钐掺杂对钛酸钡锶陶瓷结构和介电性能的影响

采用溶胶-凝胶法制备了系列Sm掺杂的Ba(0.8-3x/2)SmxSr0.2TiO3(x=0,0.001,0.003,0.006,0.008 and 0.010)粉体及陶瓷。利用X射线粉末衍射、扫描电子显微镜和精密阻抗分析表征了样品的结构和性质。X射线衍射结果表明Ba(0.8-3x/2)SmxSr0.2TiO3粉体在800℃预烧2 h后为单一的钙钛矿结构;通过对陶瓷微观形貌研究发现,Sm掺杂可以明显地抑制陶瓷晶粒生长,随着Sm掺杂量的增加,晶粒尺寸由40μm减小到2μm;居里温度随着Sm掺杂量的增加而线性降低,移动速率为10℃/mol%,室温下介电常数呈现先增加后减小的趋势,并在x=0.006时达到最大值7800。     

Sm3+含量对BaSmxFe12-xO19 (x≤0.4)铁氧体纳米纤维结构和磁性能的影响

以金属盐和柠檬酸为原料,采用溶胶-凝胶法制备直径在1μm以内的BaSmxFe12-xO19(x≤0.4)铁氧体纳米纤维。采用FTIR、SEM、EDS、XRD和VSM对BaSmxFe12-xO19(x≤0.4)铁氧体纳米纤维进行表征。结果表明,经950℃烧结后,BaSmxFe12-xO19(x≤0.4)铁氧体已成相,且其微观结构和磁性能受掺杂离子浓度的影响。随着Sm3+含量的增加,饱和磁化强度呈先减小后增大的趋势,而矫顽力随Sm3+含量增加而逐渐增大,由x=0时的348.8 kA.m-1增大到x=0.4时的427.5 kA.m-1。与之相对应,在液氮(77 K)条件下,纤维的饱和磁化强度有显著的提高,而矫顽力则明显下降,这主要是由于纳米晶的表面自旋提高造成的。     

Gd~(3+)掺杂锰锌铁氧体的高分子吸附燃烧法制备及电磁性能

采用固态高分子吸附燃烧法合成了Gd3+掺杂锰锌铁氧体Mn0.3Zn0.7Fe2-xGdxO4(x=0,0.01,0.02,0.03,0.04)。借助XRD、SEM和网络分析仪等研究了样品的物相结构和掺杂浓度与电磁特性的关系。结果表明:当x≤0.02时,制得的粉体为单一的锰锌铁氧体,样品的晶格常数随着Gd3+掺杂量的增加先增后减。少量Gd3+掺杂能有效调整锰锌铁氧体的电磁参数,当x=0.02时,微波电磁损耗(RL)最大值达到-18.7dB。     

NiFe_(2-x)Sm_xO_4纳米丝的制备与磁性能

采用溶胶-凝胶法、静电纺丝技术和热处理技术相结合制备了一维NiFe_(2-x)Sm_xO_4(x=0,0.02,0.04,0.06,0.08,0.1)纳米丝。利用X射线衍射仪(XRD)、傅立叶变换红外光谱仪(FT-IR)、扫描电子显微镜(SEM)和振动样品磁强计(VSM)对NiFe_(2-x)Sm_xO_4纳米丝的结构、形貌和磁性能进行表征。结果表明:NiFe_(2-x)Sm_xO_4纳米丝表面光滑、直径均匀、连续,直径约60 nm。掺杂Sm~(3+)没有改变NiFe_2O_4的尖晶石结构,随着Sm~(3+)掺杂量的增大,晶粒尺寸D从44.8 nm减小到19.6 nm。NiFe_(2-x)Sm_xO_4纳米丝表现出软磁特性。随着Sm~(3+)掺杂量的增大,NiFe_(2-x)Sm_xO_4纳米丝的饱和磁化强度(Ms)、剩余磁化强度(Mr)和矫顽力(Hc)先减小后增大,在x=0.08时分别达到最小值22.54,2.98emu·g~(-1),90.33 Oe。     

