纳米微晶纤维素表面改性研究

分别对纳米微晶纤维素(NCC)的表面进行醋酸酯化、羟乙基化和羟丙基化改性,利用FT-IR、TEM、13C-NMR、TGA对改性产物进行表征,研究不同的表面改性方法对纳米微晶纤维素性能的影响.结果表明,利用这几种方法改性后的NCC,经干燥后都可以重新分散在适当的溶剂中,且颗粒粒径没有明显变化,但不同改性产物的热性能有所差异.     

Structural and magnetic properties of Co50Ni50 powder mixtures

In the present work, morphological, structural, thermal and magnetic properties of nanocrystalline Co₅₀Ni₅₀ alloy prepared by high energy planetary ball milling have been studied by means of scanning electron microscopy, X-ray diffraction, and differential scanning calorimetry. The coercivity and the saturation magnetization of alloyed powders were measured at room temperature by a vibration sample magnetization. Morphological observations indicated a narrow distribution in the particle and homogeneous shape form with mean average particle size around 130 μm². The results show that an allotropic Co transformation hcp→fcc occurs within the three first hours of milling and contrary to what expected, the Rietveld refinement method reveals the formation of two fcc solid solutions (SS): fcc Co(Ni) and Ni(Co) beside a small amount of the undissolved Co hcp. Thermal measurement, as a function of milling time was carried out to confirm the existence of the hcp phase and to estimate its amount. Magnetic measurement indicated that the 48 h milled powders with a steady state particles size have the highest saturation (105.3 emu/g) and the lowest coercivity (34.5 Oe).     

Quantum-chemical ab initio study of the crystal-field and charge transfer energies of nanocrystalline Y2O3: Eu

The 4f energy levels and crystal-field parameters for several clusters representing the local coordination surroundings of Eu³⁺ in the bulk and nanocrystalline cubic Y₂O₃: Eu³⁺ crystals are obtained by using a method based on the combination of the DV-X_α calculation and the effective Hamiltonian method initialized by M.F. Reid et al. (J. Phys.: Condens. Matter, 2011, 23: 045501). The results are in reasonable agreement with the measured energy levels and the crystal-field parameters obtained from the least-square fitting. The charge transfer energies are also obtained for all the clusters from the DV-X_α calculation. The results indicate that, compared with the bulk Y₂O₃: Eu³⁺ crystal, the charge transfer band in the excitation spectra is red-shifted in the nanocrystal.     

Effect of substitution of Co ions on the structural and electrical properties of nanosized magnesium aluminate

Cobalt substituted nanosized magnesium aluminates having a nominal composition MgAl_2−xCo_xO₄ where x = 0.0, 0.5, 1.0, 1.5, 2.0 were synthesized by the chemical co-precipitation method. Aluminium (Al³⁺) ions were completely and successfully substituted by Co²⁺ ions, which yielded an electron rich terminal compound MgCo₂O₄. All the samples were characterized by means of X-ray diffraction (XRD), thermogravimetry and differential thermal analysis (TG/DTA) and dc electrical resistivity measurements. The investigated samples were found to be spinel single phase cubic close packed crystalline materials as demonstrated by XRD data. Using the Debye Scherer formula, the calculated crystallite size was found Co²⁺ concentration dependent and varied between 7 and 19 nm. The lattice constant, X-ray density and bulk density were found to increase while percentage porosity decreases on increasing the Co²⁺ concentration. The dc electrical resistivity was found to decrease as a function of temperature as expected for a typical semiconductor. The doped Co²⁺ ions are believed to form small polarons and hopping of these small polarons between the adjacent sites seems to be partially responsible for conduction in the system. The activation energy of hopping of small polarons was also calculated.     

Er~(3+),Yb~(3+)共掺杂Y_2O_3纳米晶体粉末中1.5μm近红外发光增强现象的研究

用燃烧法制备了平均粒径为10和40nm的(Y0.96Er0.02Yb0.02)O3纳米晶体样品,并通过1200℃高温退火获得了同样组分的体材料样品。利用X射线衍射谱(XRD),傅里叶变换红外吸收光谱(FTIR),透射电镜(TEM)和透射电镜(SEM)照片对样品的晶体结构和形貌进行了表征。测量了不同样品980nm激发下的上转换发射光谱和近红外发射光谱。对实验结果的分析发现,随着粒径的减小,样品发射光谱中红光和近红外发射的成分增加。产生这一现象的原因是由于纳米材料具有比表面积大的特点,能够吸附更多的OH-(振动能量3200～3800cm-1),OH-数量的增加使电子从Er3+的4I11/2→4I13/2能级(能量差3600cm-1)的无辐射弛豫速率增大,这一无辐射弛豫过程减少了4I11/2上的电子布居数,使绿光发射减弱;同时增加了4I13/2上的电子布居数,使红光和近红外发射增强。40nm样品的1.5μm发射主峰强度是体材料的1.6倍,这一结果对纳米发光材料的实际应用是很有意义的。     

