改善硼硅基质荧光玻璃发光性能的方法

制备了Na_2O-B_2O_3-SiO_2-ZnO-BaO的基质玻璃,该基质玻璃光学性能良好,透光率高,色泽纯净透明。使用基质玻璃与荧光粉共烧结,打磨至1mm可以得到荧光玻璃样品。发现共烧结30min时荧光玻璃有最大的发光强度,烧结时间过长破坏荧光粉的物理结构,烧结时间过短无法获得较好的光学性能。荧光粉含量(质量百分比)为3%时荧光玻璃发射强度最大,荧光粉过少时光转换效率低,荧光粉过多时出现浓度猝灭效应。使用碳粉还原性气氛烧结最大可以获得425%的发光效率提升。     

钢渣基高碱度微晶玻璃的一步法制备及工艺参数研究

为了提高微晶玻璃原料中高钙冶金渣的掺量,需要制备出碱度更高的微晶玻璃. 本文采用一步法,以钢渣为主要原料,制备碱度( CaO与SiO2的质量比)为0. 9的钢渣基高碱度微晶玻璃. 通过X射线衍射分析、扫描电镜和性能测试等手段,研究热处理条件对微晶玻璃微观形貌及线收缩率、体积密度和抗折强度等性能的影响规律. 研究表明,高碱度微晶玻璃适合采用一步法制备工艺,当在1100℃保温120 min时,微晶玻璃烧结过程基本完成,此时获得最大体积密度2. 4 g·cm-3 ,最高抗折强度56. 4 MPa. 微晶玻璃的主晶相为钙铝黄长石,副晶相为辉石. 基础玻璃颗粒在升温过程中完成了成核和析晶过程,而在保温过程中主要进行的是基础玻璃颗粒的烧结致密化和晶体的进一步发育. 升温至1100℃保温30 min,微晶玻璃的抗折强度超过45 MPa,微晶玻璃内部晶体呈方柱状交织排列并构成晶体骨架分布在残余的玻璃基体中;随着保温时间的增加,微晶玻璃的线性烧结收缩率、体积密度和抗折强度均逐渐增大,而晶相的含量基本保持不变,晶体逐渐由球形颗粒状和短柱状发育为长柱状. 晶体的形状以及与残余玻璃相构成的整体致密结构是导致高碱度微晶玻璃力学性能提高的主要因素.     

玻璃组成对CaO-Al2O3-SiO2系玻璃烧结、晶化和性能的影响

采用烧结法制备以钙长石为主晶相的微晶玻璃.采用差热分析(DTA)、X射线衍射(XRD)、扫描电镜(SEM)和性能测试研究玻璃组成对玻璃的烧结、晶化特性和性能的影响.结果表明:随着CaO含量的增加,玻璃转变温度和析晶放热峰温度逐渐降低,而且析晶放热峰变得尖锐;增加氧化钙降低玻璃的析晶活化能,有利于玻璃的析晶;随着SiO2量的增加,玻璃转变温度和析晶放热峰温度移向高温,使玻璃的析晶困难;玻璃样品的烧结温度随CaO含量的增加而降低, 但过多的CaO促进硅酸钙的析出,增加样品的介电常数和热膨胀系数;增加SiO2能够降低微晶玻璃样品的热膨胀系数,改善其介电性能;所制备的微晶玻璃具有相对密度高(≥98.3%),介电常数适中(6.9～7.5),介电损耗低(≤0.1%),热膨胀系数低(3.8×10-6～4.5×10-6 /℃),烧结温度(900～1 000 ℃)低,及介电常数温度稳定性低(66×10-6～113×10-6 /℃).     

