硫化铋纳米棒的制备与表征

以L-胱氨酸为硫源,采用溶剂热法在不同的溶剂中反应,制备出硫化铋(Bi2S3)纳米薄片和纳米棒,采用X射线衍射(XRD)仪、扫描电子显微镜(SEM)、透射电子显微镜(TEM)等分别对所合成的Bi2S3晶型结构、表面形貌进行表征。结果表明,所合成的Bi2S3为典型的Bi2S3正交结构。以DMF为溶剂,在160℃下反应5d,得到了长为4000～8000nm、宽为200～300nm的正交相Bi2S3纳米棒。根据实验结果对所合成的Bi2S3的形成机制进行简单探讨。     

纳米晶Cu8SnTe6的合成及半导体性能研究

分别采用微波溶剂热法和溶剂热法合成出纳米晶Cu8SnTe6,并比较得出微波溶剂热法制备的纳米晶晶化效果好,粒径细小.通过化学分析和X射线粉末衍射(XRD)、透射电子显微镜(TEM)及X射线光电子能谱(XPS)等手段表征其组成,研究其结构.讨论了反应时间和有机溶剂填充度等反应条件对该纳米晶产率和粒径的影响,探讨了微波溶剂热法合成机理.紫外可见漫反射光谱(UV-Vis)表明,该纳米晶禁带宽度为1.77 eV,具有优良的半导体性能.     

纳米晶Cu8SnTe6的合成及半导体性能研究

分别采用微波溶剂热法和溶剂热法合成出纳米晶Cu8SnTe6,并比较得出微波溶剂热法制备的纳米晶晶化效果好,粒径细小.通过化学分析和X射线粉末衍射(XRD)、透射电子显微镜(TEM)及X射线光电子能谱(XPS)等手段表征其组成,研究其结构.讨论了反应时间和有机溶剂填充度等反应条件对该纳米晶产率和粒径的影响,探讨了微波溶剂热法合成机理.紫外可见漫反射光谱(UV-Vis)表明,该纳米晶禁带宽度为1.77 eV,具有优良的半导体性能.     

L-胱氨酸辅助合成Bi_2S_3纳米片状球和花状结构(英文)

以硝酸铋[Bi(NO)3·5H2O]和L-胱氨酸为反应原料,采用溶剂热法制备出Bi2S3纳米片状球和花状结构。L-胱氨酸(一种非常普遍和实用的氨基酸)作为硫源,在实验过程中不释放出刺激性气味(H2S)。利用X-射线衍射(XRD)、扫描电子显微镜(SEM)对所合成的产物的晶型结构、组成和表面形貌等进行了表征。结果表明:所合成的产物为典型的Bi2S3正交结构;在170°C条件下反应12h,以DMF为溶剂能够得到Bi2S3纳米片状球和花状结构。根据实验结果,对所合成Bi2S3的可能形成机理进行了简单探讨。     

反应时间对溶剂热法制备Bi_2Se_3纳米片的影响

以BiCl3和Se粉为原料,二甘醇(DEG)作为溶剂,Na2SO3作为还原剂,碱性条件,在160℃的反应温度下,利用溶剂热法成功地合成Bi2Se3纳米片,并研究不同反应时间(20,22,24h)作用下所得产物结构形貌的变化。利用XRD和SEM对所合成产物的晶相结构及表面形貌进行表征。结果显示:在不同反应时间下所合成的粉体均为纯物相(均为六方晶相)的纳米片状Bi2Se3,且反应22h条件下所得产物形貌为大小均一、分散性良好的六边形片状结构,其厚度为10～50nm。并分析片状结构Bi2Se3的形成机制。     

Sb2Se3纳米线的水热合成和表征

分别以SbCl3和不同的硒源(SeO2、Se粉)为原料,采用水合肼(N2H4·H2O)为还原剂,用水热法在150 ℃下反应24 h后合成Sb2Se3纳米粉末。通过X射线粉末衍射(XRD)、透射电镜(TEM)、场发射电子扫描电镜(FESEM)以及高分辨透射电镜等分析方法对产物的物相成分和形貌等进行表征。结果表明, 产物的结构为正交晶系的Sb2Se3纳米晶体,其微观形貌为一维纳米线结构。采用不同硒源合成产物的微观形貌基本相似,其中以SeO2作为硒源水热合成的Sb2Se3纳米线比以Se粉作为硒源合成的纳米线要更加窄而薄,而且纳米线尺寸比较均匀一致。纳米线晶体沿[001]方向生长,这与Sb2Se3独特的晶体结构有着密切的联系     