纳米二氧化钛的制备及Eu3＋掺杂发光研究

以钛酸四丁酯为前驱物,采用溶胶-凝胶法制备了四种不同配方Eu3+掺杂的TiO2纳米晶.利用扫描电镜（SEM)、EDS能谱、光致发光光谱对样品的形貌、成份及性能进行了表征.研究了退火温度、稀土Eu3+离子掺杂摩尔分数、溶剂乙醇量等对发光性能的影响,并对其发光机理进行了探讨.结果表明:稀土Eu3+掺杂TiO2纳米晶样品,掺杂均匀、颗粒大约在30~80 nm|从EDS能谱分析可得Ti:O原子个数比并不是按化学计量TiO2满足1:2,这是因为在TiO2中形成的是Ti-O-Ti键,Eu3+离子很可能取代了Ti4+离子,同时又形成了氧空位,表明稀土Eu3+离子进入TiO2晶格中|样品的主发射峰在614 nm(5D0→7F2)处发光最强,且在593 nm(5D0→7F1)处出现了属于磁偶极跃迁的发射峰,制备Eu3+∶TiO2纳米晶的组分、退火温度、溶剂乙醇的量不同,发射光谱的强度也不同.     

Contact and non-contact magnetoimpedance in amorphous and nanocrystalline Fe73.5Si13.5B8CuV3Al ribbons

The giant magnetoimpedance (GMI) effect in amorphous and nanocrystalline Fe_73.5Si_13.5B₈CuV₃Al ribbons has been studied as a function of a dc magnetic field, by contact and non-contact methods. In the contact method, an MI of 19% was obtained in the nanocrystalline ribbon while it is of the order of 10⁴ in the non-contact method. The huge sensitivity of the non-contact method is promising with regard to the increase of the sensitivity of the MI sensors. Field dependence of MI has shown double peak behavior in contact method and single peak profile in non-contact method. The domains were found to lie normal to the plane of the ribbon, through MFM studies. All the experimental results were discussed using the Polivanov model.     

Preparation,microstructure, and magnetic properties of a nanocrystalline Nd12Fe82B6 alloy by HDDR combined with mechanical milling

Nanocrystalline Nd₁₂Fe₈₂B₆ (atomic ratio) alloy powders with Nd₂Fe₁₄B/α-Fe two-phase structure were prepared by HDDR combined with mechanical milling. The as-cast Nd₁₂Fe₈₂B₆ alloy was disproportionated via ball milling in hydrogen, and desorption–recombination was then performed. The phase and structural change due to both the milling in hydrogen and the subsequent desorption–recombination treatment was characterized by X-ray diffraction (XRD). The desorption–recombination behavior of the as-disproportionated alloy was investigated by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). The morphology and microstructure of the final alloy powders subject to desorption–recombination treatment were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM), respectively. The results showed that, by milling in hydrogen for 20 h, the matrix Nd₂Fe₁₄B phase of the alloy was fully disproportionated into a nano-structured mixture of Nd₂H₅, Fe₂B, and α-Fe phases with average size of about 8 nm, and that a subsequent desorption–recombination treatment at 760 °C for 30 min led to the formation of Nd₂Fe₁₄B/α-Fe two-phase nanocomposite powders with average crystallite size of 30 nm. The remanence B_r, coercivity H_c, and maximum energy product (BH)_max of such nanocrystalline Nd₁₂Fe₈₂B₆ alloy powders achieved 0.73 T, 610 kA/m, and 110.8 kJ/m³, respectively.     

Role of polytypism and degree of hexagonality on the photoinduced optical second harmonic generation in SiC nanocrystalline films

Photoinduced optiсal second harmonic generation was studied in nanocrystalline SiC films prepared by the method of direct ion deposition. For the studies were chosen three types of polytypes (with different degree of hexagonality) – 24R with degree hexagonality G=25, 27R-G=44, 33R with – G=36. The bicolor photoinduced treatment was performed by the wavelengths 1064nm/532 nm by 15 ns YAG:Nd laser. The efficiency of the output SHG was evaluated by ratio of the corresponding signal intensities with respect to the references and by the time delay between the SHG and the fundamental maxima. Explanation of the observed effect is given within a framework of the occurrence of the nano-trapping levels in the film crystalline interfaces.     

Low-temperature preparation of nanocrystalline anatase films through a sol-gel route

Nanocrystalline anatase (TiO₂) films were prepared at very low temperature through a sol-gel route using titanium isopropoxide and hydrogen peroxide in ethanol. Crystallization occurred after film deposition at 35°C in an atmosphere saturated with water vapor. Both thin and thick films of nanocrystalline anatase were prepared. Observed particle size in crystallized films is approximately 20–40 nm as measured with AFM. No residual organic material was apparent through FTIR after crystallization occurred. Dynamic light scattering studies performed on this system indicate that particle size measured in solution is strongly dependent on the amount of agitation samples received prior to measurement.