Li2O-Al2O3-SiO2系统光敏微晶玻璃的制备

光敏微晶玻璃在电子、生物医药等领域应用前景非常广泛.本论文利用XRD和SEM技术,研究了热处理和光辐照条件对Li2O-Al2O3-SiO2系统微晶玻璃光敏性能的影响,在合理确定工艺制度的基础上,制备出了孔穴排列良好的光敏微晶玻璃.     

利用滑石制备微晶玻璃的工艺及其结构

研究了以滑石为主要原料制备Na2O-MgO-AI2 O3-SiO2系统微晶玻璃的工艺,探讨了成分对微晶玻璃的结构和性能的影响规律.结果表明:微晶玻璃的主晶相取决于MgO、Al2O3、SiO2 3种成分的比例关系,通过调整这3种氧化物的含量,可以得到以镁橄榄石、斜顽辉石以及它们混合物为主晶相的微晶玻璃.微晶玻璃的热处理工艺为1 000℃保温1～2 h.Fe2O3、TiO2和ZnO成分对微晶玻璃白度的影响较大,当试样中质量分数Fe2 O3＜0.1％,TiO2＜0.01％,ZnO为1％时,微晶玻璃的白度可达85,可以满足日用陶瓷的使用要求.     

热处理对CaO-Al2O3-SiO2系微晶玻璃性能影响

以CaO-A l2O3-SiO2为主要原料,采用烧结法制备出微晶玻璃.利用DSC确定了核化温度和晶化温度.利用XRD和SEM研究微晶玻璃的物相组成和显微结构.通过研究热处理温度对微晶玻璃性能的影响,可得出在780℃核化1h、948℃晶化2h时,微晶玻璃的性能最好.     

熔融法制备金矿尾砂微晶玻璃及性能测试

以金矿尾砂、方解石为主要原料,添加其它所需原料为硼砂、ZnO、Cr2O3、Sb2O3等,采用熔融法制备CaO-Al2O3-SiO2系微晶玻璃.利用硅碳棒炉在1 300℃~1 350℃下保温4h熔制玻璃,熔好的玻璃液浇注在事先预热的不锈钢模具上,成形后放入马弗炉在600℃保温1h退火处理,对玻璃试样热处理得到微晶玻璃样品.采用TG-DSC差热分析仪测定基础玻璃的DSC曲线,确定金矿尾砂微晶玻璃较佳的热处理工艺为:800℃保温2h进行核化处理,890℃保温3h进行晶化处理.通过XRD、SEM等分析手段对试样的物相及微观结构进行了分析,测定制得微晶玻璃的抗折强度、热膨胀系数、体积密度等性能.结果表明:制得金矿尾砂微晶玻璃的主晶相为:辉石和透辉石固溶体,样品的热膨胀系数为69.5×10-7/℃,抗折强度为119.2MPa,体积密度为2.81g/cm3.     

矿渣微晶泡沫玻璃核化及晶化制度的优化

目的 利用高炉矿渣、粉煤灰和废玻璃为原材料制备矿渣微晶泡沫玻璃，在确定微晶泡沫玻璃配方范围的基础上，对制备微晶泡沫玻璃的核化和晶化工艺参数进行了优化，使之具有轻质高强的优良性能．方法 采用粉末烧成法工艺和正交试验优化设计的试验手段．结果 严格控制核化及晶化工艺参数对制备具有较高抗压强度的矿渣微晶泡沫玻璃是十分必要的。晶化温度对微晶泡沫玻璃抗压强度影响显著，晶化温度不宜过高，否则材料的抗压强度明显下降、结论 确定了热处理的优化条件：核化温度为740℃，核化时间为50min，晶化温度为910℃，晶化时间为40min、在优化条件下制备的矿渣微晶泡沫玻璃由泡径2～3mm的气孔、晶体和玻璃相组成，XRD显示主晶相为透辉石；表观密度946kg／m^3，抗压强度17．9MPa，吸水率为0．25％，可代替实心粘土砖作为墙体材料使用．     

热处理制度对增钙水渣微晶玻璃的影响

以增钙水渣为主要原料制备了微晶玻璃,研究了热处理制度对微晶玻璃的影响.利用XRD、SEM对样品进行了测试、分析,并测试微晶玻璃的相关性能.     

