废石渣白色微晶玻璃的研究
发布时间:2018-07-01 21:44
本文选题:废石渣 + 复合晶核剂 ; 参考:《山东建筑大学》2015年硕士论文
【摘要】:本文利用花岗岩废石渣为主要原料,经过除铁工艺预处理后,添加一定量的助熔剂、网络调整剂和形核剂等,采用高温熔融法制备具有优良性能的白色微晶玻璃,白度值92%左右,系统地研究了晶核剂、原料配比及热处理温度对废石渣白色微晶玻璃综合性能的影响及关系。实验采用了复合形核剂CaF2/Na5P3O10,设定CaF2/Na5P3O10比例为1/1、1/2、1/3、1/4和1/5,对制备的微晶玻璃样品进行了XRD、SEM表征和性能测试。结果表明:随CaF2/Na5P3O10比值的降低,试样的主晶相由硅灰石相转变成氟磷灰石相,且硅灰石相逐渐减弱;微观结构方面,试样析出的晶体呈长条状和颗粒状,降低CaF2/Na5P3O10比值,长条状晶体逐渐减少,颗粒状晶粒长大,分布均匀;微晶玻璃试样的力学性能随CaF2/Na5P3O10匕值的降低先升高后降低;当CaF2/Na5P3O10比值为1/2时,微晶玻璃试样中氟磷灰石相和硅灰石相分布均匀,结构致密,此时具有较优力学性能,抗折强度134.2MPa,维氏硬度802MPa。确定最佳CaF2/Na5P3O10添加比例为1/2。为了最大程度地利用废石渣,本实验设计废石渣含量分别为55%、60%、65%、70%和75%进行了废石渣微晶玻璃制备实验,并对制备的试样的物相、微观结构和性能进行了分析测试。结果表明:不同废石渣含量制备出的白色微晶玻璃的物相种类没有变化,主晶相为氟磷灰石,次晶相为硅灰石。随废石渣含量的增加,XRD图谱显示试样的衍射峰强度先增强后减弱;SEM照片显示样品中长条状晶体数量先增加后减少,颗粒状晶粒尺寸增加,废石渣含量为65%时制备的微晶玻璃结构均匀致密,析晶完全;微晶玻璃的力学性能随废石渣含量的增加先升高后降低,化学稳定性逐渐增强。当废石渣含量为65%时,获得的微晶玻璃晶相均匀分布,析晶充分,具有较优的力学性能,抗折强度150.6MPa,维氏硬度810MPa。确定最佳废石渣添加量为65%。根据DTA曲线,本论文将废石渣含量为65%,复合形核剂CaF2/Na5P3O10比值为1/2制备的基础玻璃在840℃、870℃、900℃、930℃和960℃五组不同的温度下热处理,测试制备的微晶玻璃试样的XRD、SEM及各项性能。研究结果表明:随热处理温度的升高,氟磷灰石相增强,硅灰石相逐渐减弱;通过SEM分析可知840℃~900℃热处理时,试样中长条状晶体与球形颗粒状晶粒共存,900℃~960℃热处理时,长条状晶体逐渐消失,颗粒状晶粒均匀分布,但温度过高会使内部出现裂纹等缺陷,导致微晶玻璃的力学性能降低;试样的密度和机械强度先升高后降低,化学稳定性先增强后减弱。900℃热处理时,样品结构致密,晶体分布均匀,析晶较为完全,密度取得最大值2.77g/cm3,抗折强度150.6MPa,维氏硬度810MPa,具有最优的化学稳定性。当废石渣含量为65%,复合形核剂CaF2/Na5P3O10比值为1/2时的最佳热处理温度为900℃。
[Abstract]:In this paper, the white glass-ceramics with excellent properties were prepared by high temperature melting method using granite waste rock slag as the main raw material, adding a certain amount of flux, network adjuster and nucleating agent after pretreatment of iron removal process. The effects of nucleating agent, raw material ratio and heat treatment temperature on the comprehensive properties of white glass-ceramics with waste stone slag were systematically studied. The composite nucleating agent CaF _ 2 / Na _ 5P _ 3O _ (10) was used, and the ratio of CaF _ 2 / Na _ 5P _ 3O _ (10) was set to be 1 / 1 / 1 / 2 / 3 / 3 / 4 and 1 / 5 respectively. The prepared glass-ceramics samples were characterized by XRDX SEM and their properties were tested. The results show that with the decrease of CaF _ 2 / Na _ 5P _ 3O _ 10 ratio, the main crystalline phase changes from wollastonite phase to fluoropatite phase, and the wollastonite phase decreases gradually, and the precipitated crystals are long and granular, which decreases the ratio of CaF _ 2 / Na _ 5P _ 3O _ (10), and decreases the ratio of CaF _ 2 / Na _ 5P _ 3O _ (10). The mechanical properties of glass-ceramics increased with the decrease of CaF _ 2 / Na _ 5P _ 3O _ (10) and then decreased, when the ratio of CaF _ 2 / Na _ 5P _ 3O _ 10 was 1 / 2, The fluoroapatite and wollastonite phases in glass-ceramics are uniformly distributed and have dense structure. At this time, they have better mechanical properties, the flexural strength is 134.2 MPa, and the Vickers hardness is 802MPa. The best addition ratio of CaF2 / Na5P3O10 is 1 / 2. In order to make the best use of the waste stone slag, the content of the waste stone slag was 55. 60% and 65% respectively. The glass-ceramics preparation experiment of the waste stone slag was carried out. The phase, microstructure and properties of the sample were analyzed and tested. The results showed that the white glass-ceramics prepared with different content of waste stone slag had no change in phase, the main crystal phase was fluoroapatite, and the secondary phase was wollastonite. With the increase of waste slag content, XRD pattern showed that the diffraction peak intensity of the sample first increased and then weakened. SEM photos showed that the number of long stripe crystals in the sample first increased and then decreased, and the grain size increased. The structure of the glass-ceramics was uniform and dense when the content of waste slag was 65. The mechanical properties of the glass-ceramics increased first and then decreased with the increase of the content of waste slag, and the chemical stability increased gradually. When the content of waste slag is 65, the obtained glass-ceramics have uniform distribution of crystal phase, sufficient crystallization and excellent mechanical properties. The flexural strength is 150.6 MPA, and the Vickers hardness is 810 MPA. The optimum amount of waste slag is 65. According to the DTA curve, the basic glass prepared by the composite nucleating agent CaF _ 2 / Na _ 5P _ 3O _ 10 was heat treated at 840 鈩,
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