铁磁性Cr3+掺杂纤蛇纹石纳米管的制备与表征

研究了在水热条件下,通过离子替代的方法制备Cr3+掺杂纤蛇纹石纳米管.采用X射线衍射、扫描电子显微镜、高分辨透射电子显微镜、红外光谱和磁性测试等手段对样品进行了表征.结果表明,掺杂Cr3+后的纤蛇纹石样品其晶胞参数6值增大,内外径分别为6～8nm和30～40nm,长度为50～300nm;掺杂样品中,Cr3+部分替代了Mg2+进入纤蛇纹石的八面体结构单元层中,使得其具有室温铁磁性和磁滞回线特性.     

钴铁氧体纳米管阵列制备及其磁学性能(英文)

为了研究一维钴铁氧体纳米管阵列的磁学性质,应用氧化铝模板具有的约束作用和毛细管作用,结合溶胶凝胶技术合成了钴铁氧体纳米管阵列.在140℃条件下,通过包含Fe(AO)3和Co(AO)2(物质的量之比为2∶1)的柠檬酸和乙二醇混合溶液(物质的量之比为1∶4)酯化反应得到溶胶.将氧化铝模板浸入溶胶几次后取出,取出充满溶胶的氧化铝模板,在大气气氛中,以0.6℃/min～5℃/min的升温速度将样品由室温升温至500℃,保温8 h.结果表明,在控制Fe3+离子浓度的条件下也可以合成钴铁氧体纳米线(Fe3+离子浓度大于1 mol/L)和"竹节"型纳米管(Fe3+离子浓度介于0.5 mol/L～1.0 mol/L),但重点进行了其纳米管阵列(Fe3+离子浓度小于0.5 mol/L)合成和磁学性能测试.透射电子显微镜(TEM)、高分辨电镜(HRTEM)的观察以及粉末X光衍射(XRD)测试结果表明纳米管组成为多晶结构.纳米管的直径取决于氧化铝模板的孔径,大约为200 nm,其长度约几个微米.应用样品振动磁强计对样品磁性进行了表征,结果表明纳米管阵列未表现出方向特性,矫顽力随着升温速率的降低而升高,在0.6℃/min的升温速率时,矫顽力达到最高的1 445 kOe,简单讨论了其形成原因.     

阴离子对掺杂Co2+纳米Ni（OH）2性能的影响

为了考察阴离子种类对掺杂Co2+纳米Ni(OH)2性能的影响,采用不同镍盐制备出掺杂Co2+纳米Ni(OH)2,并采用X射线衍射(XRD)、透射电子显微镜(TEM)、循环伏安技术(CV)和恒流充放电方法对材料物化性能和电化学性能进行了研究.研究结果表明,掺杂Co2+的纳米Ni(OH)2为β-Ni(OH)2,衍射峰发生明显宽化.样品颗粒的尺寸为60~100 nm,阴离子的变化对制得的Ni(OH)2的表观形貌有影响.恒流充放电实验表明,阴离子为NO3-时,样品的质量比容量较高,0.2 C放电达到了234.6 mAh.g-1.循环伏安测试表明,阴离子为SO42-时,样品有较好的可逆性,阴离子为NO3-或SO42-时有较高的质子扩散系数.     

氮镍共掺杂TiO2纳米管的制备及其光催化性能

为了制备在高温焙烧后能保持良好管形结构的可见光响应的TiO2纳米管,通过NH4Cl水-溶剂热和Ni(NO3)2浸渍法对传统水热法合成的TiO2纳米管进行掺氮和掺镍改性。通过X射线衍射(XRD)、扫描电子显微镜(SEM)、X射线光电子能谱(XPS)、紫外-可见漫反射(UV-vis DRS)和荧光光谱(PL)等方法对样品进行了表征,并以甲基橙(MO)为光催化降解模型,考察了可见光下制备的样品的光催化性能。结果表明,NH4Cl水-溶剂热掺氮处理可提高TiO2纳米管的管状结构的热稳定性;氮镍共掺杂元素之间的协同作用增强了催化剂对可见光的吸收能力,并且能有效地抑制光生电子空穴的复合,Ni/Ti添加量为0.3%的催化剂具有较高的光催化活性。可见光照射210min,氮镍共掺杂TiO2纳米管对MO的可见光降解率比单独氮和镍掺杂的TiO2分别提高了9.1%和21.2%。     