玻璃导体中两种阳离子共存时的特殊现象

玻璃导体中一价阳离子含量的多少,对玻璃电导率的影响极大。有趣的是当在玻璃导体中含有两种一价阳离子时,电导率反而比仅含一种阳离子时低很多。笔者通过对0.5[XNa_2O-(1-X)Li_2O]—0.5P_2O_5系列玻璃的制备和测量获得该系列玻璃的转变温度T_g、电导率σ_T、激活能E_a和指数前项σ_0随两种碱金属氧化物Na_2O和Li_2O含量变化的基本规律。     

山西翼城高炉渣在微晶玻璃中的应用

以山西翼城高炉矿渣为主要原料,采用烧结法制备微晶玻璃.利用差热分析仪(DTA)、扫描式电子显微镜(SEM)、X射线粉末衍射仪(XRD),研究矿渣微晶玻璃的成分、制备工艺,以及对显微结构和性能等进行分析.研究结果表明,当基础玻璃化学组成(质量分数)分别为50%～60%(SiO2),4%～8%(Al2 O3),14%～19%(CaO),7%～10%(MgO),0.7%(Fe2O3),4%(Na2O),6%(K2O)时,主晶相为透辉石,高炉渣最大引入量达到47.35%,最小量为28.06%,可以获得性能良好的烧结型微晶玻璃.     

Y-Al-Si-O-C氧碳玻璃的研制

以SiO2,Al2O3,Y2O3,α-SiC粉体为原料,采用粉末烧结法,于1550℃～1650℃无压烧结2hr.,研制Y-Al-Si-O-C氧碳玻璃.结果表明在1650℃×2h.的烧结条件下,在元素质量百分比为(wt%)Y(15.75)-Al(5.29)-Si(28.82)-O(49.14)-C(1.00)和Y(15.75)-Al(5.29)-Si(29.60)-O(47.36)-C(2.00)的两个成份点可获得氧碳玻璃.     

Al2O3对硼硅酸铅钙系玻璃性能的影响

用熔融法制备CaO-PbO-B2O3-SiO2系玻璃,以低温共烧法制备玻璃烧结体,研究不同Al2O3含量和烧成温度对玻璃的烧结性能和电性能的影响.结果表明:随着Al2O3含量的增加,玻璃的玻璃化转变温度升高,介电常数增加,介电损耗增加;X线衍射分析(XRD)显示G1玻璃在800℃析出CaSiO3和β-SiO2;G1玻璃于725℃保温30 min烧结,于10 MHz测试,介电常数(εr)=6.1,介电损耗(tanδ)=5.9×10-4;该玻璃有较低的玻璃化转变温度(tg=697.1℃)、较差的析晶能力、较低的介电损耗,适合作为低温共烧陶瓷(LTCC)的玻璃料使用.     

废液晶屏玻璃基板浮选分离与微晶化利用

针对废液晶屏玻璃基板分离困难与后续资源化利用的问题 ,提出热处理-浮选高效分离玻璃颗粒,后进一步采用烧结法制备微晶玻璃材料。发现当热处理温度为200℃时,液晶屏释放气态挥发物较少,同时热处理后浮选效率达到了93%。将得到的高纯度玻璃基板颗粒和普通废玻璃作为原料制备微晶玻璃,在最佳原料配比(废液晶显示屏玻璃基板30%,废玻璃26%),烧结温度1140℃,时间120 min条件下,烧结出的微晶玻璃具有致密度高、抗弯强度好、耐侵蚀性强的特点。     

氧化铋对低温燃烧合成堇青石粉相变和烧结性能的影响

为研究Bi2O3在堇青石基微晶玻璃烧结过程中的作用及其添加量对微晶玻璃相转变和烧结性能的影响,以硅酸、硝酸铝、硝酸镁为原料,尿素为燃料,用低温燃烧法制备了具有不同Bi2O3含量的堇青石基微晶玻璃,并对其进行了X射线衍射分析、显微分析和能谱分析.结果表明:添加Bi2O3能明显促进μ-堇青石向α-堇青石的相转变或促进α-堇青石相直接析晶,降低α-堇青石相的析出温度(由1 050℃降至900℃),有效促进微晶玻璃的烧结致密化;Bi2O3的添加量以质量分数5%左右为宜.此外,介绍了一种简便快捷地制备堇青石基微晶玻璃的新方法.     