TiO2和Cr2O3作晶核剂制取粉煤灰微晶玻璃晶化行为的研究

研究了以TiO2和Cr2O3为晶核剂制取粉煤灰微晶玻璃的晶化行为,运用DTA、XRD、SEM等测试方法,观察了制品中的晶相种类、含量和微晶体发育形貌,分析了基础玻璃的化学组成、热处理方法和晶核剂对晶化行为的影响.研究表明:利用粉煤灰可以生产透辉石为主晶相的微晶玻璃,粉煤灰掺量可达40%以上.晶核剂种类和基础玻璃的化学组成对析晶行为和晶相种类有重要影响,熔制工艺和热处理方法也会影响析晶行为,本研究的玻璃基础组成有利于透辉石晶体的生成.     

Eu~(3+)掺杂Gd_(9.33)(SiO_4)_6O_2微晶玻璃的制备及发光性能研究

采用高温熔融法制备Si O2-Na F-Na2O-Gd2O3-Eu2O3系基质玻璃,热处理后获得微晶玻璃.通过差热分析(DTA)、X射线衍射(XRD)、电子扫描电镜(SEM)和荧光光谱等对样品进行分析.XRD结果表明:基质玻璃经700、750℃热处理2~4 h获得含Gd9.33(Si O4)6O2的微晶玻璃.晶粒尺寸随热处理温度的升高和时间的延长而增大.荧光光谱研究结果表明:与基质玻璃相比,微晶玻璃的激发强度和发射强度明显增强,微晶玻璃中电荷迁移带发生偏移,5D0—7F1跃迁的发射峰出现劈裂,5D0—7F2与5D0—7F1跃迁强度比值减小,表明Eu3+进入Gd9.33(Si O4)6O2晶格中;微晶玻璃中5D0—7FJ特征发射峰和激发峰强度随热处理温度的升高和热处理时间的延长而增强.     

利用熔融态高炉渣制备微晶玻璃的研究

将高炉渣与辅料分别熔化,以在高温条件下混熔的方式制备性能稳定的基础玻璃。通过对基础玻璃的微热分析(DSC)确定玻璃的热处理工艺制度。结合X射线衍射分析(XRD)、扫描电子显微镜(FE-SEM)对微晶玻璃的结构与性能进行了研究。结果表明:基础玻璃中F含量的增加,有利于促进微晶玻璃成核和晶体长大,降低微晶玻璃的形核结晶温度。在低温热处理条件下得到微晶玻璃的主晶相为萤石,高温热处理得到的微晶玻璃同时析出了霞石和萤石两个微晶相。熔融态高炉渣微晶玻璃中,晶相的含量、种类对其抗折强度和硬度有显著影响,该实验条件下试样的抗折强度最高可达166.12 MPa,显微硬度最高可达672.13 MPa。     

Eu~(3+):YPO_4微晶玻璃的制备及其光谱研究

采用高温熔融法,将Eu3+掺杂的P2O5-Ba O-Na2O-K2O-Y2O3系统玻璃,在不同的温度下进行热处理,制备出Eu3+:YPO4的微晶玻璃.利用X射线衍射仪、扫描电子显微镜、荧光光谱仪等对微晶玻璃样品的晶相、微观形貌和光谱性能进行测试、研究.结果表明:基础玻璃在750℃热处理1 h可以得到纯相的Eu3+:YPO4的微晶玻璃,该微晶玻璃在225 nm波长的激发下,位于594 nm处Eu3+的5D0—7F1跃迁发射最强,并随着热处理温度的升高,微晶玻璃的发光强度逐渐增强.     

Preparation and optical properties of Er<Superscript>3+</Superscript>: Na<Subscript>2</Subscript>O-Al<Subscript>2</Subscript>O<Subscript>3</Subscript>-SiO<Subscript>2</Subscript> transparent glass-ceramics

Na₂O-Al₂O₃-SiO₂ glass-ceramics doped with Er³⁺ ions were synthesized by the conventional melt quenching technique at a low melting temperature. The samples were characterized by differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-vis-NIR scanning spectrophotometry, and fluorescence spectrometry. The results show that the main crystalline phase of glass-ceramics is nepheline.The best heat-treatment process is at 520 °C for 2 h. Because the up-conversion luminescence and near infrared luminescence properties of glass doped with Eu³⁺ are studied in detail.     

