低温烧结LED基板用Ca-Ba-Mg-Al-B-Si-O 玻璃/Al2O3材料的性能研究

实验以Ca-Ba-Mg-Al-B-Si-O玻璃与Al_2O_3粉料为原料,设计玻璃与Al_2O_3粉料复合的质量比分别为60∶40、55∶45、50∶50、45∶55,采用低温烧结法制备LED基板材料。研究结果表明:随着Al_2O_3含量(质量分数)增加,样品的烧成收缩率与热导率先增加后减小。添加45%Al_2O_3的玻璃/Al_2O_3材料于875℃烧结良好,试样烧成收缩率为12.82%,体积密度为3.10 kg/L,10 MHz下介电常数为8.03,介电损耗为0.000 7,热导率为2.89 W/(m·K)。高温下Ca~(2+)离子、Al~(3+)离子、Si~(4+)离子与O~(2-)离子聚集在一起发生了化学反应,形成了CaAl_2Si_2O_8晶体。玻璃/Al_2O_3烧结材料的主晶相为玻璃、氧化铝、钙长石,SEM显示烧结体微观结构致密。因此该体系材料比较适合用作低温烧结LED基板材料。     

SiO_2对Ca-Ba-Mg-Al-B-Si-O玻璃/Al_2O_3材料烧结与介电性能的影响

以Ca-Ba-Mg-Al-B-Si-O系玻璃和α-Al_2O_3粉料为原料,低温烧结玻璃/Al_2O_3系介电陶瓷材料。设计调控基质玻璃中SiO_2含量,以优化Ca-Ba-Mg-Al-B-Si-O玻璃复合氧化铝材料的烧结与介电性能。结果表明,提高SiO_2含量,玻璃/Al_2O_3材料的烧成收缩率降低,试样烧结温度升高,烧结体介电常数先增加后减小,介电损耗先减小后增加,介电性能转折点出现在SiO_2含量为60 wt%。当SiO_2含量为60 wt%时,复合材料综合性能最好,试样在875℃烧结致密,体积密度为3.10 g·cm~(-3),10 MHz频率下介电常数为8.03,介电损耗为0.0005,因此该体系材料比较适合用作LTCC封装材料。     

Ca-Ba-Mg-Al-B-Si-O玻璃/Al2O3系LED基板材料的工艺优化与性能研究

实验以玻璃与Al2O3为主要原料流延成型生瓷带,通过优化试样的压制工艺,800～950℃范围内烧结得到Ca-Ba-Mg-Al-B-Si-O玻璃/Al2O3材料。研究结果表明,随着Ca-Ba-Mg-Al-B-Si-O玻璃/Al2O3生坯压制压力变大或保压时间增加,玻璃/Al2O3材料的生坯及烧结试样的密度增加,烧成收缩率减小。850℃烧成试样结构致密,钙离子、铝离子、硅离子与氧离子在高温下聚集,并发生了物理化学反应,生成钙长石晶体,进一步促进了烧成试样的致密化。Ca-Ba-Mg-Al-B-Si-O玻璃/Al2O3材料在压力20 MPa,保压时间10 min下成型生坯性能良好,烧结体物理性能优良,适合用于LED基板材料。     

Al_2O_3颗粒级配对Ca-Ba-Mg-Al-B-Si-O玻璃/Al_2O_3系LTCC材料性能的影响

以Ca-Ba-Mg-Al-B-Si-O系玻璃和D_(50)分别为0.83μm与3.49μm的Al_2O_3粉料为原料,采用低温烧结法制备了玻璃/Al_2O_3系介电陶瓷材料。设计将两种氧化铝按一定配比混合以优化氧化铝颗粒级配,研究了氧化铝颗粒级配和烧成温度对玻璃/Al_2O_3材料的烧结性能、介电性能和力学性能的影响。随着氧化铝颗粒级配的优化,玻璃/Al_2O_3材料的收缩率、体积密度、相对介电常数、抗弯强度增加,而介电损耗减小。添加D_(50)为2.81μm的Al_2O_3混合粉料的玻璃/Al_2O_3材料于875℃烧结良好,显示出优异的性能:体积密度为3.09 g/cm~3,相对介电常数7.78,介电损耗0.53×10~(-3)(于10 MHz下测试),抗弯强度为181 MPa,因此该体系材料比较适合用作LTCC封装材料。     

