱和磁化强度为15.745emu/g,该纳米粒子既具有优异的荧光特性,也具有较强的超顺磁性.     

3-氨丙基三乙氧基硅烷表面修饰的磁性Fe3O4纳米粒子合成与表征

以FeCl3、FeSO4为铁源,利用改进共沉淀法合成磁性纳米Fe3O4,在其制备的过程中加入水合肼充当还原剂和沉淀剂,采用3-氨丙基三乙氧基硅烷(APTES),通过硅烷化反应以化学键的方式结合Fe3O4纳米颗粒,获得表面氨基化的磁性Fe3O4纳米复合颗粒。并用XRD、IR、TEM、VSM等分析手段深入研究了APTES修饰前后磁性纳米颗粒结构和性能影响。结果表明APTES成功包覆到磁性纳米粒子表面,其包覆率为21%;磁性颗粒粒径为20nm,晶型为反立方尖晶石型;磁性颗粒具有很好的分散性,其磁化率为2.36×10-6,饱和磁化强度达60.8mT。     

羧甲基-β-环糊精修饰Fe3O4磁性纳米颗粒的制备与性能研究

在水介质中以羧基取代度为1.2的羧甲基-β-环糊精对Fe3O4磁性纳米颗粒直接进行包覆修饰制备了羧甲基-β-环糊精修饰Fe3O4磁性纳米颗粒,对制备颗粒的形态、结构和成分进行了表征并对其相关性能进行了研究。结果表明,制备的羧甲基-β-环糊精修饰Fe3O4磁性纳米颗粒为近球形,粒径在15~20nm之间,修饰上的羧甲基-β-环糊精约占颗粒总重的8.2%,颗粒为超顺磁性,质量比饱和磁化强度为68.7emu/g,在水中分散良好,载药的羧甲基-β-环糊精修饰Fe3O4磁性纳米颗粒在4h内具有较强的药物突释效应,随后呈现长达26h以上的药物缓释状态。     

水热法制备CoFe2O4纳米颗粒及其穆斯堡尔谱与磁性能研究

用水热法在不同温度下制备结晶性较好、颗粒均一的CoFe2O4纳米颗粒,无需进一步煅烧。利用X射线衍射仪(XRD)、场发射扫描电镜(SEM)、穆斯堡尔谱仪和综合物性测量系统(PPMS)对不同温度下合成的样品进行表征。结果表明,随着合成温度的升高,CoFe2O4纳米颗粒的结晶性增强,粒径逐渐增大,样品的饱和磁化强度逐渐增强。当合成温度为500℃时,CoFe2O4纳米颗粒的饱和磁化强度达到64.1A.m2/kg,与块体的CoFe2O4(72A.m2/kg)接近。穆斯堡尔谱分析表明,当晶粒粒径超过了超顺磁性的临界尺寸,样品的超顺磁性消失,随着合成温度的升高,B位上Fe3+离子的比例增高,磁性能增强。     

Recovery of ammonium alum from waste solutions with a varying ratio of NH4 to Al in groundwater remediation after underground uranium leaching

Experiments with cooling crystallization of ammonium alum, (NH(4)Al(SO(4))2.12H(2)O), were performed with concentrated multicomponent acidic solutions (originating from underground uranium leaching in Stráz pod Ralskem area, Czech Republic, and containing as the principal components Al3+, NH4+, and SO4(2-) ions) as well as with similar solutions prepared in the laboratory. The yield of NH(4)Al(SO(4))2.12H(2)O crystals increased significantly with the increasing NH4+/Al3+ molar ratio, in accordance with pertinent solubility data. The purifying effect of crystallization was quantified by means of the distribution coefficients, characterizing the uptake of ionic impurities to alum crystals; the tendency of cationic impurities to crystallize with NH(4)Al(SO(4))2.12H(2)O decreased in the following order: K+ > Cr3+ >Na+ approximately Fe3+ >Mg2+ approximately Zn2+ >Fe2+. Additionally, gypsum (CaSO4.2H(2)O) solubilities at 25 degrees C, in mother liquors after NH(4)Al(SO(4))2.12H(2)O crystallization, were determined.     