Y—Al—Si—O—C氧碳玻璃的研制

以SiO_2,Al_2O_3,Y_2O_3,α-SiC粉体为原料,采用粉末烧结法,于1550℃～1650℃无压烧结2hr.,研制Y-Al-Si-O-C氧碳玻璃。结果表明:在1650℃×2h.的烧结条件下,在元素质量百分比为(wt％)Y(15.75)-Al(5.29)-Si(28.82)-O(49.14)-C(1.00)和Y(15.75)-Al(5.29)-Si(29.60)-O(47.36)-C(2.00)的两个成份点可获得氧碳玻璃。     

Microstructure and electrical conductivity of 10% Yb-doped SrCeO3 ceramics

As a candidate material for hydrogen separation, Yb-doped SrCeO₃ has attracted increasing attention in recent decades. In the present study, Yb-doped SrCe_0.9Yb_0.1O_3-α ceramics were prepared by the dry pressing and sintering approach, with the microstructure evolution and the micro morphology investigated. It was indicated that the ceramics sintered in air were of a pure perovskite structure, and that the sintering temperature had a significant effect on the growth of ceramic grains. The average grain size increased from 1 ​μm to 10 ​μm with an increase in sintering temperature from 1300 to 1500 ​°C. Further investigation of the thermodynamics and kinetics of grain growth revealed that the grain boundary diffusion was the main driving force of grain growth during solid phase sintering, with a grain growth index of 4 and an activation energy of approximately 61.23 ​kJ ​mol⁻¹. These results illustrate an obvious tendency of grain size growth. By electrochemical workstation with different atmospheres the effects of sintering temperature on the conductivity were characterized in the temperature range of 700–900 ​°C. The electrical conductivities σ of SrCe_0.9Yb_0.1O_3-α ceramics in different atmospheres were as follows: σ(wet hydrogen) ​> ​σ(dry hydrogen) ​> ​σ(dry air) ​> ​σ(wet air). In the test atmosphere containing water and hydrogen the conductivity of protons increased with increasing temperature because of the protons jump between lattices in the form of interstitial hydrogen ions or bare protons.     

养护温度对LiNO3抑制碱硅酸反应及其膨胀的影响

研究了38℃和60℃下石英玻璃在掺LiNO_3的Na OH溶液中碱硅酸反应过程,采用酸化处理法确定体系中SiO_2分布,采用等离子发射光谱(ICP)分析溶液中Na、Si和Li元素浓度变化,采用X射线衍射(XRD)和扫描电子显微镜(SEM)表征反应产物的组成和形貌;并检测了38℃和80℃湿气养护下掺LiNO_3的沸石化珍珠岩混凝土微柱的膨胀性。结果表明:加入LiNO_3降低了溶液中石英玻璃的溶蚀率和SiO_2的溶解度,减缓了ASR的反应速率;不同养护温度下形成的含锂产物不同,提高温度有利于Li_2SiO_3晶体的形成。对于混凝土微柱,掺锂试件早期抑制效果良好,后期仍膨胀;相同锂掺量下80℃湿气养护的试件膨胀率却明显低于38℃时的膨胀率。可见,高温养护下LiNO_3抑制ASR膨胀的效果不能很好地评价在低温下的作用效果。     

Preparation, crystallization, and wetting of ZnO-Al2O3-B2O3-SiO2 glass-ceramics for sealing to Kovar

A novel type of ZnO-Al₂O₃-B₂O₃-SiO₂ glass-ceramics sealing to Kovar in electronic packaging was developed, whose thermal expansion coefficient and electrical resistance are 5.2×10-6/℃ and over 1×1013 Ω·cm, respectively. The major crystalline phases in the glass-ceramic seals were ZnAl₂O₄, ZnB₂O₄, and NaSiAl₂O₄. The dielectric resistance of the glass-ceramic could be remarkably enhanced through the control of alkali metal ions into crystal lattices. It was found that crystallization happened first on the surface of the sample, leaving the amorphous phase in the inner, which made the glass suitable for sealing. The glass-ceramic showed better wetting on the Kovar surface, and sealing atmosphere and temperature had great effect on the wetting angle. Strong interracial bonding was obtained, which was mainly attributed to the interracial reaction between SiO₂ and FeO or Fe₃O₄.     