离子种类对金属掺杂纳米管TiO_2光催化活性的影响

使用市售Degussa P-25TiO2粉末,采用水热合成法制备了1.0%(原子分数)Ag+、Cu2+、Fe3+、Mn2+和V5+掺杂纳米管TiO2催化剂。结果表明,随着煅烧温度增高,样品的比表面积逐渐降低,锐钛矿含量先增后减,禁带宽度逐渐变窄,变化范围与掺杂金属的种类有关。掺杂金属后,纳米管TiO2催化剂的比表面积略有降低,锐钛矿含量略有增大,禁带宽度变窄。向纳米管TiO2中掺杂Ag+、Cu2+、Fe3+和V5+,催化剂的光催化活性提高,而掺杂Mn2+,光催化活性略有降低。550℃煅烧1.0%Fe3+掺杂纳米管TiO2具有最好的催化效果,其254nm光催化臭氧氧化对腐植酸的去除率为77.4%。     

尖晶石结构Ni掺杂ZnFe2O4纳米颗粒的性能表征

利用水热法成功合成了纯ZnFe2O4和不同含量Ni掺杂Zn1-xNixFe2O4纳米颗粒。采用X射线衍射(XRD)、高分辨透射电子显微镜(HRTEM)、选区电子衍射(SAED)、X射线能量色散分析(XEDS)、紫外可见吸收光谱(UV-Vis)、傅里叶变换红外光谱(FT-IR)和振动样品磁强计(VSM)等测试技术研究掺杂浓度对Zn1-xNixFe2O4(x=0,0.1,0.3,0.5)样品的晶体结构、形貌、光学性能和磁学性能的影响。结果表明:所制备的Zn1-xNixFe2O4纳米颗粒结晶良好,Ni2+以替代Zn2+的形式掺杂到ZnFe2O4晶格中,生成立方尖晶石结构ZnFe2O4。随着Ni含量的增加,晶粒尺寸增大,晶格常数发生收缩。样品的形貌呈不规则的椭球形,且颗粒大小比较均匀。红外光谱的吸收峰位置并没有随Ni掺杂浓度的增加而变化。Zn1-xNixFe2O4纳米晶的光学带隙随Ni掺杂浓度增加而增大,与相应块体相比发生蓝移。在室温下,纯ZnFe2O4纳米晶呈现超顺磁性,掺杂样品具有明显的铁磁性。     

共沉淀法合成NaLa(MoO_4)_2∶Eu~(3+)红色荧光粉及其发光性能的研究

采用共沉淀法合成了微米花状,四方晶系的NaLa(MoO4)2∶Eu3+红色荧光粉。利用X射线衍射仪、扫描电子显微镜、光致发光光谱等分析手段对样品的结构、形貌以及发光性能进行了表征。研究了结构控制剂种类、聚乙烯吡咯烷酮(PVP)添加量、Eu3+掺杂浓度、反应物浓度等系列对合成NaLa(MoO4)2∶Eu3+发光材料发光性能的影响。结果表明:所合成的微米花状NaLa(MoO4)2∶Eu3+红色荧光粉为四方晶系,在464nm紫外激发下,观察到其发射主峰位置在615nm。当反应条件分别为PVP=0.75g、Eu3+掺杂浓度10%、反应物浓度为0.12mol/L时样品具有最强的发光强度。在紫外灯照射下,样品呈现出明亮的红色。     

NiFe2O4纳米粒子的水热合成及表征

以Ni(NO3)2·6H2O和Fe(NO3)3·9H2O为主要原料,在聚乙二醇(PEG)存在下,采用水热法制备了磁性NiFe2O4纳米粒子,用X射线衍射仪(XRD)、透射电子显微镜(TEM)和振动样品磁场计(VSM)等分析方法对样品进行了表征.结果表明:水热法合成的NiFe2O4纳米粒子为尖晶石结构,粒度分布均匀,为方形形貌,粒子直径范围在50～60nm;比饱和磁化强度为25.83emu/g,剩磁为6.167emu/g,矫顽力达85.87Oe.     

过渡金属(Mn2+、Ni2+、Fe3+、Cu2+)掺杂ZnO基稀磁半导体的制备及性质

利用溶液腐蚀法制备了Mn2+、Ni2+、Fe3+、Cu2+离子掺杂的ZnO基稀磁半导体。XRD表明掺杂后的ZnO仍然保持单一的纤锌矿结构,没有任何杂质相产生。由紫外-可见光反射谱可知掺杂后吸收边发生了红移。掺杂前ZnO的带隙为3.20eV,对样品分别掺入Mn、Ni、Fe和Cu后的带隙分别为3.19eV、3.15eV、3.08eV和3.17eV。掺杂后样品的室温PL谱除了紫外发射峰外,对于Mn掺杂的样品还在蓝光区域出现了2个分别位于424nm和443nm的发射峰,Fe掺杂的样品出现了一个位于468nm的微弱发射峰,Cu掺杂的样品出现了位于469nm及535nm的很宽的发射峰。室温磁滞回线显示掺杂后样品有明显的铁磁性,掺入Mn、Ni、Fe和Cu样品的剩余磁化强度(Ms)分别为0.3902×10-3emu/cm3、0.454emu/cm3、0.372emu/cm3和0.962×10-3emu/cm3,矫顽力分别为47Oe、115.92Oe、99.33Oe和23Oe。经分析室温铁磁性来源于缺陷调制的Mn2+-Mn2+长程铁磁交换相互作用。     