Sm-Co共掺杂锶铁氧体的固相制备与磁防蜡性能

以硝酸锶、硝酸铁、硝酸钐、硝酸钴为原料,采用低热固相法制备出前驱体,经灼烧后得到最终产物,使用XRD、EDX、SEM对其表征,表明产物为Sm-Co共掺杂的Sr1-xSmxCoxFe12-xO19(x=0~0.5)锶铁氧体;并发现所制产物具有单一的六方相晶体结构,粒子尺寸在40~100 nm,随着Sm-Co掺杂量的增大,晶粒尺寸逐渐减小。经VSM测试:产物的磁性能(Ms,Mr,Hc)随Sm-Co的共掺杂量的增加(0~0.5),先增大后减小,在x=0.1时表现为最大值(Ms=64.32 A·m2·kg-1、Mr=36.17 A·m2·kg-1、Hc=417.45 k A·m-1)。将制得的共掺杂锶铁氧体磁粉,添加到醇酸清漆中形成防蜡涂层,通过拉伸强度测试、涂层防蜡率实验、以及晶相显微表征,发现该涂层随磁粉用量增加,抗拉强度提高;同时随磁粉磁性的增强,涂层的防蜡效果增加,在磁粉用量为2%时,涂层磁性最大,防蜡率也达到最大值77.3%。     

Sm-Co共掺杂锶铁氧体的固相制备与磁防蜡性能（英文）

以硝酸锶、硝酸铁、硝酸钐、硝酸钴为原料,采用低热固相法制备出前驱体,经灼烧后得到最终产物,使用XRD、EDX、SEM对其表征,表明产物为Sm-Co共掺杂的Sr1-xSmxCoxFe12-xO19(x=0~0.5)锶铁氧体;并发现所制产物具有单一的六方相晶体结构,粒子尺寸在40~100 nm,随着Sm-Co掺杂量的增大,晶粒尺寸逐渐减小。经VSM测试:产物的磁性能(Ms,Mr,Hc)随Sm-Co的共掺杂量的增加(0~0.5),先增大后减小,在x=0.1时表现为最大值(Ms=64.32 A·m2·kg-1、Mr=36.17 A·m2·kg-1、Hc=417.45 k A·m-1)。将制得的共掺杂锶铁氧体磁粉,添加到醇酸清漆中形成防蜡涂层,通过拉伸强度测试、涂层防蜡率实验、以及晶相显微表征,发现该涂层随磁粉用量增加,抗拉强度提高;同时随磁粉磁性的增强,涂层的防蜡效果增加,在磁粉用量为2%时,涂层磁性最大,防蜡率也达到最大值77.3%。     

掺杂铬对NiFe2O4的磁性和结构稳定性影响

利用物理特性测试仪对共沉淀法制备的Cr3+掺杂NiFe2O4的磁性能进行测试,发现掺杂Cr3+并经350、 600℃焙烧的NiFe2O4样品,饱和磁化强度Ms和剩磁Mr随掺杂量的增加而下降,矫顽磁场强度Hc随掺杂量的增加而增加.XRD平均晶粒测试结果显示,样品的平均晶粒大小随掺杂量的增加而减小.在共沉淀过程掺杂的Cr3+经600℃热处理后已进入NiFe2O4晶格.晶格中的Cr3+对NiFe2O4分解CO2的H2/CO2循环反应性能产生很大影响,纯NiFe2O4循环反应15次失活,而掺4%Cr3+的NiFe2O4循环反应50次仍然具有活性.     

Mg-Co-Ti共掺杂对M型钡铁氧体磁性能的影响

采用溶胶-凝胶方法制备了不同Mg-Co-Ti掺杂量的Ba(MgCo)_x/2Ti_xFe_11.5-2xO₁₉磁性粉体，运用XRD和SEM对样品成分及颗粒大小进行了表征，并运用VSM测试了样品的磁性能。结果表明：所制备的粉体1100℃煅烧2小时，粉体结晶良好，呈纯相结构，粉体颗粒大小平均在250 nm左右。随着掺杂含量x从0.1增加到0.6，矫顽力Hc从342 kA/m下降至143 kA/m，而饱和磁化强度Ms先增加，随后降低，在x=0.3时获得最大Ms为55.27 Am²/kg。剩余磁化强度Mr，随着掺杂含量x的增加，先增加，然后逐渐减少。当x=0.3时剩余磁化强度最大值为30.90 Am²/kg。研究表明，可以通过在Fe位掺杂不同含量的Mg-Co-Ti，调整钡铁氧体的磁性能，以适应不同的应用需求。     

