CN113933330B - 一种表征稀土在球团矿中分布状态的方法 - Google Patents
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Abstract
本发明公开了一种表征稀土在球团矿中分布状态的方法，用扫描电镜背散射探测器，将原子序数不同的化学元素及其相简便、准确的分析出来，为研究稀土对球团矿还原膨胀性提供了数据支撑，本发明作为扫描电镜检测领域的一项重要方法，特别适用于高炉冶炼材料球团矿中不同组分的检测。
Description
技术领域
本发明涉及高炉冶炼材料检测领域，尤其涉及一种表征稀土在球团矿中分布状态的方法。
背景技术
球团矿是为高炉冶炼生铁提供的原料，是铁矿石经过一定制备工艺而成的。球团矿的性能直接影响高炉的稳定性及顺行程度，其中高温冶金性能是球团矿的重要性能指标之一。优良的高温冶金性能是指球团矿具有较好的还原性、较低的还原粉化率及低的还原膨胀率。球团矿的还原膨胀率较高时，会使高炉料柱透气性变差，煤气分布失常，炉况不顺，严重影响高炉的正常冶炼。因此，控制球团矿的还原膨胀率是提高高炉冶炼效率的重要指标。技术人员在研究稀土元素对球团矿的还原膨胀作用时，试图找到合适的稀土加入量、稀土的分布状态等影响因素。
扫描电镜(SEM)是冶金材料表征时广泛使用的强有力工具。对于扫描电镜来说，用于成像的两类电子分别是背散射电子(BSE)和二次电子(SE)。背散射电子来自于入射电子束，这些电子与样品发生弹性碰撞，其中一部分反弹回来，这就是背散射电子。另一方面，二次电子则来自于样品原子，它们是入射电子与样品发生非弹性碰撞所产生的。BSE来自于样品的较深层区域，而SE则产生于样品的表面区域。因此，BSE和SE代表不同的信息。BSE图像对原子序数差异非常敏感；材料的原子序数越大，对应在图像中就越亮。
球团矿主要成分为SiO2、Al2O3、CaO、MgO、TFe、Mn、P、S等，原子序数最大的是铁(原子序数26),添加到球团矿中的稀土元素是铈(原子序数58)。基体与添加剂两者的原子序数相差大，利用扫描电镜背散射电子能够简单、快速、准确地表征稀土在球团矿中的分布状态。
目前，尚无此方面的文献及专利。
发明内容
本发明的目的是提供一种表征稀土在球团矿中分布状态的方法，此方法作为扫描电镜检测领域的一项重要方法，特别适用于高炉冶炼材料球团矿中不同组分的检测。
为解决上述技术问题，本发明采用如下技术方案：
一种表征稀土在球团矿中分布状态的方法，主要包括以下步骤：
1)试样准备
将球团矿试样进行磨制和抛光处理，得到一个表面平整的矿物分析试样；
2)仪器准备
使用洗耳球将试样表面灰尘等污染物吹拂干净，装在扫描电镜样品台上，将样品台放入扫描电镜样品仓；抽真空，5-10分钟后，真空度达10-6mbar；设置高压；打开钨灯丝，调节灯丝像、灯丝电流使灯丝像明亮且居中；
3)矿相检测
升高样品台，使用二次电子探测器，调节亮度、对比度、像散参数，聚焦图像；将工作距离调至合适位置，再次聚焦图像，直到得到一张清晰的二次电子图像；
插入背散射探测器，调节亮度和对比度，聚焦图像，直到得到一张清晰的背散射电子图像，原子序数不同的元素呈现不同的明暗相，稀土在球团矿中的分布状态一目了然；配合能谱仪，对化学元素进行定性分析，以验证稀土等化学元素的准确性；
5)结果分析
使用EDAX Genesis进行数据分析，导出结果。
进一步的，所述步骤)2中设置高压15KV。。
与现有技术相比，本发明的有益技术效果：
本发明提供了一种表征稀土在球团矿中分布状态的方法，金相显微镜、扫描电镜二次电子等技术手段都不易观察到稀土在球团矿中的分布状态，使用扫描电镜背散射探测器，将原子序数不同的化学元素及其相简便、准确的分析出来，为研究稀土对球团矿还原膨胀性提供了数据支撑。
附图说明
下面结合附图说明对本发明作进一步说明。