Effects of heat treatment temperature on crystallization and thermal expansion coefficient of Li2O-Al2O3-SiO2

The basic glass of Li₂O-Al₂O₃-SiO₂ system using P₂O₅ as nucleator was prepared by means of conventional melt quenching technology, and the heat-treatment process was determined by using differential thermal analysis. The crystalline phases and the microstructure of the glass-ceramics were investigated by using X-ray diffraction and scanning electron microscopy. The results show that the glass based on Li₂O-Al₂O₃-SiO₂ oxides using P₂O₅ as nucleator can be prepared at lower melt temperature of 1450°C and the glass-ceramics with lower thermal expansion coefficient of 21.6 × 10⁻⁷°C⁻¹ can also be obtained at 750°C. The glass-ceramics contain a few crystal phases in which the main crystal phase is β-quartz solid solution and the second crystal phase is β-spodumene solid solution. When the heat treatment temperature is not higher than 650°C, the transparent glass-ceramics containing β-quartz solid solution can be prepared. β-quartz solid solution changes into β-spodumene solid solution at about 750°C. And the appearance of the glass-ceramics changes from translucent, part opaque to complete opaque with increasing temperature.     

SrO-Al2O3-SiO2系统微晶玻璃的晶化行为及性能

通过改变玻璃成分,在不同的热处理制度下制备SrO-Al2O3-SiO2系统微晶玻璃,用DTA、XRD、SEM等手段对该系统微晶玻璃材料的析晶过程进行了研究。在此基础上,讨论了晶化行为对微晶玻璃的热学及力学性能的影响。结果表明:材料的热学性能及力学性能与玻璃成分及热处理制度密切相关。可以找到某一确定组分的基础玻璃,经过较低的核化温度与较高晶化温度热处理后,能够得到力学性能优良、热学性能较好的微晶玻璃材料。     

Mg-Al-Si堇青石微晶玻璃及其微观结构

以氧化铝、苏州土、滑石为原料,以TiO2为晶核剂,采用粉末烧结法制备了堇青石微晶玻璃。采用差热热重分析仪(TG-DTA)确定了基础玻璃的核化、晶化温度,采用X射线衍射仪(XRD)、扫描电镜(SEM)分析了材料的相组成及显微结构。结果表明:通过热处理工艺的调控可得到不同晶粒尺寸和性能的堇青石微晶玻璃。最佳的热处理工艺为:核化温度780℃,核化时间1 h;晶化温度1055℃,晶化时间2 h。最佳配方M-4微晶玻璃的体积密度为2.76 g/cm3,抗折强度达86.58 MPa,热膨胀系数为3.56×10-6℃-1。可望用于太阳能热发电关键材料。     

The phase transformation of R<Subscript>2</Subscript>O-CaO-SiO<Subscript>2</Subscript>-F glass-ceramics

The phase transformation of R₂O-CaO-SiO₂-F system glass-ceramics with various additions of K₂O and F was investigated by DTA, XRD, SEM and other techniques. The crystallization and the microstructure of the obtained glass-ceramics were also evaluated. The phase separation occurred in CN1 specimen after being quenched in water, but phase separation did not appear in other quenched specimens with the content of K₂O and F increasing obviously, showing K₂O and F modified the structure of the glass-forming melts. The increase of K₂O and F resulted in the reduction of phase separation and the enhancement of crystallization. The main crystalline phase formed after heat-treatment was canasite and CaF₂. The microstructures of the crystalline specimens consisted of interlocking radial and granular crystals. Moreover, the crystallinity was increased as the content of K₂O was increased from 0.07 mol to 0.08 mol.     