共沉淀法合成y3fe5o12∶r（r:co，ni）及其磁性

以碳酸氢铵为沉淀剂,用反滴加共沉淀法获得前驱体,将前驱体在900℃下煅烧5 h,合成了Co∶Y3Fe5O12(YIG)及Ni∶Y3Fe5O12(YIG)。通过对YIG前驱体的TG-DTA分析结果表明,样品的晶相形成温度为778℃。利用XRD测试技术对样品结构进行表征,Y3Fe5-xRxO12中的x为0～0.15时,样品为立方相,Ia3d空间群,当x=0.25时转变为四方相。样品中Y3Fe5-xRxO12的掺杂浓度x高于0.15时均出现杂相。用振动磁强计测试样品的磁性质的结果表明,Y3Fe5-xNixO12和Y3Fe5-xCoxO12样品的比饱和磁化强度均随着掺杂量的增加而增大,但杂相的出现引起磁化强度降低,Y3Fe5-xCoxO12中x=0.25时,比饱和磁化强度最大值为22.6 A.m2/kg,Y3Fe5-xNixO12中x=0.25时,样品为单相比饱和磁化强度最大值为24.5 A.m2/kg。     

共沉淀法合成Y3Fe5O12:R(R:Co,Ni)及其磁性

以碳酸氢铵为沉淀剂,用反滴加共沉淀法获得前驱体,将前驱体在900℃下煅烧5 h,合成了Co:Y3Fe5O12(YIG)及Ni:Y3Fe5O12(YIG).通过对YIG前驱体的TG-DTA分析结果表明,样品的晶相形成温度为778℃.利用XRD测试技术对样品结构进行表征,Y3Fe5-xRxO12中的x为0～0.15时,样品为立方相,Ia3d空间群,当x=0.25时转变为四方相.样品中Y3Fe5-xRxO12的掺杂浓度x高于0.15时均出现杂相.用振动磁强计测试样品的磁性质的结果表明,Y3Fe5-xNixO12和Y3Fe5-xCoxO12样品的比饱和磁化强度均随着掺杂量的增加而增大,但杂相的出现引起磁化强度降低,Y3Fe5-xCoxO12中x=0.25时,比饱和磁化强度最大值为22.6 A·m2/kg,Y3Fe5-xNixO12中x=0.25时,样品为单相比饱和磁化强度最大值为24.5 A·m2/kg.     

Effect of support and reactant on the yield and structure of carbon growth by chemical vapor deposition

The effect of catalyst support and reactant on the yield and structure of carbon growth has been investigated in the chemical vapor deposition (CVD) process. Powder Fe and Fe/Al(2)O(3) were the catalysts studied, and CO/H(2), CO, CH(4), and C(2)H(6)/H(2) were used as gas precursors. Platelet and fishbone-tubular structures were produced on powder and supported Fe from CO/H(2), with average diameters of 115 and 45 nm and yields of 28.8 and 17.6 g of C/g of cat. in 8.5 h, respectively. Onionlike carbon was the main structure produced from pure CO on both catalysts. In contrast, from hydrocarbons the highest yield of 2.24 g of C/g of cat. was achieved on Fe/Al(2)O(3), with predominantly tubular structures produced and average tube diameters close to 21 nm. It is concluded that the reactivity and carbon nanostructures are dictated by the size and crystallographic orientation of the catalyst particles. It has been suggested that the tubular structures were grown by continuous carbon supply directly to the tube, but the fiber structures were grown in a layer-by-layer manner. Controlled synthesis of carbon nanotube, platelet nanofiber, fishbone-tubular nanofiber, and onionlike carbon with high selectivity and yield was demonstrated.     

Impingement mixing and its effect on the microstructure of RIM polyurethanes

The effect of impingement mixing on the microstructures developed during a reaction injection molding process in a thermoplastic urethane system was investigated. The polyurethane studied was a 4,4′-diphenylmethane diisocyanate/l,4-butane diol/poly(propyleneoxide) end-capped with poly(ethy1eneoxide) polyol system with a 5/4/1 molar ratio. Three different impingement mixing levels ranging from Re = 80 to Re = 210 were implemented by a laboratory RIM machine. The samples were characterized by gel permeation chromatography (GPC), differential scanning calorimetry (DSC), optical microscopy, and transmission electron microscopy (TEM). Morphologies of hard-segment globules, hard-segment spherulites, and soft-segment rich matrix were observed. The multiple DSC endotherms were related to different crystalline structures. A higher level of mixing was found to increase the molecular weight and produce more paracrystalline structures. A lower mixing level produced better phase separation and spherulitic structures. High temperature annealing caused transurethanization, which may allow molecular rearrangement and change the crystalline structures.     