L-半胱氨酸分子辅助溶剂热合成铜铟硫光伏材料

以CuCl2·2H2O为铜源,InCl3·4H2O为铟源,L-半胱氨酸为硫源,N,N二甲基甲酰胺(N,N-dimethylformamide,DMF)为溶剂,在180℃下反应16h合成了CuInS2微晶。用X射线粉末衍射仪、X射线光电子能谱、场发射扫描电子显微镜对产物的结构、形貌、相组分进行表征。结果表明产物是由厚度为10～50nm纳米片组成的球状CuInS2微晶。并对由纳米片组成的球状CuInS2微晶的形成机理进行了简单探讨。     

High-concentration Facile Synthesis of Self-assembled Micronsized Flower Silver Particles by Stainless Steel- Assisted Vitamin C Reduction Method

以Ag NO3为原料,在不锈钢辅助的条件下,通过Vc还原的方法快速合成了微米花球状Ag。产物的形貌和相结构用扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线粉末衍射(XRD)进行了表征。通过改变反应温度和不锈钢可以获得1~6μm的片状花球Ag和棒状花球Ag。对花状Ag的形成机理进行了探讨,其花状结构由多个纳米片或纳米棒团聚而成。     

Ag作催化剂制备的SiC纳米材料的形貌及其发光性能

用化学气相沉积法(CVD)通过碳热还原反应在Si(100)衬底上以Ag纳米颗粒为催化剂制备了糖葫芦状的SiC纳米棒。硅源为溶胶凝胶制备的SiO_2,碳源为炭粉。采用X射线分析衍射仪(XRD)、扫描电镜(SEM)、透射电镜(TEM)、高分辨率透射电镜(HRTEM)、荧光光谱(PL)对产物的组成、形貌、微观结构等进行了表征。结果表明,SiC纳米棒都其有周期性的凹凸,形状貌似糖葫芦状,长度范围为300~600 nm,而直径为30~50 nm。纳米结构生长机制为VLS生长模式,其中Ag催化剂对其形貌起到至关重要的影响。室温下SiC纳米棒的PL发光峰与块体SiC的发光特征峰相比有蓝移。     

添加剂对新型AgTiB2触头材料微结构和性能的影响

以乙二胺为溶剂采用微波溶剂热法合成铜铟镓硒(CIGS)粉体,研究了反应温度、表面活性剂对合成产物物相及形貌的影响.采用X射线衍射仪、扫描电镜及X射线能谱仪对产物的物相、形貌及组成进行表征.结果表明:在反应温度为230℃(反应时间为2 h)条件下可以获得物相单一,颗粒尺寸较小的CIGS粉体.在基准溶液中加入表面活性剂十二烷基硫酸钠(SDS)后对合成产物形貌有明显改善作用,粉体分散性较好,呈圆球状且粒径较小,为100～200 nm.     

La2/3Ca1/3MnO3∶Ag0.4与La2/3Ba1/3MnO3∶Ag0.4的制备及其性能研究

采用化学共沉淀法合成制备了Ag掺杂摩尔百分比为0.4的La2/3Ca1/3MnO3∶Ag0.4 (LCMO∶Ag0.4)、La2/3Ba1/3MnO3∶Ag0.4(LBMO∶Ag0.4)多晶复合材料,通过XRD和R-T分别对两种材料的结构和性能进行测试分析.实验结果表明:所得样品均为正交晶系钙钛矿结构;LCMO∶Ag0.4的金属-绝缘转变温度(Tp=280.2 K)比LBMO∶Ag0.4要高(Tp=256.8 K);LCMO:Ag0.4样品的电阻值比LBMO∶Ag0.4要小两个数量级;LCMO∶Ag0.4的TCR最大值为28％,要远远高于LBMO∶Ag0.4的TCR最大值(0.5％).     

Thermodynamic analysis of the CsNO3-KNO3-NaNo3 system

The thermodynamic properties of the CsNO₃-KNO₃-NaNO₃ system have been derived from an optimization procedure using experimental and published information concerning phase diagram and thermodynamic data for the constituent binary systems and ternary liquid phase. The results are in very close agreement with the experimental data.     