Fe2+、Fe3+对CaO-Al2O3-SiO2-MgO系微晶玻璃析晶性能的影响规律

为了利用大量的含铁铝硅酸盐固体废弃物制备具有高附加值的微晶玻璃,采用DTA、XRD、SEM、EDS等手段研究了Fe2+、Fe3+对CASM系微晶玻璃析晶性能的影响.结果表明,Fe2+在微晶玻璃中与Mg2+的作用相同,取代以网络外体形式存在的Al3+,使得微晶玻璃的析晶温度逐渐下降,而对析晶能力几乎没有影响,并当Fe2+掺入量为2%时,主晶相由铝黄长石转变为镁黄长石,在7.5%时,进一步转变为透辉石.Fe3+掺量小于7.5%时,起到补充Si4+不足的作用,当大于7.5%时,部分Fe3+起到与Fe2+、Mg2+相同的作用,使得析晶温度呈先升后降的变化,在掺量为7.5%时,铝黄长石主晶相才开始转变为镁黄长石,在10%时,转变为透辉石,且析晶能力得到大幅提升.随着Fe2+和Fe3+含量增加,虽然微晶玻璃中主晶相的变化顺序相同,但Fe2+具有降低微晶玻璃析晶温度的作用,而一定量的Fe3+可作为晶核剂提高微晶玻璃的析晶能力.     

磁性La3+掺杂TiO2的制备及性能

利用溶胶-凝胶法,在室温条件下,以钛酸四丁酯、硝酸镧为主要原料,无水乙醇为溶剂,冰醋酸为抑制剂,浓硝酸为催化剂制得稳定的掺La3+TiO2溶胶,陈化后的凝胶经不同温度煅烧3h后制得不同掺La3+量的TiO2。通过XRD对不同煅烧温度及不同掺La3+量的TiO2进行了表征;以紫外光为光源,研究了掺La3+-TiO2对甲基橙溶液的光降解效果。用化学共沉淀法制备了具有强磁性的Fe3O4水基磁流体,再与La3+掺杂TiO2进行复合,制备了Fe3O4负载量不同的磁性La3+掺杂TiO2,研究了Fe3O4负载量不同的La3+掺杂TiO2对甲基橙的光催化降解效果、磁分离回收率的影响。结果表明,掺La3+量及煅烧温度对TiO2的晶型、各晶型TiO2的相对含量及对甲基橙的光降解效果均有影响。La3+掺杂TiO2比纯TiO2显示出更强的光催化性能,掺La3+量2%,热处理温度450℃的La3+掺杂TiO2光催化活性最高。Fe3O4负载量为10%的Fe3O4/La3+-TiO2对甲基橙的降解率8h时为99.4%;磁分离回收率达97.39%。     

Quenchability and Magnetic Properties of Nd_4Fe_(82)B_(14)

The glass forming ability (GFA), crystallization behaviour and magnetic properties of Nd4Fe82B14 produced by melt spinning were investigated. The experimental results show that the GFA is rather Strong; the crystals precipitation sequence is as follows: Am(amorphous)→Am'+bcc-Fe →Nd2Fe23B3+Fe23B6+bcc-Fe→Fe23B6+Fe3B+Nd2Fe14B+bcc-Fe→Fe3B+Nd2Fe14B+bcc-Fe. The magnetic properties after crystallization are not affected by the cooling rate and the best magnetic properties are Br=0.8436 T, Hcj=266.4 kA/m, (BH)max=48.08 kJ/m3.     

耐磨复合磷化膜的研制

按磷化的成膜机理，设计了复合磷化液配方，进行了多种实验，研究了多种金属离子如K^ ,NH4^ ,Na^ ,Fe^2 ,Mn^2 ,Zn^2 ,Ca^2 ,Sb^2 ,Cu^2 ,Ni^2 的含量，温度，酸比等工艺参数对磷化成膜的影响，结果表明，复合磷化克服了常规磷化的不足，磷化膜耐磨性能好，复合磷化膜具有好的热稳定性及耐磨抗磨性能。     

Fe3O4核壳磁性絮凝剂的制备及其应用

原油炼化过程中产生的大量采出水污染严重,亟待处理。为此,利用多巴胺对自制的纳米Fe3O4进行改性,然后再与丙烯酰胺单体混合,通过添加适量的过硫酸铵(NH4)S2O8作为引发剂,在适宜的条件下引发聚合反应,制备出聚丙烯酰胺包裹的四氧化三铁复合絮凝剂[PAM@(PDA-Fe3O4)];核壳絮凝剂的最佳制备条件为Fe3O4改性温度60℃,m(DA): m(Fe3O4)= 1:5,聚合过程中,m(Fe3O4): m(AM)为1:5,引发剂过硫酸鮫用量为AM质量的0.5%,反应时间4h。利用最佳条件下制得的核壳絮凝剂对采出水进行絮凝处理,结果显示:在pH值为9,投加量为0.2g/L时,对采出水的浊度去除率达到79.6%;在外加磁场的辅助下,絮体在43s时基本完全沉降,取得了比常规阳离子聚丙烯酰胺和聚合氯化铝单独使用时更好的处理效果。     

Synthesis of size-controlled Fe3O4@SiO2 magnetic nanoparticles for nucleic acid analysis

