两步法合成双氰胺工艺

采用两步法由氰氨化钙合成双氰胺,通过正交试验,考察了水解温度、聚合温度、聚合时间对产品收率的影响,确定了最佳的工艺条件:水解温度42℃、聚合温度70℃、聚合时问150 min,此条件下,双氰胺收率可达85.73％。     

PEG20000中试放大的工艺研究

在一定温度和催化剂作用下 ,分别利用本体聚合和溶剂聚合的方法 ,在 1L、10 0L不锈钢高压反应釜中合成了相对分子质量为 2 0 0 0 0的聚乙二醇 ,并讨论了聚合反应机理 ,研究了催化剂用量、反应温度、反应时间对聚合反应的影响。经过红外、核磁共振、凝胶色谱、化学分析等方法对产物进行了表征。     

场激活加压燃烧合成WC-Ni复合材料的工艺参数研究

以钨、碳和镍为原料,在电场激活下,材料的燃烧合成和致密化同时进行,短时间内完成了碳化钨镍复合材料的制备。研究了场激活 加压燃烧合成中的工艺参数,如脉冲电流、能量控制模式、升温速率、最高温度和压力对反应的影响。测量了在反应合成和致密化前后的样品 收缩率。所制备的复合材料的相对密度,490N载荷下Vickers硬度和断裂韧性分别为99.2%,13.965GPa和5.9MP·m1/2。     

A new colloidal precursor cooperative conversion route to nanocrystalline quaternary copper sulfide

A novel milk-like Cu-thiourea colloid has been synthesized. Nanocrystalline quaternary copper sulfide Cu₂FeSnS₄ was obtained through the Cu-thiourea colloidal precursor cooperative conversion route at low temperature. The samples were characterized by means of X-ray powder diffraction, transmission electron microscopy, scanning electron microscopy, inductively coupled plasma atomic emission spectroscopy, and X-ray energy dispersive spectroscopy techniques. The reaction details and features were described and discussed.     

The reaction of ceria coatings on mica with H2S: An in-situ X-ray diffraction study

Thin layers of ceria were deposited on the surface of mica platelets in solution. The reaction of such particles with hydrogen sulfide yields a red colored special effect pigment. The ceria layer reacts with H₂S to produce a variety of sulfide and oxysulfide phases. The reaction path discovered in situ by time and temperature resolved X-ray diffraction is CeO₂→CeS₂→C-Ce₂S₃→Ce₁₀S₁₄O. The reaction itself is extremely variable depending on gas flow, heating rates and decomposition atmospheres. Effects on the thin film are recorded by scanning electron microscopy (SEM) and revealed a destruction of the layer once red Ce₁₀S₁₄O was formed. The product layer then reveals the typical nonwetting behaviour of a liquid on a surface.     

A comparative study of the gas sensing behavior of nanostructured nickel ferrite synthesized by hydrothermal and reverse micelle techniques

A comparative study of gas sensing behavior of nanocrystalline nickel ferrite synthesized by micro-emulsion and hydrothermal method to liquefied petroleum gas (LPG) is presented. Nanocrystalline nickel ferrite synthesized by hydrothermal method indicated higher electrical conductivity and gas sensitivity at low operating temperature compared to nanocrystalline nickel ferrite synthesized by reverse micelle technique. This difference in the gas sensing behavior can be attributed to the presence of more oxygen vacancies (i.e. non-stoichiometry) in the hydrothermally synthesized nickel ferrite. Incorporation of palladium had a catalytic effect and the operating temperature was significantly reduced in both the samples. The higher operating temperature of the reverse micelle nickel ferrite material makes the sensor response speed faster (∼10 s) compared to the hydrothermally synthesized material (∼1 min).     

Electrical conductivity and gas sensitivity of Zn-Sb-O thick films

The thick film of Zn-Sb-O was prepared by coating the paste of nanoparticles mixture (Sb₂O₃:ZnO=1:3) on the alumina substrate, followed by sintering at 500-900 °C for 2 h in air. The electrical resistance and gas-sensing properties to benzene, alcohol and acetone of Zn-Sb-O films were found to be dependent on the change of phase structure caused by sintering temperature.     

The Influence of Ir and Pt Addition on the Synthesis of Fullerenes at Atmospheric Pressure

The addition of metallic Ir and Pt to a fullerene-forming, atmospheric-pressure plasma reactor was found to influence the generation of carbonaceous products. It was observed that the added metals were efficiently dispersed into the plasma and that their presence increased the yield of fullerenes. The addition of Ir led to a noticeable shift in the fullerene distribution towards C₆₀, whereas the addition of Pt increased the proportion of C₆₀ oxides and decreased the proportion of higher fullerenes. Addition of Ir also caused a reduction of the soot particle size and the formation of a considerable quantity of carbon nanotubes.     

利用铝（100）面隧道孔制备纳米模板及有序阵列材料

高纯铝箔通常通过电化学扩面后用作铝电解电容器的阳极材料。利用铝箔（100）面隧道孔制备纳米模板。这种纳米模板的特点是制作简单、模板面积大，纳米阵列材料形状可控性强。还利用两步电化学侵蚀铝箔的特殊工艺，研制出纵横交错的TiO2纳米有序阵列材料。     

Ionothermal synthesis of a three-dimensional zinc phosphate with DFT topology using unstable deep-eutectic solvent as template-delivery agent

A three-dimensional zinc phosphate compound with DFT topology, designated as ZnPO₄-EU1, has been synthesized by an ionothermal approach from the system HF-ZnO–P₂O₅-choline chloride-imidazolidone. Ethylenediamine, derived from decomposition of the imidazolidone component of the deep-eutectic solvent (DES) itself, is delivered to the synthesis and serves as an appropriate template for ZnPO₄-EU1. Experiments in which the synthesis conditions were varied showed that ZnPO₄-EU1 may be prepared over a wide molar ratio of P/Zn = 0.55–13.0. Powder X-ray diffraction patterns have been obtained at intervals to track the crystallization process of this material. The experimental data show that Zn₃(PO₄)₂ · 4H₂O (a dense phase) was first isolated from the DES after reaction for 1 h. Subsequently, the pure phase of ZnPO₄-EU1 was obtained with increasing crystallization time from 12 h to 72 h. The experimental results show that the nucleation and crystallization take place with relatively low levels of solvent degradation, demonstrating that zinc phosphate with a three-dimensional framework can be synthesized by in situ generation of an appropriate template using an unstable DES at high temperatures (150–200 °C).