图1是球团矿试样实物照片。
图2是球团矿二次电子图像。
图3是球团矿背散射电子图像。
图4是能谱对稀土的定性定量分析结果。
具体实施方式
实施例
一种表征稀土在球团矿中分布状态的方法，将添加了稀土元素铈的球团矿试样进行磨制和抛光处理，得到一个表面平整的矿物分析试样，如图1所示；
使用洗耳球将试样表面灰尘等污染物吹拂干净，装在扫描电镜样品台上，将样品台放入扫描电镜样品仓；抽真空(机械泵+分子泵)，6分钟后，真空度达10-6mbar；设置高压15KV；打开钨灯丝，调节灯丝像、灯丝电流等使灯丝像明亮且居中；
升高样品台，使用二次电子探测器，调节亮度、对比度、像散等参数，聚焦图像；将工作距离调至WD＝13mm位置，再次聚焦图像，直到得到一张清晰的二次电子图像，如图2所示；
插入背散射探测器，调节亮度和对比度，聚焦图像，直到得到一张清晰的背散射电子图像，原子序数不同的元素呈现不同的明暗相，稀土铈属于原子序数最大的元素，所以图像中最亮的部分是铈的分布位置，稀土铈在球团矿中的分布状态如图3所示。配合能谱仪，对化学元素进行定性分析，以验证稀土等化学元素的准确性，如图4所示。最后，将结果导出至word文件。
使用扫描电镜背散射模式，将球团矿中稀土的分布状态快速、准确的表征出来，为研究稀土对球团矿还原膨胀性提供可靠的数据支撑。
以上所述的实施例仅是对本发明的优选方式进行描述，并非对本发明的范围进行限定，在不脱离本发明设计精神的前提下，本领域普通技术人员对本发明的技术方案做出的各种变形和改进，均应落入本发明权利要求书确定的保护范围内。
Claims (2)
1.一种表征稀土在球团矿中分布状态的方法，其特征在于：主要包括以下步骤：
1)试样准备
将球团矿试样进行磨制和抛光处理，得到一个表面平整的矿物分析试样；
2)仪器准备
使用洗耳球将试样表面灰尘等污染物吹拂干净，装在扫描电镜样品台上，将样品台放入扫描电镜样品仓；抽真空，5-10分钟后，真空度达10-6mbar；设置高压；打开钨灯丝，调节灯丝像、灯丝电流使灯丝像明亮且居中；
3)矿相检测
升高样品台，使用二次电子探测器，调节亮度、对比度、像散参数，聚焦图像；将工作距离调至合适位置，再次聚焦图像，直到得到一张清晰的二次电子图像；
插入背散射探测器，调节亮度和对比度，聚焦图像，直到得到一张清晰的背散射电子图像，原子序数不同的元素呈现不同的明暗相，稀土在球团矿中的分布状态一目了然；配合能谱仪，对化学元素进行定性分析，以验证稀土等化学元素的准确性；
4)结果分析
使用EDAX Genesis进行数据分析，导出结果。
2.根据权利要求1所述的表征稀土在球团矿中分布状态的方法，其特征在于：所述步骤)2中设置高压15KV。
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| CN105755364A (zh) * | 2016-05-13 | 2016-07-13 | 湖南化工职业技术学院 | 一种VCp增强复合耐磨合金材料及其制备方法 |
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| WO2014102733A1 (en) * | 2012-12-28 | 2014-07-03 | Fei Company | Process for performing automated mineralogy |
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| CN105755364A (zh) * | 2016-05-13 | 2016-07-13 | 湖南化工职业技术学院 | 一种VCp增强复合耐磨合金材料及其制备方法 |
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