We present a systematic study on the preparation, characteration and potential application of Fe3O4 and Fe3O4@SiO2 nanoparticles. Fe3O4 nanoparticles of controllable diameters were successfully synthesized by solvothermal system with tuning pH. The magnetic properties of nanoparticles were measured by vibration sample magnetometer. Fe3O4@ SiO2 nanoparticles were obtained via classic St?ber process. Streptavidin coated Fe3O4@SiO2 nanoparticles were prepared by covalent interaction. The quantity of streptavidin bound to nanoparticles was determined by UV-Vis spectrometer. To evaluate the binding efficiency and capacity of nucleic acid on nanoparticles, the capture of biotinylated oligonucleotide on streptavidin coated Fe3O4@SiO2 nanoparticles at different concentration was estimated by fluorescence detection. Both Fe3O4 and Fe3O4@SiO2 nanoparticles exhibited well crystallization and magnetic properties. The maximal amount of streptavidin immobilized onto the Fe3O4@SiO2 nanoparticles was 29.3 microg/mg. The saturation ratio of biotinylated oligonucleotides captured on streptavidin coated Fe3O4@SiO2 nanoparticles was 5 microM/mg within 20 minutes, indicating that FeO4@SiO2 nanoparticles immobilized by streptavidin were excellent carriers in nucleic acid analysis due to their convenient magnetic-separation property. Therefore, the synthesized Fe3O4 and Fe3O4@SiO2 nanoparticles with controllable size and high magnetic saturation have shown great application potentials in nucleic acid research.     

低应力氨基磺酸镀镍在航空维修中的应用

低应力氨基磺酸镀镍尽管在航空零部件制造、维修中应用广泛,但仍需对其存在的应力、氢脆等问题给予足够的关注和严格的工艺控制。为此,采用螺旋收缩测量法定量研究了氨基磺酸盐镀镍层内应力的影响因素,并用静态拉伸法测试了镀镍工艺对高强度钢氢脆性能的影响。结果表明:氨基磺酸镍及硼酸含量对镀层内应力影响较小;使用氨基磺酸或碳酸镍调整溶液p H值都会提高镀层内应力,但不会造成基体发生氢脆,实际生产中应谨慎使用;溶液中的Cl^-、Fe²⁺、Cu²⁺、Cr⁶⁺浓度的增加都会不同程度提高电镀镍层的内应力,尤其Cr6+对镀层外观、内应力、氢脆性能等都会产生很大影响,生产中应注意控制;结合工艺标准的要求及试验数据,给出了推荐的镀镍工艺配方:H3BO340～50 g/L(达到饱和状态),Ni(NH2SO3)2·4H2O 325～345 g/L,Ni2+76.0～80.7 g/L,Cl-3～10 g/L,pH值3～4,湿润剂0.2 m L/L,温度50～55℃,电流密度5.4 A/dm2,Fe²⁺<100 mg/L,Cu²⁺<50 mg/L,Cr⁶⁺<2.5 mg/L。     

Seed-mediated synthesis of iron oxide and gold/iron oxide nanoparticles

In this study, we prepared magnetic iron oxide and gold/iron oxide nanoparticles (NPs) and characterized their morphologies and properties by XRD, TEM, EDX, VSM and UV-vis measurements. The magnetite iron oxide NPs of 10 nm were synthesized by coprecipitation of Fe2+ and Fe+3 in the solution of NH4OH and then they were used as seed particles for the subsequent growth to prepare the magnetite NPs of different particle sizes and also to prepare gold/iron oxide composite NPs. All those magnetite NPs are superparamagnetic and the gold/iron oxide composite NPs combine the optical and magnetic properties, which are contributed by gold and iron oxide components, respectively.     

Green synthesis of uniform magnetite (Fe3O4) nanoparticles and micron cubes

Single-crystalline Fe3O4 microcubes were obtained through a green hydrothermal procedure using Fe3+, Fe2+ and H2O2 as starting materials. The structures and morphologies of the as-prepared samples were characterized in detail by X-ray diffraction (XRD), Transmission electron microscopy (TEM) and scanning electron microscopy (SEM) respectively. Magnetite (Fe3O4) cubes averaging 3 microm in diameter were synthesized by H2O2 oxidation of Fe3+ and Fe2+ under neutral conditions. The contrastive experiments were designed to elucidate the effects of Fe3+, Fe2+ and H2O2 on the morphology of the final products. Irregular and ellipsoidal Fe2O3 structures were obtained by H2O2 oxidation of Fe3+ and Fe2+ respectively. Meanwhile, Fe3O4 nanotubes and nanoparticles were obtained when H2O2 was replaced by NH4HCO3 and urea respectively. The results show that H2O2, Fe3+ and Fe2+ in the reactive system play critical roles in obtaining micrometric cube-like Fe3O4. While, other nanometric Fe2O3 and Fe3O4 particles with tube-like and other morphologies could also be developed by controlling the reaction parameters.