注浆成型法制备的钇稳定化氧化锆电解质性能研究

采用注浆法制备了钇稳定化氧化锆（ＹＳＺ）电解质。制得的样品的密度随烧结温度的升高而提高,经１５５０℃烧结的样品的相对密度对９３％,当其厚度大于０．２ｍｍ时,可以达到气密的程度,从而可以作固体氧化物燃料电池的电解质。样品经１３００℃以上温度的烧结后,可得到完全的立方萤石结构。扫描电镜测量结果表明,随烧结温度的升高,样品的晶粒尺寸变大,孔洞变小。对样品的电阻能结果表明,在相同的温度下,各样品的晶粒电阻     

低成本YSZ电解质膜管的制备和性能研究

用真空注浆法制备出膜厚为0.2mm的8mol%YSZ电解质膜管，用排水法、SEM和复阻抗等分析手段研究了YSZ电解质膜管烧结密度、表面形貌及其电导性能，确定了可使YSZ电解质膜管获得最佳烧结性能的烧结温度。研究结果表明，真空注浆法是一种制备高烧结性能YSZ电解质膜管的简单方法。用这一方法已制备出相对密度为98.1%、长度为254mm的致密YSZ电解质膜管，其烧结温度范围比传统注浆法制备YSZ电解质管降低了190～200℃。研究还表明，随烧结温度升高，样品致密度增大，导电性能也逐渐提高。经1600℃烧结2h样品的烧结密度和导电性能均达到最佳值；进一步提高烧结温度，样品的致密度和电学性能均有所下降。     

ZrO2-Y2O3(CaO)固体电解质的致密化烧结及电性能研究

研究了Ｙ２Ｏ３、ＣａＯ稳定剂及Ａｌ２Ｏ３、ＳｉＯ２（ＡＳ）添加剂对ＺｒＯ２固体电解质的烧结性能和电特性的影响。结果表明,加入ＡＳ的样品微观结构致密,其相对密度达到９７％。ＡＳ添加剂导致ＺｒＯ２固体电解质的粒界偏析和电导率下降,但是在ＡＳ含量很少时,对ＺｒＯ２的电特性影响不大。     

管状YSZ电解质的制备及其在固体氧化物燃料电池中的应用*

以 8mol %钇稳定化氧化锆 (YSZ)为原料 ,以阿拉伯树胶为分散剂和粘接剂 ,采用改进注浆法制备出长度为 2 2 6～2 60mm、壁厚为 0 .4～ 0 .9mm的致密YSZ电解质薄管。设计并制出带有一定锥度的空芯石膏模 ,研究了球磨时间对成型料浆稳定性的影响 ,烧结温度对YSZ样品致密度的影响。研究结果表明 :球磨时间在 75～ 14 0min的范围内料浆的稳定性较好 ,随烧结温度的升高 ,样品的致密度提高。用这种YSZ薄管制成固体氧化物燃料电池 ,电池的电学性能随温度的升高而明显提高 ,三节电池串联的最大功率为 2 .2W。     

管状YSZ电解持的制备及其在固体氧化物燃料电池中的应用

以8mol%钇稳定化氧化锆（YSZ）为原料,以阿拉伯树胶为分散剂和粘接剂,采用改进注浆法制备出长度为226－260mm、壁厚为0.4-0.9mm的致密YSZ电解质薄管。设计并制出带有一定锥度的空芯石膏膜,研究了球磨时间对成型料浆稳定性的影响,烧结温度对YSZ样品致密度的影响。研究结果表明：球磨时间在75-140min的范围内料浆的稳定性较好,随烧结温度的升高,样品的致密度提高。用这种YSZ薄管制成固体氧化物燃料电池,电池的电学性能随温度的升高而明显提高,三节电池串联的最大功率为2.2W。     

