原位氧化工艺制备Ag-92SnO2In2O3电接触材料研究

以Ag-65SnIn-8熔炼雾化粉体为原料,采用原位氧化工艺制备了Ag-60SnO₂In₂O₃中间体粉体,与雾化纯银粉配比成Ag-92SnO₂In₂O₃材料,通过混粉-等静压-烧结-热压-挤压技术制备Ag-92SnO₂In₂O₃带材,再通过固相复合工艺制备所需要的Ag-92SnO₂In₂O₃/Cu/Fe电接点材料。相对比常规氧化工艺制备的Ag-60SnO₂In₂O₃中间体粉体制备的Ag-92SnO₂In₂O₃/Cu/Fe电接点材料,原位氧化工艺制备的Ag-92SnO₂In₂O₃/Cu/Fe电接点材料电阻率可达2.1μΩ.cm以下,硬度可达85~110HV;产品应用于380V,65A,功率因数0.7的电动机负载电路的热保护器中,电器寿命满足5000次分断要求,替代AgCdO/Cu/Fe电接点材料,实现环保,无镉化切换。     

SnO2 增强相对AgCuOIn2O3 电触头材料显微组织与性能的影响

采用反应合成法结合塑性变形工艺制备了不同SnO₂含量的AgCuOIn₂O₃SnO₂电触头材料,利用扫描电镜和金相显微镜表征了材料的微观形貌及显微组织,分析对比了不同SnO₂含量的材料金相组织及其增强相的分布均匀性,并利用X射线衍射分析了材料的物相结构。测量了材料的抗拉伸强度、硬度、电阻等性能。结果表明：添加适量的SnO₂能使组织中的孔隙尺寸缩小、其他缺陷明显减少。氧化物弥散分布在银基体中,极大地改善了AgCuOIn₂O₃电触头材料的显微组织均匀性。在SnO₂含量不变时,材料的电阻率随塑性变形程度增加而有所降低;随着SnO₂含量增多,电阻率呈现先降低后升高的趋势,最后趋于定值,约为2.4 μΩ·cm。添加SnO₂后各试样材料的硬度均显著升高,SnO₂含量为1%（质量分数）的材料具有最优的抗拉伸强度和延伸率。     

SnO_2@TiO_2核-壳纳米线的制备及其光催化性能

通过固-液-气(VLS)生长机制,利用化学气相沉积法(CVD)制备SnO_2纳米线。利用原子层沉积(ALD)以钛酸四异丙酯为前驱体在SnO_2纳米线表面沉积不同厚度的TiO_2壳层,形成SnO_2@TiO_2核-壳纳米线结构。通过中间Al_2O_3插层,分别制备出金红石和锐钛矿2种不同晶型的TiO_2,从而制备出2种不同复合结构的SnO_2@TiO_2核-壳纳米线。实验研究该复合结构中TiO_2的厚度与晶型对紫外光下光催化降解甲基橙溶液活性的影响。     

HOPG上ALD沉积Al2O3介电薄膜的生长行为研究

本文采用原子层沉积(ALD)的方法,选择三甲基铝(TMA)和H₂O₂作为反应前驱体,在高定向热解石墨(HOPG)基体上沉积Al₂O₃。系统研究了反应温度和生长周次对Al₂O₃生长行为的影响。研究表明：受HOPG表面饱和成键的影响,Al₂O₃在衬底表面处形核困难,在生长初期主要表现为台阶处择优生长,其形态为线状结构。当沉积100周次Al₂O₃时,其中在沉积温度为50 °C、150 °C和200 °C时呈现为纳米线状结构,而在100 °C时呈现为非连续薄膜。随着生长周次的增加,不同温度下沉积态Al₂O₃都趋于形成连续薄膜,表明其生长行为发生了由三维岛状生长模式向二维平面生长模式的转变。分析认为,生长模式的转变是由纳米线状结构横向生长造成的;横向生长速率主要受生长温度影响。拉曼结果表明：沉积后的石墨烯层结构未受影响,可保留其原有的优越性能。     

