CN116297583A - 一种脱碳退火态取向硅钢ebsd样品制备方法 - Google Patents
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Abstract
本发明公开了一种脱碳退火态取向硅钢EBSD样品制备方法，包括：(1)取样；(2)机械制样；(3)配置电解抛光液，选用5％的高氯酸乙醇溶液作为电解抛光液；(4)实验装置准备；(5)电解抛光工艺参数：60V电压下抛光20S，电解液温度控制在22℃以下。本发明的目的是提供一种脱碳退火态取向硅钢EBSD样品制备方法，通过本方法可以制备出合格的EBSD样品，在EBSD探测器下观察到了良好的菊池衍射花样图像。
Description
技术领域
本发明涉及试样制备与检测技术领域，尤其涉及一种脱碳退火态取向硅钢EBSD样品制备方法。
背景技术
随着材料领域的飞速发展，对材料的各种分析测试技术的要求不断提高，新型分析测试技术备受研究学者们的关注。EBSD技术改变了以往织构分析的方法，形成了将显微组织和晶体学分析相结合全新的科学领域，已成为材料研究中一种有效的分析手段。但是这些所有应用是建立在获得高质量EBSD结果的基础之上的，因此制备高质量的EBSD样品是所有EBSD技术使用者遇到的首要问题。
采用常规金相样品的制备方法可以制备EBSD试样，但是不能有效去除应力应变层，得到的菊池衍射花样效果不佳，影响EBSD实验数据的准确性。采用离子减薄、聚焦离子束及截面抛光等方法制备的EBSD样品重复性好但设备昂贵，运行及制样成本高，应用受限。机械抛光后再电解抛光腐蚀方法是钢铁材料操作简单、快速、低成本、实用的方法。
电解抛光样品制备方式由于其自身的特点,对电压、温度和时间均有精准的要求。制样时电解抛光的工艺参数会影响电流的稳定性，制备的EBSD样品质量不佳会影响实验数据的准确性，浪费实验时间和成本。不同钢铁材料因电导率的不同，想要获得理想的EBSD结果需要摸索出最佳的样品制备方法。
取向硅钢在生产过程中，尤其是在轧制过程及退火工序下，其微观结构变化十分明显且有特点，其磁性能与晶粒、织构及再结晶现象有着密不可分的关联，因此检测织构是取向硅钢研究的重点，制备合格的取向硅钢EBSD样品是其工作者开展实验研究的首要任务，基于此现状提出了一种用于脱碳退火态取向硅钢的EBSD样品制备方法，适用于从事物理检测与金属材料研究领域的相关行业及科研院所，极具推广应用价值。
发明内容
本发明的目的是提供一种脱碳退火态取向硅钢EBSD样品制备方法，通过本方法可以制备出合格的EBSD样品，在EBSD探测器下观察到了良好的菊池衍射花样图像。
为解决上述技术问题，本发明采用如下技术方案：
本发明一种脱碳退火态取向硅钢EBSD样品制备方法，包括：
(1)取样
用钼丝切割机切取试样，放入无水乙醇溶液中超声波清洗5min，去除样品表面油污；
(2)机械制样
将试样在颗粒度为400#-1000#的砂纸上轻磨至试样磨面上只有单一方向均匀的细磨痕，将预磨好的试样在金相试样抛光机上使尼龙抛光绒布配合5.0μm高效金刚石研磨剂进行抛光至呈现镜面；
(3)配置电解抛光液
电解抛光液由酸类和溶剂配置，选用5％的高氯酸乙醇溶液作为电解抛光液；
(4)实验装置准备
将500ml的电解液置于电解抛光机的电解液罐中并插入温度计测温，为了使电解液温度均匀，缓慢向电解液中倾倒液氮制冷至-20℃；试样为阳极，不锈钢板为阴极，阴极极板上放入1cm2孔径绝缘样品模具，将试样磨面放置于绝缘模具的孔径上，用阳极臂将试样夹持，保持试样与模具孔径相对稳定且平行，使得阳极、阴极与电解液连通于稳压稳流直流电源；
(5)电解抛光工艺参数
60V电压下抛光20S，电解液温度控制在22℃以下。
进一步的，所述试样的规格为10mm*10mm。
进一步的，所述电解抛光机具体为struerslectropol-5型电解抛光机。
进一步的，EBSD检测，将制备好的样品放入扫描电镜中，选择适用于EBSD信号的参数调试设备至观察到清晰的样品形貌，点击样品任意微区均能观察高质量的菊池花样图像。
与现有技术相比，本发明的有益技术效果：
本发明找到了一种适用于脱碳退火态取向硅钢的EBSD样品制备方法，合适的电解抛光工艺参数使得样品制备过程电流稳定，样品表面光洁无污染。以EBSD探测器观察电解抛光后的试样表面状态，可看到传统机械抛光过程中造成的抛光损伤已经去除，表面比较平滑，可以得到质量较高的EBSD花样图象，适用于脱碳退火态取向硅钢EBSD检测的样品制备，实验过程简单快捷，极具推广应用价值。
附图说明
下面结合附图说明对本发明作进一步说明。
图1为本发明脱碳退火态取向硅钢EBSD样品制备方法的流程图。
具体实施方式