Thermodynamic properties and phase diagrams of the binary systems B2O3–Ga2O3, B2O3–Al2O3 and B2O3–In2O3

We calculated the binary phase diagrams B₂O₃–Ga₂O₃, B₂O₃–In₂O₃ and B₂O₃–Al₂O₃, and the Gibbs energy of formation of the binary compounds, using experimental liquidus data. The B₂O₃–Ga₂O₃ system is of industrial importance, because liquid B₂O₃, in which Ga₂O₃ is not very soluble, is used to protect GaAs during growth of single crystals of GaAs. During recovery of noble metals B₂O₃ is added to slags containing Al₂O₃ to lower the melting point and the viscosity. The B₂O₃–In₂O₃ system is of much less importance to industry. In all three systems we have a liquid miscibility gap, and also solid binary compounds, none of which melt congruently. The miscibility gaps are not surprising, because even in the B₂O₃–Bi₂O₃ system where four congruently melting compounds are present, a liquid miscibility gap exists close to B₂O₃.     

Y2O3-BaO-SiO2-B2O3-Al2O3 glass sealant for solid oxide fuel cells

A glass based on Y₂O₃-BaO-SiO₂-B₂O₃-Al₂O₃ (named YBA) has been investigated as sealant for planar solid oxide fuel cells (SOFCs). The YBA glass has been systematically characterized by differential thermal analysis, dilatometer, scanning electron microscopy, impedance analysis, and open circuit voltage to examine their suitability as sealant. The coefficient of thermal expansion of YBA is 11.64 × 10⁻⁶ K⁻¹ between 323 and 873 K. The resistivity is 9.1 × 10⁴ Ω cm at 800 °C. The glass sealant is found to be well adhered with other cell components, such as electrolytes and stainless steels, at an optimum sealing temperature of 800 °C. All measured results showed that the YBA glass appears to be a promising sealant for SOFCs.     

Al2O3-Sm2O3-CeO2电解质的性能（英文）

采用溶胶-凝胶法和低温燃烧技术制备Ce1-xSmxO2（x=0,0.1,0.2,0.3）和掺杂Sm和（2%-8%）Al2O3的二氧化铈;研究其合成、结构、致密化、导电性和热膨胀等性能,并利用XRD研究其结构和相组成。结果表明,于1300°C烧结球团,获得致密的陶瓷,于1250°C在Ce0.8Sm0.2O0.2中加入2%和4%的Al2O3以促进烧结。利用扫描电子显微镜观察烧结后球团的表面形貌,使用双探针交流阻抗谱研究总离子电导率。     

Zur Kenntnis von RbBa3Ca4Cu3V7O28

Single crystals of RbBa₃Ca₄Cu₃V₇O₂₈ were prepared above the melting point of the reaction mixture. It crystallizes with hexagonal symmetry, space group C_6V⁴-P6₃mc, a 11.1751, c 12.434 Å, Z = 2. RbBa₃Ca₄Cu₃V₇O₂₈ is the second member of a new structure type of the copper-oxovanadates. Ba²⁺ shows an unusual 12-fold coordination. The two calcium positions are coordinated by trigonal prisms and octahedra respectively. The copper coordination is characterized by a stretched square pyramid. The Cu²⁺ ions are outside the centre nearly in plane of the pyramids.

Zusammenfassung

Einkristalle von RbBa₃Ca₄Cu₃V₇O₂₈ wurden oberhalb des Schmelzpunktes der Reaktionsmischung erhalten. Die Verbindung kristallisiert hexagonal, Raumgruppe C_6V⁴-P6₃mc, a 11.1751, c 12.434 Å, Z = 2. RbBa₃Ca₄Cu₃V₇O₂₈ ist das zweite Beispiel für einen neuen Strukturtyp der Kupfer-Oxovanadate, mit 12-fach koordinierten Ba²⁺ -Ionen. Die zwei Calciumpositionen sind trigonal prismatisch bzw. oktaedrisch koordiniert. Die Koordination der Cu²⁺-Ionen ist durch eine gestreckte Pyramide charakterisiert. Cu²⁺ ist auβerhalb des Polyederzentrums nahezu in der quadratischen Fläche der Pyramide angeordnet.     