Nanostructures of polyelectrolyte gel–surfactant complexes

Small‐angle X‐ray scattering was used to investigate the nanostructures of complexes formed by slightly crosslinked anionic copolymer gels of poly(sodium methacrylate‐co‐N‐isopropylacrylamide) [P(MAA/NIPAM)] with cetyltrimethylammonium bromide (CTAB), and didodecyldimethylammonium bromide (DDAB), respectively, at room temperature (∼ 23°C). Several highly ordered supramolecular structures were observed in the polyelectrolyte gel–surfactant complexes. In P(MAA/NIPAM)–CTA systems, in sequence with decreasing charge density of the P(MAA/NIPAM) copolymer chains, structures of the Pm3n space group cubic, face‐centered cubic close packing of spheres, and hexagonal close packing of spheres were determined at a charge content of ≥ 75, 67, and 50%, respectively. The spheres and rods in these structures were the spherical and cylindrical micelles formed by the self‐assembly of CTA cations with their paraffin chains inside. Both the aggregation number and the size of the micelles decreased with a decreasing charge density of the copolymer chains. In the P(MAA/NIPAM)–DDA systems, the bilayer lamellar structures formed at charge contents ≥ 75% transferred to bicontinuous cubic structures of the Ia3d space group at charge contents of 50–67%. The rods in the Ia3d cubic structures were formed by the self‐assembly of double‐tailed DDA cations with polar moieties inside. The formation of these highly ordered structures were driven by both electrostatic and hydrophobic interactions of the charged copolymer chains/surfactants and the surfactants/surfactants inside the charged gels. The structures became less ordered by further decreasing the charge content of the P(MAA/NIPAM) chains. © 1999 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 37: 2165–2172, 1999     

Surface characterizations of spin-coated films of ethylcellulose and hydroxypropyl methylcellulose blends

Films of pure ethylcellulose (EC) and hydroxypropyl methylcellulose (HPMC) polymers and EC/HPMC blends were prepared from solutions by spin coating where isopropyl alcohol (IPA), water, and IPA/water cosolvent were used as solvents. Surface structures of the films were investigated using optical microscopy, atomic force microscopy (AFM), and Raman mapping and spectroscopy. For the films prepared from EC/HPMC blend solutions using the IPA/water cosolvent, different domain structures such as islands or pits and phase separation between EC and HPMC were observed by optical microscopy and AFM. The nature of the polymer components on the surface of the films was identified by Raman mapping and spectroscopy. Experimental results also indicated that polymer composition, solvent, and temperature during spin coating had significant impacts on surface structures of the films.     

Photovoltaic Properties of Titanium Dioxide Nanowires with Different Crystal Structures

Titanium dioxide(TiO₂) nanowires with different crystal structures were successfully synthesized, and their charge transfer properties were further investigated by surface photovoltage(SPV), transient photovoltage(TPV) and surface photocurrent(SPC) techniques. The results reveal that both the surface states and the charge transfer rate of different TiO₂ nanowires are highly dependent on their crystal structures.     

Application of Crosslinked Acrylamidoxime/2-Acrylamido-2-methylpropane Sulfonic Acid Copolymer in Wastewater Treatment

Crosslinked acrylonitrile/acrylamidoxime/2-acrylamido-2-methylpropane sulfonic acid (AN/AAx/AMPS) based hydrogels was prepared by radical solution polymerization technique. The structures of hydrogels were characterized by FTIR analysis and the results were consistent with the expected structures. These hydrogels were used for the separation of Cd(II), Cu(II), and Fe(III) ions from their aqueous solutions. The influence of the uptake conditions such as pH, time, and initial feed concentration on the metal ion binding capacity of hydrogel was also tested. The selectivity of the hydrogel toward the different metal ions tested was Cd(II)>Fe(III)>Cu(II). The recovery of metal ions was also investigated in acid media.     