YSZ包覆YDC纳米晶复合固体电解质的制备

研究了YSZ包覆YDC纳米晶复合固体电解质的制备工艺.首先,以分析纯的Ce(NO3)3·6H2O和Y(NO3)3·6H2O为原料,采用沉淀法制备了分散性较好的YDC纳米粉体,然后将其均匀分散于含有分析纯的ZrOCl2·8H2O、Y(NO3)3·6H2O的醇水溶液中,采用溶胶凝胶法制备了ZrO2(Y2O3)包覆CeO2(Y2O3)复合纳米粉体.XRD、TEM、IR分析结果表明经600℃焙烧后的CeO2-Y2O3复合纳米粉体为单一萤石相,晶粒尺寸为15nm左右且分散性良好;成功合成了的YSZ包覆YDC复合纳米粉体,其中反应温度在75℃时粉体的包覆性及其分散性较好.以合成的包覆型纳米粉体为原料,通过常压烧结制备了包覆型YSZ/YDC复合固体电解质.研究表明,在相同保温时间内(2h),随着烧结温度从800℃提高到1350℃,试样相对密度从52%迅速增加95%以上.当烧结条件为从室温升温到1300℃,迅速降温到1250℃保温2h后,烧结体的相对密度可达95%以上,平均晶粒度为100nm左右.     

素坯高压成型对纳4YSZ烧结的影响

在纳米4YSZ粉中加入少量纳米Al2O3粉，素坯两次400MPa加压成型后在4GPa高压下再成型，素坯相对密度达72．4％，降低了烧结密温度，超密实坯体在1100℃常下烧结2小时，陶瓷体密度达99．2％。烧结样品的晶胞四方度atct^-1为1．012，晶胞体积V为0.132nm^3，1100℃常压煅以烧，烧结体晶粒大小在40－70nm。烧结体研磨成粉后含有12－14％的单斜相。     

低温烧结ZnNb2O6/TiO2复合陶瓷的制备及介电性能研究

本文研究了ZnO∶Nb2O5∶TiO2=1∶1∶x系统中x量的变化对材料烧结特性、相组成及介电性能的影响.随x的增加,致密化温度逐步升高,晶相组成逐步从ZnTiNb2O8相转变为(Zn0.15Nb0.3Ti0.55)O2相,介电常数增大,Q.f值先增后减,τf向正温度系数方向移动.当x=1.92,在930℃保温4h,可获得晶粒大小均匀、结构致密的烧结体,并有较佳的介电性能:εr=37.71,Q.f=10370GHz(fo=2.5GHz),τf=-2ppm/℃;x>1.92或<1.92,会出现气孔、晶粒异常长大等现象,从而导致材料损耗的增大.     

预烧结温度对注浆成型3Y-TZP齿科陶瓷可加工性的影响

基于注浆成型技术采用两次烧结法(预烧结—加工—最终烧结)制备3Y-TZP(3%(摩尔分数)Y2O3稳定ZrO2)齿科陶瓷材料,研究了预烧结温度对其收缩率、维氏硬度、断裂韧性和磨损量的影响,结合脆性指数和磨损量对其可加工性进行评价,并表征了最终烧结后3Y-TZP微观形貌和力学性能。结果表明,随着预烧结温度的提高,3Y-TZP的收缩率、维氏硬度和 断裂韧性均 增加,而单 位面积磨损 量下降;1250℃预烧结的3Y-TZP脆性指数为244.6,高速涡轮牙钻钻孔后边缘清晰、无崩裂现象;1500℃完全烧结后晶粒尺寸增大,维氏硬度为(9339.4±823.2)MPa,断裂韧性为(3.66±0.41)MPa·m1/2,可以满足齿科材料对力学性能的要求。     

Yb2O3掺杂8YSZ电解质材料的制备和性能研究

用共沉-胶化-低温干燥制备2Yb-8YSZ粉末,喷雾制粒获得球状颗粒.用激光粒度分析,X射线衍射仪(XRD),比表面测定仪(BET)和扫描电子显微镜(SEM)检测粉末和陶瓷体的性能,组织结构和相组成.结果表明,煅烧粉末的粒径为0.86μm,喷雾造粒的颗粒尺寸为17 μm,晶粒尺寸为100 nm,BET=26.66 m2/g.粉末和陶瓷体材料为面心立方结构.高于1 400 ℃烧结陶瓷体的烧结密度大于98%理论密度.陶瓷体电导率的测定结果表明,在1 400～1 600 ℃之间烧结,对材料的电导率影响不明显.2Yb-8YSZ具有高的离子电导率,操作温度大于600 ℃下的电导率达1×10-3 S/m.2Yb-8YSZ材料完全适用于作中温固体氧化物燃料电池(SOFC)的电解质.     