多孔ZrO2-8 wt% Y2O3涂层的制备及性能

航空发动机的效率与转动叶片和机匣之间的间隙密切相关。为了控制转子和静子之间的间隙,需要在机匣表面制备可磨耗的封严涂层。在发动机的高温端,ZrO₂-8wt% Y₂O₃涂层是经常采用的封严涂层基体。涂层中的孔隙可以增加涂层的可磨耗性。本文利用聚苯酯(PHB)增加等离子喷涂的ZrO₂-8 wt% Y₂O₃涂层的孔隙率。为了避免聚苯酯在等离子喷涂过程中的烧损,利用溶胶-凝胶法在聚苯酯颗粒表面沉积一层TiO₂层。文中将讨论采用此方法制成的涂层的形态、孔隙率、硬度和可磨耗性。结果表明,在喷涂粉末中混合包覆型的聚苯酯后,涂层的孔隙率将会得到提升,涂层硬度将会下降。磨耗试验的结果表明涂层的磨耗深度随着涂层孔隙率的增加而增加。     

水热制备TiO2纳米管及其光催化性能

本文利用TiO₂粉体在高浓度NaOH溶液中水热反应制备TiO₂纳米管,采用X射线衍射(XRD)、扫描电镜(SEM),透射电镜(TEM),紫外可见分光光度计(UV-Vis)考察了NaOH浓度、水热反应温度、水热反应时间等因素对TiO₂纳米管结构和性能的影响。结果表明：当NaOH浓度为10mol/L,水热反应温度为160℃,水热反应时间20h时,所制备的TiO₂纳米管显示出较高的光催化活性,经紫外光照30min后,对甲基橙(MO)的降解率可达75.48%。     

Fe2O3-CaO-TiO2 体系下铁酸钙的合成过程及TiO2 和CaTiO3 的影响

为了确定高钛型钒钛磁铁矿烧结过程中铁酸钙的生成是受TiO₂还是TiO₂和CaO形成的CaTiO₃影响,首先利用Fe₂O₃和CaO的纯试剂合成了铁酸钙,并研究了TiO₂和CaTiO₃对钛铁酸钙 （FCT） 形成的影响。在Factsage 7.0软件进行热力学计算的基础上,通过在空气气氛下进行烧结,获得了在1023~1423 K温度范围内、不同烧结时间的不同样品。通过X射线衍射和扫描电镜-能谱分析等表征手段,对烧结样品的物相转变和微观结构变化进行了表征。发现FCT的形成过程主要分为2个阶段：前一阶段为1023~1223 K温度范围内Fe₂O₃与CaO之间的反应,合成产物为Ca₂Fe₂O₅,反应方程式为“Fe₂O₃(s)+ 2CaO(s)= Ca₂Fe₂O₅(s)”;后一阶段为1223~1423 K温度范围内Ca₂Fe₂O₅和Fe₂O₃的反应,主要产物为CaFe₂O₄,反应为“Ca₂Fe₂O₅(s)+ Fe₂O₃(s)= 2CaFe₂O₄(s)”,该阶段尤其是温度为1423 K时,反应速率显著加快,随温度的升高CaTiO₃显著增加。然而,Ti元素在铁酸钙中的固溶很难实现,TiO₂与铁酸钙之间的反应不是形成FCT的有效途径。随着保温时间的延长,CaTiO₃和FCT相界中Fe元素含量增加。FCT主要是通过Fe组分在CaTiO₃中固溶形成的,主要反应是“Fe₂O₃+CaTiO₃(s)=FCT(s)”。     

Al2O3/Ti2AlN复合材料在900℃,1000℃和1100℃空气中的氧化行为

利用综合热分析仪、背散射扫描电镜(BSE)和能谱分析(EDS)对Al₂O₃/Ti₂AlN复合材料在900 ℃,1 000 ℃和1 100 ℃/20 h空气中连续氧化20h后的氧化增重及氧化层截面进行了研究。结果表明：Al₂O₃/Ti₂AlN复合材料在空气中的氧化行为符合抛物线规律,在900 ℃,1 000 ℃和1 100 ℃/20 h氧化增重分别为2.78×10_-2 kg/m₂、10.4 ×10_-2 kg/m₂、21.9 ×10_-2 kg/m₂,抛物线速率常数相应为1.08×10_-8 kg₂/m₄s、1.44×10_-7 kg₂/m₄s、6.56×10_-7 kg₂/m₄s,氧化激活能为274 kJ/mol。氧化层主要由TiO₂和Al₂O₃组成的,连续的Al₂O₃次外层可以提高其抗氧化性能。氧化层结构的改变是由于氧化温度对Ti₄₊、Al₃₊由基体表面向外扩散和O_2-向内扩散的影响,以及TiO₂和Al₂O₃在不同温度下的形核生长速率导致的。对Al₂O₃/Ti₂AlN而言,控制材料与氧化气氛的界面是提高该材料抗氧化性能的关键。     