溶胶-凝胶水热法合成纤蛇纹石纳米管

采用四甲氧基硅和氯化镁为前躯体,通过溶胶-凝胶和高温水热法合成了内径5nm~10nm,外径约15nm~35nm,长度400nm~2μm的纤蛇纹石纳米管,利用X射线衍射仪(XRD)、扫描电子显微镜(FSEM)和高分辨透射电子显微镜(HRTEM)对合成样品的物相、形貌和结构进行了表征;初步试验表明,纤蛇纹石纳米管的形成过程是氢氧化镁优先在一维方向上生长成针状或纤维状结构,在溶液中形成结构导向模板后与非晶态的二氧化硅反应形成纳米管状结构;通过控制化学计量比在一定范围内可以实现纳米管的内外径尺寸的调控。     

镍纳米管阵列的电沉积合成及其磁学性能表征

以氧化铝膜为模板、金属汞为电阴极,采用简单的直流电沉积方法制备出高度有序的镍纳米管阵列。利用扫描电子显微镜、透射电子显微镜、选区电子衍射、能谱仪、X射线粉末衍射和样品振动磁强计对样品进行形貌表征、成分及磁性能分析。结果表明,阵列中的镍纳米管彼此平行,尺寸均匀,纳米管外径为260～360nm;镍纳米管阵列表现出良好的磁各向异性,其易磁化方向垂直于镍纳米管阵列。以金属汞为电阴极是易形成纳米管的关键条件。     

A novel fabrication method of magnetic Co/Ni0.4Zn0.6Fe2O4 coaxial nanocables

A highly ordered Co/Ni0.4Zn0.6Fe2O4 coaxial nanocable array has been synthesized based on porous anodized aluminum oxide template via a new approach, which combines an improved sol-gel template method and alternating current electrochemical deposition. Scanning electron microscopy and transmission electron microscopy images show the nanocables are uniform with outer diameter of about 50 nm and inner diameter of about 17 nm. X-ray diffraction patterns and energy dispersive spectrometer confirm that Co nanowires are successfully deposited into the pores of the Ni0.4Zn0.6Fe2O4 nanotubes. Normalized magnetic hysteresis loops demonstrate the coercive force and the squareness with the applied field parallel to the axis of the nanocables increase dramatically compared with that of the nanotubes.     

纳米镍颗粒填充碳纳米管的制备与磁性能

采用自制的实验装置, 通过阳极弧放电等离子体技术成功制备了Ni纳米颗粒填充的碳纳米管, 利用高分辨透射电子显微镜(HRTEM)、 XRD、 TEM、 X射线能量色散分析谱仪(XEDS)和振动样品磁强计(VSM)等测试手段对样品的化学成分、 形态、 微观结构和磁性能进行了表征。实验结果表明, 采用本文中实验方法能获得大量被纳米金属颗粒填充的碳纳米管, 其内部填充物为面心立方(FCC)结构的纳米Ni颗粒, 外围薄层为石墨碳层。碳纳米管的外径为30~40 nm, 壁厚5~8 nm, 内部填充的纳米颗粒呈球形和椭球形, 粒径均匀, 在管腔内不连续分布。产物具有顺磁特性, 矫顽力是78 Oe, 饱和磁化强度是33 enu/g。     

Synthesis and photoluminescence of Y2O3:RE3+ (RE=Eu, Tb, Dy) porous nanotubes templated by carbon nanotubes

Y2O3:RE3+(RE=Eu, Tb, Dy) porous nanotubes were first synthesized using carbon nanotubes as template. The morphology of the coated precursors and porous Y2O3:Eu3+ nanotubes was determined by scanning electron Microscopy (SEM) and transmission electron microscopy (TEM). It was found that the coating of precursors on carbon nanotubes (CNTs) is continuous and the thickness is about 15 nm, after calcinated, the Y2O3:Eu3+ nanotubes are porous with the diameter size in the range of 50-80 nm and the length in micrometer scale. X-ray diffraction (XRD) patterns confirmed that the samples are cubic phase Y2O3 and the photoluminescence studies showed that the porous rare earth ions doped nanotubes possess characteristic emission of Eu3+, Tb3+, and Dy3+. This method may also provide a novel approach to produce other inorganic porous nanotubes used in catalyst and sensors.     