YSZ纳米粉料流延成型电解质薄膜性能研究

探索了以YSZ纳米粉体为原料,采用流延成型的方法制备YSZ电解质薄膜的工艺过程,具体探讨了不同粒度粉体流延后坯体的性能,结果表明,纳米范围内颗粒粒度粗可以获得致密度较高的坯体。但在烧结过程中,细粒度粉料表现出更好的性能,实验制备的YSZ电解质薄膜的面积比电阻在1123K,比德国D样品大幅度下降。573～1023K的阻抗谱显示出实验制备的YSZ电解质试样的晶粒、晶界和电极处的阻抗都明显降低,综合性能明显优于国外同类产品。流延成型工艺可以获得尺寸为100mm×100mm×0.125mm的8YSZ电解质薄片,这为平板式SOFC在中国的快速发展做好了材料上的准备。     

Ion conducting properties of hydrogen-containing Ta2O5 thin films prepared by reactive sputtering

Hydrogen-containing Ta₂O₅ (Ta₂O₅:H) thin films are considered to be a candidate for a proton-conducting solid-oxide electrolyte. In this study, Ta₂O₅:H thin films were prepared by reactively sputtering a Ta metal target in an O₂ + H₂O mixed gas. The effects of sputtering power and post-deposition heat treatment on the ion conducting properties of the Ta₂O₅:H thin films were studied. The ionic conductivity of the films was improved by decreasing the RF power and a maximum conductivity of 2 × 10⁻⁹ S/cm was obtained at an RF power of 20 W. The ionic conductivity decreased by heat-treatment in air, and no ion-conduction was observed after treatment at 300 °C due to the decrease in hydrogen content in the films.     

Structural, electrical, and optical properties of copper indium diselenide thin film prepared by thermal evaporation method

Stoichiometric compound of copper indium diselenide (CuInSe₂) was synthesized by direct reaction of high-purity elemental copper, indium and selenium in an evacuated quartz ampoule. The phase structure and composition of the synthesized pulverized material analyzed by X-ray diffraction (XRD) and energy dispersive analysis of X-rays (EDAX) revealed the chalcopyrite structure and stoichiometry of elements. Thin films of CuInSe₂ were deposited onto organically cleaned soda lime glass substrates held at different temperatures (i.e. 300 K to 573 K) using thermal evaporation technique. CuInSe₂ thin films were then thermally annealed in a vacuum chamber at 573 K at a base pressure of 10^− 2 mbar for 1 h. The effect of substrate temperature (T_s) and thermal annealing (T_a) on structural, compositional, morphological, optical and electrical properties of films were investigated using XRD, transmission electron microscopy, EDAX, atomic force microscopy (AFM), optical transmission measurements and Hall effect techniques. XRD and EDAX studies of CuInSe₂ thin films revealed that the films deposited in the substrate temperature range of 423-573 K have preferred orientation of grains along the (112) plane and near stoichiometric composition. AFM analysis indicates that the grain size increases with increase of T_s and T_a. Optical and electrical characterizations of films suggest that CuInSe₂ thin films have high absorption coefficient (10⁴ cm^− 1) and resistivity value in the interval 10^− 2-10¹ Ω cm influenced by T_s and T_a.     

钨精矿粉掺杂Fe-Al合金激光引燃自蔓延合金组织及性能

在钨精矿粉质量分数为1%前提下, 通过改变Al原子分数, 分别为50%、 60%、 70%、 80%, 对其粉末进行压制, 进而将压坯激光点火, 使其发生自蔓延合成反应生成Fe-Al合金, 利用XRD、 SEM、 EDX、 硬度测试、 磨损测试等表征手段, 分析研究了掺杂定量的钨精矿粉后, 不同Fe、 Al配比对烧结Fe-Al合金微观组织结构及宏观性能的影响。结果表明: 在烧结过程中, 压坯实现了自蔓延烧结。产物物相主要为AlFe、 AlFe₃、 WO₃、 AlCrFe₂等, 且随着Al含量的增加, 形成了富Al相。烧结Fe-Al合金组织随着Al含量的增加, 伴随微小裂纹产生。当Al含量达到60%时, 烧结Fe-Al合金显微硬度最大, 达到HK1053; 磨损率最低, 为0.04 mg·mm^-2。     