MSM结构TiO2基紫外探测器的制备及光电特性研究

采用RF磁控溅射技术在石英衬底上生长了厚度可调的锐钛矿相TiO₂薄膜,继而采用光刻技术在薄膜上生长了Ag叉指电极,获得了MSM结构TiO₂基紫外探测器。I-V特性测试结果表明Ag与TiO₂之间表现出优良的欧姆接触特性,所制备探测器为欧姆接触。此外,TiO₂薄膜厚度对探测器的光电性能影响显著,当薄膜厚度达到197 nm时,光电性能达到最高。此时,光电流高出暗电流近2.5个数量级,紫外光区的响应度高出可见光区近2个数量级。所制备Ag/TiO₂MSM紫外探测器表现出高灵敏度和可见盲特性。     

SNDC/La2Mo2O9复合电解质材料的制备及性能表征

本文采用甘氨酸-硝酸盐法(GNP)和溶胶凝胶法分别合成了Sm_0.1Nd_0.1Ce_0.8O_1.9(SNDC) 和La₂Mo₂O₉(LAMOX)粉末,并用常压烧结的方法制备了不同比例的SNDC和LAMOX的复合材料,通过XRD和SEM等手段表征了不同复合比例样品的物相和表面形貌并测试了烧结样品的电导率。结果表明,复合样品的电导率在相变点前后随着复合量增加变化趋势相反,其中LAMOX含量为20mol%的样品在550℃时的电导率能达到0.01S/cm,高于同温度下SNDC电导率。     

Modification of TiO2 nanorods by Bi2MoO6 nanoparticles for high performance visible-light photocatalysis

In this work, TiO₂ nanorods were prepared by a hydrothermal process and then Bi₂MoO₆ nanoparticles were deposited onto the TiO₂ nanorods by a solvothermal process. The nanostructured Bi₂MoO₆/TiO₂ composites were extensively characterized by X-ray diffraction, scanning and transmission electron microscopy, X-ray photoelectron spectroscopy and UV-vis diffuse reflectance spectroscopy. The photocatalytic activity of the Bi₂MoO₆/TiO₂ composites was evaluated by degradation of methylene blue. The Bi₂MoO₆/TiO₂ composites exhibit higher catalytic activity than pure Bi₂MoO₆ and TiO₂ for degradation of methylene blue under visible light irradiation (λ > 420 nm). Further investigation revealed that the ratio of Bi₂MoO₆ to TiO₂ in the composites greatly influenced their photocatalytic activity. The experimental results indicated that the composite with Bi₂MoO₆:TiO₂ = 1:3 exhibited the highest photocatalytic activity. The enhancement mechanism of the composite catalysts was also discussed.     

Controlled synthesis of TiO2 mesoporous microspheres via chemical vapor deposition

Anatase titanium dioxide (TiO₂) mesoporous microspheres with core-shell and hollow structure were successfully prepared on a large scale by a one-step template-free chemical vapor deposition method. The effects of various reaction conditions on the morphology, composition and structure of the products were investigated by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Brunauer-Emmett-Teller (BET) technique and photoluminescence (PL) method. The results indicate that the product near the source was composed of core-shell structure TiO₂ microspheres with diameters from 3 to 5 μm. With increasing the distance between the source materials and the substrate, the hollow TiO₂ spheres with 1-2 μm dominant the products. A localized Ostwald ripening can be use to explain the formation of core-shell and hollow structures, and the size of the initial TiO₂ solid nanoparticles plays an important role in determining the evacuation manner of the solid in the ripening-induced hollowing process. The surface area of TiO₂ hollow microspheres determined by the adsorption isotherms was measured to be 74.67 m²/g. X-ray photoelectron spectroscopy (XPS) analysis revealed that the O-H peaks of hollow structures have a chemical shift compared with the core-shell structures. The optical property of the products was also discussed.     