Gd~(3+)/Ga~(3+)共掺杂石榴石型Yb_3Al_5O_(12)材料的制备及热物理性能

采用柠檬酸溶胶-凝胶法制备了Gd~(3+)/Ga~(3+)双掺杂的石榴石型Yb_(3-x)Gd_xAl_(5-x)Ga_xO_(12)固溶体陶瓷材料(x=0,0.1,0.2,0.3,0.4,0.5;YGAGO)。结果表明:Gd~(3+)/Ga~(3+)共掺杂的YGAGO保持了石榴石相结构;随着Gd~(3+)/Ga~(3+)掺杂量的增加,固溶体样品的衍射峰位整体向低角度偏移;SEM形貌表明Yb_3Al_5O_(12)材料的微观形貌由纳米级晶粒和高密度晶界构成;大离子Gd~(3+)与Ga~(3+)分别对Yb_3Al_5O_(12)晶体结构中Yb~(3+)与Al~(3+)晶格位的取代,不仅因引入的点缺陷明显降低了材料的热导率,同时还造成石榴石型Yb_3Al_5O_(12)晶体结构的松弛,利于热膨胀系数的提高。随着Gd~(3+)/Ga~(3+)掺杂量的增加,晶体中点缺陷浓度不断升高,声子平均自由程不断减小,使得YGAGO的热导率在x=0.5时达到最低值(λ=1.67W/(m·K),T=1273 K),热膨胀系数达到最高值(α_1=11.71×10~(-6)K~(-1),T=1273 K)。     

Mechanochemical synthesis of Al2O3-TiB2 nanocomposite powder from Al-TiO2-H3BO3 mixture

Alumina-titanium diboride nanocomposite (Al₂O₃-TiB₂) was produced using mixtures of titanium dioxide, acid boric and pure aluminum as raw materials via mechanochemical process. The phase transformation and structural characterization during mechanochemical process were utilized by X-ray diffractometry (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), and thermogravimetric analyses (TG-DTA) techniques. A thermodynamic appraisal showed that the reaction between TiO₂, B₂O₃ and Al is highly exothermic and should be self-sustaining. XRD analyses exhibited that the Al₂O₃-TiB₂ nanocomposite was formed after 1.5 h milling time. The results indicate that increasing milling time up to 40 h had no significant effect other than refining the crystallite size.     

Phase transition and piezoelectric properties of K0.48Na0.52NbO3-LiTa0.5Nb0.5O3-NaNbO3 lead-free ceramics

Plate-like NaNbO₃ (NN) particles were used as the raw material to fabricate (1 − x)[0.93 K_0.48Na_0.52Nb O₃-0.07Li(Ta_0.5Nb_0.5)O₃]-xNaNbO₃ lead-free piezoelectric ceramics using a conventional ceramic process. The effects of NN on the crystal structure and piezoelectric properties of the ceramics were investigated. The results of X-ray diffraction suggest that the perovskite phase coexists with the K₃Li₂Nb₅O₁₅ phase, and the tilting of the oxygen octahedron is probably responsible for the evolution of the tungsten-bronze-typed K₃Li₂Nb₅O₁₅ phase. The Curie temperature (T_C) is shifted to lower temperature with increasing NN content. (1 − x)[0.93 K_0.48Na_0.52NbO₃-0.07Li(Ta_0.5Nb_0.5)O₃]-xNaNbO₃ ceramics show obvious dielectric relaxor characteristics for x > 0.03, and the relaxor behavior of ceramics is strengthened by increasing NN content. Both the electromechanical coupling factor (k_p) and the piezoelectric constant (d₃₃) decrease with increasing amounts of NN. 0.01-0.03 mol of plate-like NaNbO₃ in 0.93 K_0.48Na_0.52NbO₃-0.07Li(Ta_0.5Nb_0.5)O₃ gives the optimum content for preparing textured ceramics by the RTGG method.     

Eu^3＋掺杂ZnO-MgO-La2O3-B2O3基发光光纤的弹脆塑性

采用高温固相反应法制备了Eu^3＋掺杂ZnO-MgO-La203-B203基质的光致发光光纤，通过轴向拉伸试验测量了该光纤的应力-应变曲线。应用弹脆塑性理论研究了屈服面的变化和应力-应变的本构关系，计算了拉伸弹性模量、拉伸强度、拉伸最大负荷、拉伸强度的应变、断裂伸长率和材料的脆性指数。结果表明，该光纤弹性模量高于普通玻璃和大理石，接近于硬铝合金和轧制铝，其拉伸强度和所能承载的负荷都较大。