不同晶相TiO2负载Cu2O催化甲醛乙炔化反应

分别以金红石相和锐钛矿相TiO₂为载体, 采用液相还原-沉积法制备了Cu₂O/TiO₂催化剂. 采用氮气物理吸附-脱附(N₂-physisorption)实验、 氢气程序升温还原(H₂-TPR)、 X射线衍射(XRD)、 X射线光电子能谱(XPS)、 CO红外光谱(CO-IR)及高分辨透射电子显微镜(HRTEM)等技术, 研究了不同晶相TiO₂载体对Cu₂O/TiO₂结构及其催化甲醛乙炔化反应性能的影响. 结果表明, 以金红石相TiO₂为载体的催化剂炔化活性明显高于以锐钛矿相TiO₂为载体的催化剂, 原因在于金红石相TiO₂主要暴露(110)晶面, 其与铜物种的配位环境及较高的空位密度形成了更多的Cu—O—Ti结构物种, 表现为Cu₂O与TiO₂之间强的相互作用. 这导致Cu₂O高效转变为乙炔亚铜活性物种, 并保持了较高的分散度与稳定性, 抑制了过度还原物种金属Cu的生成, 进而使催化剂表现出较高的催化性能.     

Study of three-dimensional configurations of (γ-methacryloxypropyl)-silsesquioxanes by ultraviolet laser matrix-assisted desorption/ionization time-of-flight mass spectrometry and quantum chemical calculation

[(3-Methacryloxy)propyl]silsesquioxanes (MSSO) were prepared from the hydrolytic condensation of [(3-methacryloxy)-propyl]trimethoxysilane (MPMS) in the presence of an acid catalyst (HCOOH). The proposed MSSO structures were characterized with Fourier transform infrared (FTIR) and nuclear magnetic resonance (NMR) ((1)H, (13)C and (29)Si), and were assigned by ultraviolet laser matrix-assisted desorption/ionization time-of-flight mass spectrometry (UV-MALDI-TOF MS). The large organic group connected to silicon was simplified for the quantum chemical calculation (QCC), and the correlation of the calculated total energies (E(T)) before and after simplification was analyzed by multiple linear regression, verifying no significant influence on the final conclusions of the research of structural formulas by a correlation coefficient (r). The geometric parameters (Si-O bond length and Si-O-Si, O-Si-O bond angles) and E(T) of the simplified MSSO were calculated by QCC to determine the relative stability of various MSSO structures. The structural geometry (silicon ring), the fraction of intramolecular cycles (f) and the number of the silicon rings (F) were also employed to qualitatively determine the relative stability. The results of the calculation showed that almost all of the cage structures had a lower E(T) than the isomeric ladder structures; therefore, most MSSO structures are of the cage type.     

ZnO掺杂的SnO_2纳米纤维的制备、表征及气敏机理(英文)

以二水氯化亚锡(SnCl2·2H2O)为盐原料,采用静电纺丝的方法制备了SnO2纳米纤维.为了研究ZnO掺杂对SnO2形貌、结构及化学成分的影响,分别制备了不同含量ZnO掺杂的SnO2/ZnO复合材料.利用热重-差热分析(TG-DTA)、X射线衍射(XRD)、傅里叶变换红外(FTIR)光谱仪、扫描电镜(SEM)及能量色散X射线(EDX)光谱对材料的结晶学特性及微结构进行了表征.制备的SnO2/ZnO复合材料是由纳米量级的小颗粒构成的分级结构材料.ZnO含量不同,对应的SnO2/ZnO复合材料结构不同.表征结果表明ZnO的掺杂量对SnO2材料的形貌及结构均起着重要作用.将制备的不同ZnO含量的SnO2/ZnO复合材料进行气敏测试,测试结果表明,Sn:Zn摩尔比为1:1制作的气敏元件对甲醇的灵敏度优于其它摩尔比的气敏元件.讨论了SnO2/ZnO复合材料气敏元件的敏感机理.同时针对Sn:Zn摩尔比为1:1时表现出最好的气敏响应,分析了其原因,包括Zn的替位式掺杂行为、ZnO的催化作用、过量ZnO对SnO2生长的抑制作用以及SnO2与ZnO晶粒界面处的异质结.     

Theoretical Studies on Structures and Stabilities of C4H2+ Isomers

The structures, energies, stabilities and spectroscopies of doublet C₄H₂⁺ cations were explored at the DFT/B3LYP/6-311G(d,p), CCSD(T)/6-311+G(2df,2pd)(single-point), and G3B3 levels. Ten minimum isomers including the chainlike, three-member-ring, and four-member-ring structures are interconverted by means of 15 interconversion transition states. The potential energy surface was investigated. At the CCSD(T)/6-311+G(2df,2pd) and G3B3 levels, the global minimum isomer was found to be a linear HCCCCH. The structures of the stable isomer and its relevant transition state are further optimized at the QCISD/6-311G(d,p) level. The bonding nature and structure of isomer HCCCCH were analyzed.