不同成核剂对Na_2HPO_4·12H_2O相变过冷性能的影响

以Na_2HPO_4·12H_2O作为相变材料,研究不同的成核剂对其过冷度的影响。结果显示,Na_2B_4O_7·10H_2O、Na_2SiO_3·9H_2O、Al_2O_3都能有效减低其过冷度,其中Al_2O_3效果最好,2%的Al_2O_3可以将Na_2HPO_4·12H_2O的过冷度降低至2.2℃,同时可延长放热时间。多次循环实验显示,添加2%Al_2O_3的Na_2HPO_4·12H_2O的相变温度和相变潜热变化很小,稳定性较好。     

不同成核剂对Na_2HPO_4·12H_2O相变过冷性能的影响

以Na_2HPO_4·12H_2O作为相变材料,研究不同的成核剂对其过冷度的影响。结果显示,Na_2B_4O_7·10H_2O、Na_2SiO_3·9H_2O、Al_2O_3都能有效减低其过冷度,其中Al_2O_3效果最好,2%的Al_2O_3可以将Na_2HPO_4·12H_2O的过冷度降低至2.2℃,同时可延长放热时间。多次循环实验显示,添加2%Al_2O_3的Na_2HPO_4·12H_2O的相变温度和相变潜热变化很小,稳定性较好。     

K2O含量对B2O3-Al2O3-Na2O玻璃结构及物理性能的影响

选取B_2O_3-Al_2O_3-Na_2O三元玻璃系统,研究改变玻璃系统中K_2O的含量对硼酸盐低熔点封接玻璃性能的影响。通过XRD、DTA等手段对玻璃样品的膨胀系数、转变温度、软化温度、电阻率、介电常数等性能进行了测试。结果表明:在B_2O_3-Al_2O_3-Na_2O三元玻璃系统中,随着K_2O含量的增加,硼酸盐玻璃的膨胀系数呈先下降后上升的趋势,在K_2O含量位于5 mol%左右时,硼酸盐玻璃的膨胀系数小幅下降,这是硼反常现象的体现。K_2O含量在7～8 mol%左右时,膨胀系数出现最低值。玻璃的体积电阻率和介电常数的变化也存在着硼反常现象,随着K_2O含量的增加,均呈现先下降再上升后又下降的趋势。玻璃的转变温度T_g和软化温度T_f的变化趋势基本一致,均呈现先下降后上升再下降的趋势。     

K_2O-Al_2O_3-WO_3三元系中Al_2(WO_4)_3-K_2O和Al_2(WO_4)_3_K_2WO_4截面的相平衡研究

用DTA和XRD方法研究了K_2O-Al_2O_3-WO_3三元系中Al_2(WO_4)_3-K_2O和Al_2(WO_4)_3-K_2WO_4截面相平衡关系。在Al_2(WO_4)_3-K_2O赝二元系中由包晶反应形成三个化合物:2Al_2(WO_4)_3·K_2O_4、Al_2(WO_4)_3·K_2O和Al_2(WO_4)_8·3K_2O。其包晶反应温度分别为937±3℃、786±3℃和902±3℃。在Al_2(WO_4)_3-K_2WO_4截面中,33.3mol%K_2WO_4和50mol%K_2WO_4组份其主要成份分别为2Al_2(WO_4)_3K_2O和Al_2(WO_4)_3K_2O。     