飞秒激光刻蚀微结构对NaOH水热法制备TiO_2光催化性能的影响

Ti基底三维微纳米结构TiO_2(3D-TiO_2)具有比表面积大、光捕获能力强、电荷传输快、可循环利用的优点,在光催化领域具有重要的研究意义和应用前景。采用飞秒激光刻蚀复合Na OH水热法制造Ti基底3D-TiO_2,并研究飞秒激光刻蚀的微阵列结构对3D-TiO_2光催化性能的影响。采用激光共聚焦显微镜(LSCM)、SEM、TEM、XRD对3DTiO_2进行表征分析,并对3D-TiO_2在紫外光照下进行甲基橙降解性能测试。结果表明,复合方法制备的3D-TiO_2由飞秒激光刻蚀的微阵列和Na OH水热法制备的TiO_2纳米线组成。与采用Na OH水热法直接在平整Ti表面制备的TiO_2纳米线相比,3D-TiO_2的染料吸附能力提升100%,光催化性能提升37%。微阵列结构尺寸对3D-TiO_2的性能具有明显影响,随着微阵列宽度的减小或高度的增加,3D-TiO_2的比表面积增大、入射光反射率降低、光催化性能提高。     

TiO2/膨润土复合光催化材料的常温制备及性能研究

采用改进的溶胶-凝胶法,在以水为主要溶剂的反应体系中,控制钛酸四丁酯充分水解、缓慢聚合,在 常压、低温(70℃)的温和条件下制备出稳定的TiO₂纳米晶溶胶,并利用TiO₂纳米晶溶胶在膨润土表面负载,获得TiO₂/膨润土复合光催化材料。采用 X 射线衍射、扫描电镜、比表面积测定等研究手段对样品的结构形貌进行了表征,并考察了其光催化活性。结果表明：较高的水用量有利于TiO₂晶体形成,当去离子水:钛酸四丁酯摩尔比大于167:1时,在溶胶体系中出现了锐钛矿型TiO₂纳米晶体;TiO₂纳米晶主要负载于膨润土表面,并未嵌入到膨润土层间结构,但相对于单一膨润土,TiO₂负载显著提高了材料比表面积;当去离子水:钛酸四丁酯摩尔比=192:1时,在紫外光照射下,复合光催化材料表现出最高的光催化活性,对亚甲基蓝的降解率达到93.8%。     

Fe掺杂TiO2纳米材料的合成及光催化性能

以钛酸丁酯为钛源,Fe(NO3)3·9H2O为铁源,采用溶胶-凝胶法制备Fe/TiO2纳米粉体,利用溶胶结合静电纺丝技术制备Fe/TiO2纳米纤维,从材料改性及形貌改善两个角度共同提高TiO2纳米材料的光催化活性及实用性。借助XRD、SEM、TEM等分析技术,探究了Fe/TiO2纳米材料在可见光区的光催化活性,分析了煅烧温度及掺铁量对Fe/TiO2纳米材料光催化性能的影响。结果显示,铁的掺入及形貌的改善有助于提高TiO2的光催化性能。     

Photocatalytic performance of nano-photocatalyst from TiO2 and Fe2O3 by mechanochemical synthesis

Nano-particles of homogeneous solid solution between TiO₂ and Fe₂O₃ (up to 10 mol%) have been prepared by mechanochemical milling of TiO₂ and yellow Fe₂O₃/red Fe₂O₃/precipitated Fe (OH)₃ using a planetary ball mill. Such novel solid solution cannot be prepared by conventional co-precipitation technique. A preliminary investigation of photocatalytic activity of mixed oxide (TiO₂/Fe₂O₃) on photo-oxidation of different organic dyes like Rhodamine B (RB), Methyl orange (MO), Thymol blue (TB) and Bromocresol green (BG) under visible light (300-W Xe lamp; λ > 420 nm) showed that TiO₂ having 5 mol% of Fe₂O₃ (YFT1) is 3-5 times higher photoactive than that of P25 TiO₂. The XRD result did not show the peaks assigned to the Fe components (for example Fe₂O₃, Fe₃O₄, FeO₃, and Fe metal) on the external surface of the anatase structure in the Fe₂O₃/TiO₂ attained through mechanochemical treatment. This meant that Fe components were well incorporated into the TiO₂ anatase structure. The average crystallite size and particle size of YFT1 were found to be 12 nm and 30 ± 5 nm respectively measured from XRD and TEM conforming to nanodimensions. Together with the Fe component, they absorbed wavelength of above 387 nm. The band slightly shifted to the right without tail broadness, which was the UV absorption of Fe oxide in the Fe₂O₃/TiO₂ particle attained through mechanochemical method. This meant that Fe components were well inserted into the framework of the TiO₂ anatase structure. EPR and magnetic susceptibility show that Fe³⁺ is in low spin state corresponding to μ_B = 1.8 BM. The temperature variation of μ_B shows that Fe³⁺ is well separated from each other and does not have any antiferromagnetic or ferromagnetic interaction. The evidence of Fe³⁺ in TiO₂/Fe₂O₃ alloy is also proved by a new method that is redox titration which is again support by the XPS spectrum.     