下面结合图1对本发明的具体实施方式进行说明：
一种脱碳退火态取向硅钢EBSD样品制备方法，包括：
第一步，取样
用钼丝切割机切取10mm*10mm规格脱碳退火态取向硅钢EBSD试样，放入装有无水乙醇溶液的烧杯中在超声波水域中震荡清洗5min，去除样品表面的残渣污垢；
第二步，机械制样
将试样在颗粒度为400#-1000#的砂纸上轻磨至试样磨面上只有单一方向均匀的细磨痕，将预磨好的试样在金相试样抛光机上使用尼龙抛光绒布配合5.0μm高效金刚石研磨剂抛光至样品表面呈镜面即可，磨制力度应尽可能小，去除应力应变层的同时避免产生新的应力层；
第三步，电解抛光
首先，配置电解抛光液。用55.5ml高氯酸+500ml无水乙醇配置电解抛光液；
其次，实验准备。在电解液罐中加入500ml电解液，插入温度计测温，缓慢向电解液中倾倒液氮制冷至-20℃，将制备好的电解液置于电解槽中，插入搅拌棒。阴极极板上放入1cm2孔径绝缘样品模具，将试样磨面放置于绝缘模具的孔径上，用阳极臂将试样夹持，保持试样与模具孔径相对稳定且平行，使得阳极、阴极与电解液连通于稳压稳流直流电源；
进一步，电解抛光工艺参数选择，应用struerslectropol-5型电解抛光机对机械抛光好的试样进行电解抛光。进入usermethods界面植入一个空白界面进行编程：抛光腐蚀程序→抛光面积1cm2区域→保持电解液温度控制在22℃以下→60V电压→抛光20S→启动程序，电流稳定，实验效果良好；
进一步，待电解抛光结束后迅速用样品夹将样品取出后用无水乙醇溶液冲洗并吹干；
进一步，更换电解液为500ml去离子水，进入manualfuntions界面中的changeelectrolyte界面后，启动程序清洗与电解液接触的抛光装置；
第四步，EBSD检测
将制备好的样品放入扫描电镜中，选择适用于EBSD信号的参数调试设备至观察到清晰的样品形貌，点击样品任意微区均可观察高质量的菊池花样图像。
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 (4)
1.一种脱碳退火态取向硅钢EBSD样品制备方法，其特征在于，包括：
(1)取样
用钼丝切割机切取试样，放入无水乙醇溶液中超声波清洗5min，去除样品表面油污；
(2)机械制样
将试样在颗粒度为400#-1000#的砂纸上轻磨至试样磨面上只有单一方向均匀的细磨痕，将预磨好的试样在金相试样抛光机上使尼龙抛光绒布配合5.0μm高效金刚石研磨剂进行抛光至呈现镜面；
(3)配置电解抛光液
电解抛光液由酸类和溶剂配置，选用5％的高氯酸乙醇溶液作为电解抛光液；
(4)实验装置准备
将500ml的电解液置于电解抛光机的电解液罐中并插入温度计测温，为了使电解液温度均匀，缓慢向电解液中倾倒液氮制冷至-20℃；试样为阳极，不锈钢板为阴极，阴极极板上放入1cm2孔径绝缘样品模具，将试样磨面放置于绝缘模具的孔径上，用阳极臂将试样夹持，保持试样与模具孔径相对稳定且平行，使得阳极、阴极与电解液连通于稳压稳流直流电源；
(5)电解抛光工艺参数
60V电压下抛光20S，电解液温度控制在22℃以下。
2.根据权利要求1所述的脱碳退火态取向硅钢EBSD样品制备方法，其特征在于，所述试样的规格为10mm*10mm。
3.根据权利要求1所述的脱碳退火态取向硅钢EBSD样品制备方法，其特征在于，所述电解抛光机具体为struers lectropol-5型电解抛光机。
4.根据权利要求1所述的脱碳退火态取向硅钢EBSD样品制备方法，其特征在于还包括：EBSD检测，将制备好的样品放入扫描电镜中，选择适用于EBSD信号的参数调试设备至观察到清晰的样品形貌，点击样品任意微区均能观察高质量的菊池花样图像。
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| CN117233188A (zh) * | 2023-11-08 | 2023-12-15 | 包头市威丰稀土电磁材料股份有限公司 | 一种硅钢ebsd大尺寸拼接样品的制备方法 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117233188A (zh) * | 2023-11-08 | 2023-12-15 | 包头市威丰稀土电磁材料股份有限公司 | 一种硅钢ebsd大尺寸拼接样品的制备方法 |
| CN117233188B (zh) * | 2023-11-08 | 2024-01-30 | 包头市威丰稀土电磁材料股份有限公司 | 一种硅钢ebsd大尺寸拼接样品的制备方法 |
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