蜡石砖中杂质含量对高温性能的影响

为了研究蜡石砖中杂质含量对其性能的影响,对不同K_2O、Na_2O、Al_2O_3含量的蜡石砖样品进行了对比研究。结果表明:随着蜡石砖中杂质K_2O+Na_2O和Al_2O_3含量的增加,其抗折强度增大,耐火度、荷重软化温度以及抗渣侵蚀性能等均大幅下降。因此,在作为电炉钢包等高温容器的工作层使用时,蜡石砖中K_2O+Na_2O必须控制在0.6%(w)以下。而Al_2O_3的含量控制范围以及其对蜡石砖高温性能的影响还需进一步研究。     

Al2O3对R2O-CaO-SiO2-F系废渣微晶玻璃析晶与性能的影响

以花岗岩废渣为主要原料,用熔融法制备了R_2O-CaO-SiO_2-F系微晶玻璃。采用差示扫描量热法、X射线衍射、扫描电子显微镜等测试方法研究了Al_2O_3含量对RO-CaO-SiO_2-F系微晶玻璃的析晶与性能的影响。结果表明:随着Al_2O_3含量的增加,硅碱钙石与硬硅钙石晶体细化;Al_2O_3含量(质量分数)为6.0%的基础玻璃经560℃核化2 h、910℃晶化2 h后的主晶相为硅碱钙石,其抗弯强度和断裂韧性分别为(154±20)MPa、(2.37±0.12)MPa·m~(-1/2);当Al_2O_3含量增加至6.5%时,硅碱钙石减少、氟化钙增多,力学性能降低。     

Na2O-Al2O3-Fe2O3系烧结过程中铝、铁的反应行为

以Al2O3, Fe2O3和Na2CO3为原料,对Na2O-Al2O3-Fe2O3系烧结过程中的反应行为进行了详细研究. 基于溶出率与时间、温度的关系,证明Na2O×Al2O3和Na2O×Fe2O3的生成反应动力学都服从Zhuralev-Lesokin-Tempelman模型,表观活化能分别为186.59和80.92 kJ/mol,表明Na2O×Fe2O3比Na2O×Al2O3在动力学上更易形成;Al2O3易与Na2O×Fe2O3反应形成Na2O×Al2O3和Fe2O3,在1273 K烧结30 min,所得熟料Al2O3溶出率达98.51%;Fe2O3对Na2O×Al2O3的形成有双重作用,在1273 K下可加速Na2O×Al2O3的形成,超过1323 K,促使Na2O×Al2O3分解成Na2O和b-Al2O3,且随着温度升高或时间延长,分解程度增高,从而导致熟料中Al2O3溶出率显著降低.     

钕-铝系稀土色料的研制

通过钕-铝系列色料合成实验,分析不同配比及不同矿化剂等对色料呈色效果的影响,确定最佳工艺方法。对实验结果进行XRD及色度分析,确定其主晶相为钕酸铝,试样的明度均在70以上,色彩鲜艳亮丽。     

TNT的O3/H2O2降解规律

利用自制装置,采用连续投加O3、H2O2的方式,研究了O。／H：O：对废水中TNT的降解规律。结果表明,与Oa作用相比,O3／H2O2工艺可显著提高TNT的降解率,还可避免中间产物的形成与积累;在试验研究条件下,H2O2：O3的最优摩尔比为1,最佳初始pH值在11左右,利用缓冲溶液可维持反应体系pH值的稳定,但不利于O3／H2O2功效的发挥,反应适合在常温下进行,尽量避开40℃左右;动力学特征分析表明,O／H2O2降解TNT偏离伪一级反应动力学规律。     

UV-Enhanced Exchange of O2with H2O Adsorbed on TiO2

Ultraviolet light dramatically increases the rate of isotope exchange between gas-phase O₂and water adsorbed on TiO₂at room temperature, but it does not affect the rate of CO₂–water exchange. Both ethanol and acetaldehyde, when coadsorbed with H₂¹⁸O, dramatically decrease the rate of O₂exchange, but not CO₂exchange, with adsorbed H₂¹⁸O. This decrease is attributed to a combination of competition for adsorbed oxygen between exchange and photocatalytic oxidation of the adsorbed organic and blocking of the oxygen adsorption sites by the organic. The same oxygen species participate in O₂-H₂¹⁸O exchange and photocatalytic oxidation.     