Plasma electrolytic oxidation preparation and characterization of SnO2 film

SnO₂ film is firstly prepared by plasma electrolytic oxidation technology in sodium stannate solution. The structure and photocatalytic property of the film are characterized by SEM, XRD and UV-Vis spectrophotometer. Rough and porous netlike film formed on the substrate. The XRD result showed the oxide was pure SnO₂. The absorption edge of the film was determined as 420 nm. Photocatalytic degradation of rhodamine indicated SnO₂ film was an effective photocatalyst.     

Characteristics of N-doped TiO2 nanotube arrays by N2-plasma for visible light-driven photocatalysis

N-doped TiO₂ nanotube arrays were prepared by electrochemical anode oxidation of Ti foil followed by treatment with N₂-plasma and subsequent annealed under Ar atmosphere. The morphologies, composition and optical properties of N-doped TiO₂ nanotube arrays were characterized using field-emission scanning electron microscope (FE-SEM), transmission electron microscope (TEM), X-ray photoelectron spectroscopy (XPS), X-ray diffraction spectrometer (XRD), Photoluminescence (PL) and UV-vis diffusion reflection spectroscopy (UV-vis DRS). Methylene blue (MB) solution was utilized as the degradation model to evaluate the photocatalytic activity of the samples under visible light irradiation. The results suggested N₂-plasma treatment created doping of nitrogen onto the surface of photoelectrodes successfully and the N-doped TiO₂ nanotube arrays display a significantly enhancement of the photocatalytic activity comparing with the pure TiO₂ nanotube arrays under the visible light irradiation.     

Microstructure characterization and photocatalytic activity of mesoporous TiO2 films with ultrafine anatase nanocrystallites

A series of mesoporous TiO₂ films on borosilicate glass with ultrafine anatase nanocrystallites were successfully synthesized using a non-acidic sol gel preparation route, which involves the use of nonionic surfactant Tween 20 as template through a self assembly pathway. The microstructure of these TiO₂ films was characterized by XRD, SEM, HR-TEM, UV-Vis spectroscopy, and N₂ adsorption-desorption isotherm analysis. Their photocatalytic activities were investigated by using creatinine as a model organic contaminate in water. It was found that all mesoporous TiO₂ films prepared with Tween 20 exhibited a partially ordered mesoporous structure. The photocatalytic activity of the TiO₂ films could be remarkably improved by increasing Tween 20 loading in the sol at the range of 50% (v/v), which yielded large amount of catalyst (anatase) on the glass support and enhanced specific surface area. The optimum Tween 20 loading was 50% (v/v) in the sol, above which good adhesion between TiO₂ films and borosilicate glass could not be maintained. The final TiO₂ film (Tween 20: final sol = 50%,v/v) exhibits high BET surface area (∼ 120 m²/g) and pore volume (0.1554 cm³/g), ultrafine anatase nanocrystallinity (7 nm), uniform and crack free surface morphology, and improved photocatalytic activity.     

P-type transparent conducting SnO2:Zn film derived from thermal diffusion of Zn/SnO2/Zn multilayer thin films

Highly transparent, p-type conducting SnO₂:Zn thin films are prepared from the thermal diffusion of a sandwich structure of Zn/SnO₂/Zn multilayer thin films deposited on quartz glass substrate by direct current (DC) and radio frequency (RF) magnetron sputtering using Zn and SnO₂ targets. The deposited films were annealed at various temperatures for thermal diffusion. The effect of annealing temperature and time on the structural, electrical and optical performances of SnO₂:Zn films was studied. XRD results show that all p-type conducting films possessed polycrystalline SnO₂ with tetragonal rutile structure. Hall effect results indicate that the treatment at 400 °C for 6 h was the optimum annealing parameters for p-type SnO₂:Zn films which have relatively high hole concentration and low resistivity of 2.389 × 10¹⁷ cm^− 3 and 7.436 Ω cm, respectively. The average transmission of the p-type SnO₂:Zn films was above 80% in the visible light range.