Synthesis of glass ceramics from kaolin and dolomite mixture

Cordierite-and anorthite-based binary glass ceramics of the CaO-MgO-Al₂O₃-SiO₂ (CMAS) system were synthesized by mixing local and abundant raw minerals (kaolin and doloma by mass ratio of 82/18). A kinetics study reveals that the activation energy of crystallization (Ea) calculated by the methods of Kissinger and Marotta are 438 kJ·mol-1 and 459 kJ·mol-1, respectively. The Avrami parameter (n) is estimated to be approximately equal to 1, corresponding to the surface crystallization mechanism. X-ray diffraction (XRD) analysis shows that the anorthite and cordierite crystals are precipitated from the parent glass as major phases. Anorthite crystals first form at 850℃, whereas the μ-cordierite phase appears after heat treatment at 950℃. Thereafter, the cordierite allotropically transforms to α-cordierite at 1000℃. Complete densification is achieved at 950℃; however, the density slightly decreases at higher temperatures, reaching a stable value of 2.63 kg·m-3 between 1000℃ and 1100℃. The highest Vickers hardness of 6 GPa is also obtained at 950℃. However, a substantial decrease in hardness is recorded at 1000℃; at higher sintering temperatures, it slightly increases with increasing temperature as the α-cordierite crystallizes.     

Effect of sintering temperature on the electrolysis of TiO2

The effects of sintering temperature on the microstructure and the conductivity of TiO₂ cathodes were studied by examining the phase composition, microstructure, and element contents of the sintered cathodes and the cathodic products using X-ray diffraction and scanning electronic microscopy-energy dispersive spectrometry. The oxygen vacancy, conductivity, average pore diameter, and specific surface area of the sintered cathodes were detected by X-ray photoelectron spectroscopy, four-point probe, and ASPA 2010. The results showed that TiO₂ phase transformations occurred, and oxygen vacancies formed with the increase of sintering temperature. The cathodic conductivity improved, but the average pore diameter and the effective response area of the TiO₂ cathode were reduced when the sintering temperature increased. These phenomena could weaken the contact between reaction ions and electrons and also had the same effect on the cathodes and the molten salt. Moreover, they were disadvantageous to ion migration, so a lower sintering temperature was favorable for the microstructure of electrolysis. Consequently, the cathodic conductivity may be improved, but the microstructure became compact with the increase of sintering temperature. The cathodic products at different temperatures indicated that the cathodic conductivity was more important for electrolysis.     

Lal／3Ndl／3Bal／aMn03的电阻率双峰和低温电阻率反常现象

用固相反应法制备了二元稀土掺杂的La1／3Ndl／3Ba1/3Mn03多晶庞磁电阻块材．x射线衍射分析表明在1200℃烧结的样品具有立方对称的晶格结构．热磁曲线显示材料在低温处于自旋冰状态．自旋冰的熔点随着外磁场的增大而降低．在磁场达到40kOe时,自旋冻结现象消失．材料的居里温度为-250K,但室温磁化曲线中出现由微弱不均匀品格畸变造成的寄生铁磁性行为．电阻率一温度曲线出现双峰现象．在居里温度附近出现的电阻率峰由晶体的本征特性贡献,在低于居里温度的～190K附近出现的电阻率峰由界面隧穿效应贡献．电阻率在～40K附近出现极小值．经过曲线拟合证实,其行为与近藤效应相似．研究结果较为全面地分析了单相多晶CMR材料的基本磁电相关特性．     