Properties of RO-Y2O3-Al2O3-SiO2 glasses

The coefficient of linear expansion, glass-transition temperature, temperature at the orset of deformation (strain point), density. Young modulus, microhardness, crystallizability, and contact angle are studied as a function of the composition in RO–Y₂O₃–Al₂O₃–SiO₂ (R=Ca and/or Mg) glass systems. The composition ranges for glasses (with strain point >900°C and coefficient of linear expansion of (32–45)×10^–7°C^–1) that can be used for soldering silicon-nitride ceramics were established.Translated from Steklo i Keramika, No. 12, pp. 5–7, December, 1996     

Fe2O3-MnO-Cr2O3-La2O3系统紫色颜料的制备及表征

采用溶胶均匀共沉淀法于低温下合成了含少量稀土氧化物La2O3的紫色颜料，并采用颜色测定、SEM、XRD等手段对颜料的颜色、检度及结晶构造等进行了表征。     

Phase equilibrium in binary La2O3-Dy2O3 and ternary CeO2-La2O3-Dy2O3 systems

Cerium oxide doped with oxides of rare earth elements is a multifunctional material, a wide range of uses which is associated with its unique physicochemical properties. Phase diagrams of multicomponent systems are the physicochemical basis for the creation of new materials with improved characteristics.In this work, phase equilibria in ternary CeO₂–La₂O₃–Dy₂O₃ and binary La₂O₃–Dy₂O₃ systems in the whole concentration range were studied. No new phases have been identified in these systems. An isothermal section of the phase diagram of the CeO₂–La₂O₃–Dy₂O₃ system at a temperature of 1500 °С is constructed. No new phases have been detected in the system. It was found that in the studied ternary system solid solutions are formed on the basis of (F) modification of CeO₂ with structure of fluorite type, monoclinic (B), cubic (C) and hexagonal (A) modifications of Ln₂O₃.In the La₂O₃–Dy₂O₃ binary system (1500–1100 °С) three types of solid solutions are formed: based on hexagonal modification A-La₂O₃, monoclinic modification B-Dy₂O₃ and cubic modification C-Dy₂O₃ separated by two-phase fields (A+B) and (B+C), respectively. The boundaries of the regions of homogeneity of solid solutions based on A-La₂O₃ are determined by compositions containing 35–40, 20–25, 15–20 mol% Dy₂O₃ at 1500, 1250, 1100 °C, respectively. From the obtained data it follows that the solubility of Dy₂O₃ in the hexagonal modification of lanthanum oxide is 39 mol% at 1500 °C, 23 mol. % at 1250 °C and 16 mol% at 1100 °C. The limits of existence of solid solutions based on monoclinic B-modification are determined by compositions containing 30–35, 65–60 (1250 °С), 35–40, 55–60 (1100 °С) 40–45, 70–75 (1500 °C) mol% Dy₂O₃.In the studied system, with a decrease in temperature from 1500° to 1100°C, there is a decrease in the solubility of La₂O₃ in the crystal lattice of cubic solid solutions of C-type from 16 to 10 mol%.     

Polycrystalline In2O3 and In2O3/Y2O3 photoanodes

Single crystal In₂O₃ shows promise as a photoanode for the decomposition of water. Because of various difficulties in the preparation of the single crystal material, two simple techniques were developed for the preparation of polycrystalline In₂O₃ anodes. One method involves the thermal decomposition of the nitrate while the other utilizes the chemical vapour deposition technique. Voltammograms and photoresponse spectra of these anodes are compared to the single crystal material. Among other observations, it is noted that the quantum efficiencies of the thermally decomposed films are comparable to the single crystal material. It is also shown that the on-set potential can be shifted to more negative values by forming the mixed oxide In₂O₃/Y₂O₃.