Structural and optical properties of Ti-doped ZnO thin films prepared by the cathodic vacuum arc technique with different annealing processes

Highly transparent Ti-doped ZnO thin films were prepared on glass substrates at a deposition rate of approximately 33 nm/min using the cathodic vacuum arc technique with a Zn target power of 550 W and a Ti target power of 750 W, respectively. X-ray diffraction measurements have shown that the Ti-doped ZnO thin film with a vacuum post-annealing condition is c-axis oriented but an amorphous phase at the other post-annealing atmosphere and as-deposited condition. Transmittance measurements show that the best optical quality of the Ti-doped ZnO thin films occurred at a post-annealing atmosphere of N₂/H₂ mixed gases. Additionally, the optical transmittance of all films has been found more than 85% in a range of 500-700 nm. The lowest electrical resistivity was 3.48 × 10⁻³ Ω cm, obtained on as-deposited films. However, the post-annealing condition greatly increased the resistivity.     

Structural and optical properties of indium tin oxide (ITO) thin films with different compositions prepared by electron beam evaporation

Tin-doped Indium oxide thin films in different compositions (Sn = 0,5,10,15,20 at.wt%) were prepared on glass substrates at the substrate temperature of 250 °C in an oxygen atmosphere by electron beam evaporation. The structural and morphological studies were carried out by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The grain size of the ITO films decreased when increasing the dopant concentration of Sn in the In₂O₃ lattice. Optical properties of the films were studied in the UV-Visible-NIR region (300-1000 nm). The optical energy band gap (E_g), as determined by the dependence of the absorption coefficient on the photon energy at short wavelengths was found to increase from 3.61 to 3.89 eV revealing the ascending loading profile of dopant concentration. Optical Parameters, such as absorption depth, refractive index (n), extinction coefficient (k), packing density, porosity, dispersion energy and single effective oscillator energy were also studied to show the composition dependence of tin-doped indium oxide films.     

1.7MeV电子束在VO2热致相变薄膜中引起的结构和光电性能的变化

利用能量为1.7MeV,注量分别为10^13-10^15/cm^2的电子辐照VO2薄膜,采用XPS,XRD等测试手段对电子辐射前后的样品进行分析,并采用光透射性能和电光性能测试研究了电子辐照对样品相变过程中光电性能的影响,结果表明电子辐照在VO2薄膜中出现变价效应,产生新的X射线衍射峰,带来薄膜化学成分的变化,电子辐照在样品中产生的这些变化对VO2的热致相变特性有明显影响。     

Study of structural, electrical, optical, thermoelectric and photoconductive properties of S and Al co-doped SnO2 semiconductor thin films prepared by spray pyrolysis

In this paper, the effect of S and Al concentrations on the structural, electrical, optical, thermoelectric and photoconductive properties of the films was studied. The [Al]/[Sn] and [S]/[Sn] atomic ratios in the spray solutions were varied from 10 at.% to 40 at.% and 0 to 50 at.%, respectively. X-ray diffraction analysis showed the formation of SnO₂ cassiterite phase as a main phase and the numerous sulfur phases including S, SnS, SnS₂ and Sn₂S₃ in SnO₂:Al films. Scanning electron microscopy studies showed that in the absence of S, increasing the Al content results in a smaller grain size and with the addition of S, the films appear to contain small cracks and nodules. The minimum resistance of 0.175 (kΩ/□) was obtained for S-doped SnO₂:Al (40 at.%) film with 20 at.% S-doping. From the Hall effect measurements, the majority carrier concentration was obtained in order of 10¹⁷-10¹⁸ cm^− 3. The thermoelectric measurements showed that majority carriers change from electrons to holes for S-doping in SnO₂:Al (40 at.%) thin films. The maximum Seebeck coefficient of + 774 μV/K (at T = 370 K) was obtained for S-doped SnO₂:Al (10 at.%) film with 50 at.% S-doping. The band gap values were obtained in the range of 3.8-4.2 eV. The S-doped SnO₂:Al (40 at.%) films have shown considerably photoconductivity more than S-doped SnO₂:Al (10 at.%) with increasing S-doping. The best photoconductive property was obtained for co-doped SnO₂ thin film with 40 at.% Al and 5 at.% S concentration in solution.