Effects of nucleating additives on crystallization and properties of CaO-B2O3-SiO2 glass-ceramics

ZrO₂, TiO₂ and P₂O₅ were doped in CaO-B₂O₃-SiO₂ glass-ceramics as nucleating additives. Effects of different nucleating additives on the phase separation and crystalline behaviors were investigated by using gradient temperature furnace, DTA and XRD. Then, sintering process of the glass-ceramics was investigated by testing sintering shrinkage, dielectric constant and loss. The experimental results shows that the glass-ceramics doped with nucleating additives represents higher crystallization, with ZrO₂ as an exceptional effective dopant to promote the precipitation of wollastonite crystal. Finally, ZrO₂ containing glass-ceramics was chosen to study the influence of sintering temperature and soaking time with the help of X-ray diffraction analysis and density measurement. The glass-ceramics can be well consolidated at 850 °C for 10 min, with low dielectric constant (5.87) and loss (3.21 × 10⁻⁴), which is desirable for LTCC application.     

利用冶金高炉渣制备微晶玻璃的研究

利用X荧光、X-ray和DTA等技术分析高炉渣原料的成分、晶相组成和热学性能,并以冶金高炉渣为主要原料添加少量长石,通过较简单的烧结法制备出CaO-Al2O3-SiO2-MgO 4元系为基础的微晶玻璃,测试分析炉渣微晶玻璃的性能.结果表明,炉渣微晶玻璃晶相主要为钙黄长石,样品的吸水率为0.1%,维氏硬度为5~6 GPa,三点弯曲强度为60~70 MPa,其性能明显优于黏土砖.     

Influence of crucible material on the microstructure and properties of iron rich glass-ceramics

Slag glass melting is usually performed on a laboratory scale in crucibles, which are economically viable tools for the production of slag glass-ceramics. In this work, quaternary CaO-Al₂O₃-MgOSiO₂ (CAMS) glass-ceramics were prepared by melting the tailing of Bayan Obo mine tailing, blast furnace slag, and fly ash in alumina and graphite crucibles. The effect of the crucible material on the microstructure and properties of the glass-ceramics was investigated using differential scanning calorimetry, X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy and inductively coupled plasma atomic emission spectroscopy. Results indicated that the contents of Al₂O₃ and Fe₂O₃ in the initial glass were significantly changed by the corrosion of the alumina crucibles during the glass melting process and by the reducing action of the graphite crucibles. The main crystal phases of glass-ceramics melted in alumina crucibles and graphite crucibles were Ca (Mg, Fe, Al) (Si, Al)₂O₆, coesite and Ca (Mg, Al) (Si, Al)₂O₆, respectively. According to these findings, we conclude that the microstructure and properties of the glass-ceramics are affected by the crucibles.     

CaO-Zr02-Ti02-A1203-B203-Si02玻璃陶瓷的制备及化学稳定性研究

玻璃陶瓷是固化处理中、高放废物和α废物较为理想的候选材料之一。研究了特定条件下制备的CaO-ZrO2-TiO2-A120,-B20,-SiOz体系玻璃陶瓷在水淬和空气中自然冷却的两种冷却制度对其结晶行为和显微结构的影响,用粉末浸泡实验方法测试了其化学稳定性。结果表明：自然冷却形成的玻璃陶瓷晶相主要是ZrSiO。和ZrTiOt;在25-70℃范围内,温度对玻璃陶瓷浸出率无明显影响,90℃下浸出率比25℃,40℃,70℃的浸出率高一个数量级;7d元素总的归一化浸出为1．87g／m^2。     

Effect of nucleating agents on microstructure and mechanical properties of SiO2-Al2O3-ZrO2 glass-ceramics

SiO2-Al2O3-ZrO2 glasses with different nucleating agents were crystallized under special processing schedule. The microstructure and mechanical properties of the glass-ceramics in SiO2-Al2O3-ZrO2 system were investigated by differential scanning calorimetry, scanning electron microscopy, X-ray diffraction and three-point bending method. The results show that ZrO2 is not an effective nucleating agent in SiO2-Al2O3-ZrO2 system, while TiO2 is effective for the separation of spinel, and P2O5 facilitates solubility of ZrO2 in glass and crystallization. The main crystalline phases of the glass-ceramics are spinel, anorthite and tetragonal zirconia. With the increase of ZrO2 content in the glass, glass-ceramics show higher bending strength （120 MPa） than others.