Large scale synthesis and characterization of Ni nanoparticles by solution reduction method

Ni nanoparticles were mass synthesized by solution reduction process successfully. The influence of the parameters on the particle size of Ni nanoparticles were studied and the referential process parameters were obtained. The morphology and structure of the synthesized Ni nanoparticles were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), Brunauer-Emmett-Teller (BET) surface area analysis and infrared spectroscopy (IR). The results show that Ni nanoparticles are of high purity and are covered by hydroxyethyl carboxymethyl cellulose (HECMC) layer and the mean size being about 31 nm. The magnetic measurement revealed that Ni nanoparticles are ferromagnetic.     

Size-controlled synthesis, microstructure and magnetic properties of Ni nanoparticles

Ni nanoparticles with different mean diameters of 15-83 nm were synthesized by solution reduction process. The size of Ni nanoparticles can be controlled by varying the concentration of NiCl₂·6H₂O and synthesis temperature. The samples were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), infrared spectroscopy (IR) and X-ray photoelectron spectroscopy (XPS). Results show that the synthesized particles are single-phased Ni with a face-centered cubic crystal structure. Magnetic measurements indicate that Ni nanoparticles are ferromagnetic. The lattice constants and coercivities of the samples are size-dependent.     

Effect of Ni+2-substituted Fe2TiO5 on the H2-reduction and CO2 Catalytic Decomposition Reactions at 500℃

CO2 is a major component of the greenhouse gases, which causes the global warming. To reduce CO2 gas, high activity nanosized Ni＋2 substituted Fe2TiO5 samples were synthesized by conventional ceramic method. The effect of the composition of the synthesized ferrite on the H2-reduction and CO2-catalytic decomposition was investigated. Fe2TiO5 （iron titanate） phase that has a nanocrystallite size of -80 nm is formed as a result of heating Fe2O3 and TiO2 while the addition of NiO leads to the formation of new phases （-80 nm） NiTiO3 and NiFe2O4, but the mixed solid of NiO and Fe2O3 results in the formation of NiFe2O4 only. Samples with Ni^＋2=0 shows the lowest reduction extent （20%）; as the extent of Ni＋2 increases, the extent of reduction increases. The increase in the reduction percent is attributed to the presence of NiTiO3 and NiFe2O4 phases, which are more reducible phases than Fe2TiO5. The CO2 decomposition reactions were monitored by thermogravimetric analysis （TGA） experiments. The oxidation of the H2-reduced Ni＋2 substituted Fe2TiO5 at 500℃ was investigated. As Ni^＋2 increases, the rate of reoxidation increases. Samples with the highest reduction extents gave the highest reoxidation extent, which is attributed to the highly porous nature and deficiency in oxygen due to the presence of metallic Fe, Ni and/or FeNi alloy. X-ray diffraction （XRD） and transmission electron microscopy （TEM） of oxidized samples show also the presence of carbon in the sample containing Ni＋2〉0, which appears in the form of nanotubes （25 nm）.     

Synthesis, Characterization and Electromagnetic Studies on Nanocrystalline Nickel Zinc Ferrite by Polyacrylamide Gel

Nanocrystalline nickel zinc ferrite powders （Ni=Zn1-xFe2O4, A for x=0, B for x=0.2, C for x=0.5, D for x= 0.8 and E for x= 1） were synthesized by polyacrylamide gel method. X-ray diffraction （XRD）, transmission electron microscopy （TEM） and wave-guide were used to characterize the composition. The XRD results show that the dried gel powders are amorphous, and the characteristic peaks of the spinel Ni0.5Zn0.5Fe2O4 appear after the gel is calcined at 400℃ for 1 h. When the calcining temperatures are 600 and 800℃, the average grain sizes are identified by TEM to be 10 and 30 nm, respectively. The NixZn1-xFe2O4 powders have both dielectric loss and magnetic loss in the frequency range of 8.2-11.0GHz. With the increase of Ni^2＋ ions content, the dielectric parameters （ε′） and permeability （u′） of the NixZn1-xFe2O4 powders decrease while the dielectric loss （ε″）, magnetic loss （u″） and the reflection loss increase.     

Ni_(0.5)Zn_(0.5)Fe_2O_4铁氧体的制备及其电磁损耗性能

以Zn(NO3)2.6H2O、Ni(NO3)2.6H2O和Fe(NO3)3.9H2O及柠檬酸为原料,采用溶胶-凝胶法制备前驱体,在1 200℃下煅烧3 h合成ZnFe2O4和Ni0.5Zn0.5Fe2O4铁氧体粉体。利用差热分析、X射线衍射、扫描电镜、透射电镜和红外光谱等测试手段对产物进行分析和表征。结果表明:ZnFe2O4和Ni0.5Zn0.5Fe2O4属于立方晶系尖晶石结构,结晶完整,晶粒大小在100 nm左右。在0.2~1.8 GHz的频率下对产品进行了电磁损耗性能测试,发现Ni0.5Zn0.5Fe2O4具有较好的电磁损耗特性。