Sintering mechanism of Cu-9Al alloy prepared from elemental powders

The sintering behavior of Cu-9Al alloys prepared from die pressing of elemental powders was investigated. The experimental results and kinetic analysis showed the formation of three consecutive layers of Al₂Cu, Al₄Cu₉, and AlCu phases, with Al₂Cu appearing first in the initial solid phase sintering stage. A liquid phase formed in the intermediate stage, resulting from the eutectic reaction between Al and Al₂Cu phases at 500 °C, which is 47 °C lower than the equilibrium reaction temperature. Swelling occurred when the liquid phase infiltrated the gaps between the copper particles, leaving pores at the original sites of Al particles and Al₂Cu. In the final stage of sintering, the Al-rich phases (Al₂Cu and AlCu) transformed to Al-poor phases (Al₄Cu₉ and α-Cu) in the temperature range of 500–565 °C. Al₄Cu₉ and α-Cu then transformed to AlCu₃ (β) above the eutectoid reaction temperature (565 °C), whereas AlCu₃ transformed to α-Cu and eutectoid phases (α-Cu + Al₄Cu₉) during cooling. The pure copper transformed to AlCu₃, and the pore volume decreased at 1000 °C. The microstructure study helps manipulate precisely the sintering process of Cu-Al alloys and optimize the microstructure with a high dimensional accuracy.     

Effect of KNbO3 content on the crystal structure and electrical properties of (1 − x)PbZr0.54Ti0.46O3-xKNbO3 piezoelectric ceramics

(1 ? x)PbZr_0.54Ti_0.46O₃-xKNbO₃ (0 ≤ x ≤ 25mol%) (abbreviated as PZT-xKN) piezoelectric ceramics were successfully fabricated by a traditional sintering technique at 1225°C for 30 min. The influence of KNbO₃ content on the crystal structure and electrical properties of the PZT-xKN piezoelectric ceramics was studied. Samples with 0 ≤ x ≤ 0.20 show a pure perovskite structure, indicating that all KNbO₃ diffused into the crystal lattice of PZT to form a single solid solution in this compositional range. A second Pb₃Nb₄O₁₃ phase is observed in the PZT-0.25KN sample, showing that the maximum solid solubility of KNbO₃ in PZT matrix ceramic is less than 25mol%. Compared with pure PZT piezoelectric ceramics, samples containing KNbO₃ have smaller crystal grains. PZT-0.15KN exhibits excellent piezoelectric properties with d ₃₃ = 209 pC/N.     

Influence of catalyst on structural and morphological properties of TiO2 nanostructured films prepared by sol–gel on glass

Transparent TiO2 thin films have been prepared by the sol-gel method using titanium alkoxides as precursors.Thin films were deposited on glass supports by the dip-coating technique.The TiO2 layer acts as a self-cleaning coating generated from its photocatalysis and photoinduced superhydrophilicity.The crystalline structure of TiO2 films was dominantly identified as the anatase phase,consisted of uniform spherical particles of about 14-50 nm in size,which strongly depends upon catalyst-type and heat treatment temperature.Increasing heat treating temperature can lead to an increase in crystalline size.The results indicated that the sample S.S(sample derived from sol containing sulfuric acid as catalyst) exhibits superhydrophilic nature and better photocatalytic activity,which can be attributed to its higher anatase content and lower crystalline size.Morphological studies,carried out using Atomic Force Microscopy(AFM),confirm the presence of crystalline phase with such a grain size and low surface roughness.Thus,the applied films exhibiting high photocatalytic activity,superhydrophilic behavior,and low surface roughness can be used as an efficient self-cleaning coating on glass and other optical applications.     

Mechanism research on arsenic removal from arsenopyrite ore during a sintering process

The mechanism of arsenic removal during a sintering process was investigated through experiments with a sintering pot and arsenic-bearing iron ore containing arsenopyrite; the corresponding chemical properties of the sinter were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES), X-ray diffraction (XRD), and scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS). The experimental results revealed that the reaction of arsenic removal is mainly related to the oxygen atmosphere and temperature. During the sintering process, arsenic could be removed in the ignition layer, the sinter layer, and the combustion zone. A portion of FeAsS reacted with excess oxygen to generate FeAsO₄, and the rest of the FeAsS reacted with oxygen to generate As₂O₃(g) and SO₂(g). A portion of As₂O₃(g) mixed with Al₂O₃ or CaO, which resulted in the formation of arsenates such as AlAsO₄ and Ca₃(AsO₄)₂, leading to arsenic residues in sintering products. The FeAsS component in the blending ore was difficult to decompose in the preliminary heating zone, the dry zone, or the bottom layer because of the relatively low temperatures; however, As₂O₃(g) that originated from the high-temperature zone could react with metal oxides, resulting in the formation of arsenate residues.