CN111982943B - 一种ebsd测试样品台及其应用 - Google Patents
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Abstract
本发明涉及一种EBSD测试样品台,属于试验器材领域,包括夹具体和底座,夹具体通过其底端设置在底座上,其特征在于,夹具体为直角梯形的四棱柱,所述夹具体的四个侧端面沿其周向依次为第一端面、第二端面、第三端面、第四端面,第一端面作为夹具体的工作面,其与夹具体的底端呈70°夹角,夹具体上开有至少一开槽,开槽分别与第一端面、第二端面、第三端面相连通;与夹具体相配合的还设置有挡板,挡板设置于所述开槽中并与夹具体可分离式连接,且挡板的一侧端面作为工作端;本发明能够适用于薄型样品如电池极片、无机晶体薄膜等的EBSD测试,尤其适用于日立SU8000系列冷场扫描电镜的EBSD测试。
Description
技术领域
本发明涉及试验器材领域,具体涉及一种EBSD测试样品台及其应用。
背景技术
上世纪九十年代以来,晶体微区取向及晶体结构的分析技术取得了较大发展,电子背散射衍射(Electron Back scattered Diffraction简称EBSD)在材料微观组织结构及微织构表征中得到广泛应用。EBSD的主要特点除了保留扫描电子显微镜的常规特点外,该技术还基于扫描电镜中电子束在倾斜样品表面激发出并形成的衍射菊池带的分析,进而确定晶体结构、取向及相关信息的方法,在晶体材料的组织表征和分析中有着重要的作用。EBSD主要应用于钢铁和无机晶体材料的物相、组织鉴定、取向分析、微织构分析、晶界分析和晶粒度测量等。
EBSD测试的样品台,为了得到较强的信号,相对于入射电子束,样品需要倾斜60-70°,最简单的做法是做一个倾斜70°的小台,把样品固定到小台上,然后再粘接到电镜样品台底座上,即使如此,在高倍下(如5万倍)和大电子束流,样品成像还是会受到上述不稳定因素的影响。这很难保证定位的精确性,也很难保证粘接的牢固程度。该方法的缺点是在进行大变形、组织细小、残余应力较大的样品高倍率分析测试时,常常会在测试过程中出现图片分辨率低,甚至是图片出现漂移的状况;由于样品夹台较重,在实验过程中会发生图像的漂移,导致结果存在较大误差。
现有技术中已有相关文献对上述问题提出了改进:例如,申请号为CN201511022163.0的专利申请针对图像漂移的现象,开发了一种EBSD分析测试用的样品台,但是该技术主要是解决由于重量的原因造成的图像漂移情况,但对于厚度很薄的薄片样品(0.1um-5mm)很难实现多方向分析测试。
此外,在高倍率下,EBSD分析测试大变形薄板材料组织的另一种方法是制成透射电镜薄膜样品,厚度约为几十个微米,然后用银胶固定在样品台上,但是该方法对于厚度低于5mm的薄板不太适用,一方面原因是薄板厚度过小,在制样研磨过程中造成靠近薄板表面处的组织无法观察,另一方面原因是当薄板厚度很小时,很难制成直径为3mm的圆片,无法进行电解双喷制样、成功率低。它们要么过于复杂,要么调节过于繁琐,要么不适于日立U8系列冷场发射扫描电子显微镜的样品台。而且,现有的EBSD样品台主要为观察样品表面的样品,针对狭小的断面样品,尤其是片状(电池极片,无机晶体薄膜等)样品的端面无法稳定地放置在普通的样品台上,且遮挡了背散射电子衍射的信号,严重影响EBSD衍射花样和解析效果。
因此,薄型产品如电池极片的截面样需要特殊固定结构的截面样品台。
发明内容
本发明所要解决的技术问题是针对现有技术的不足,提供一种能够适用于薄型样品如电池极片、无机晶体薄膜等的EBSD测试,尤其适用于日立U8系列冷场扫描电镜的EBSD测试样品台及其应用。
本发明解决上述技术问题的技术方案如下:一种EBSD测试样品台,包括夹具体和底座,夹具体通过其底端设置在底座上,其特征在于,所述夹具体为直角梯形的四棱柱,所述夹具体的四个侧端面沿其周向依次为第一端面、第二端面、第三端面、第四端面,所述第一端面作为夹具体的工作面,其与夹具体的底端呈70°夹角,所述夹具体上开有至少一开槽,所述开槽分别与第一端面、第二端面、第三端面相连通;与所述夹具体相配合的还设置有挡板,所述挡板设置于所述开槽中并与夹具体可分离式连接,且挡板的一侧端面作为工作端,挡板的上表面作为薄片型样品的承载面,所述挡板的工作端与所述第一端面相平齐,且其齐于第一端面。
进一步的,所述夹具体的高度不大于25mm。
进一步的,所述开槽的宽度为1-5mm。
进一步的,所述挡板的工作端设有一补偿角α,开槽与第一端面的夹角设为β,β=90°±α。
更进一步的,α≤5°。
进一步的,所述夹具体底端设置有定位螺孔及至少一固定螺孔,夹具体通过螺柱与定位螺孔相配合连接在底座上,夹具体通过螺钉与固定螺孔相配合用于将挡板固定在开槽中。
进一步的,所述挡板相对于其工作端的另一端设置有手柄。
进一步的,所述薄片型样品与挡板之间通过导电胶带或导电银浆固定粘结相连。
进一步的,所述薄片型样品的厚度设为0.1um-5mm。
及一种如上所述的EBSD测试样品台的应用,其特征在于,应用于日立U8系列冷场电镜中,用于薄片型样品的截面EBSD测试。
本发明的有益效果是:本发明通过设置的具有特殊开槽结构的夹具体以及与之相配合的挡板,能够实现薄型产品如电池极片的截面微米尺度区域内微区相结构的标定,解决了日立U8系列冷场扫描电镜使用常规样品台夹具时遮挡了背散射电子衍射的信号和样品采用导电胶粘结在样品台上在测试过程中会出现移动而导致的图像位置改变而产生背散射区域偏移的问题,适用于日立U8系列冷场电镜下薄型样品如电池极片截面的EBSD样品分析。
附图说明
图1是本发明的结构示意图;
图2是本发明夹具体的立体结构示意图;
图3是本发明夹具体的左视结构示意图;
图4是本发明夹具体的右视结构示意图;
图5是本发明挡板的立体结构示意图;
图6是本发明挡板的截面结构示意图;
图7是图6的局部放大结构示意图;
图8是1mm厚硅片的截面扫描电镜图;
图9是1mm厚硅片的截面EBSD衍射花样;
图10是1mm厚硅片的截面花样解标定;
图11是电极片的截面扫描电镜图;
图12是电极片的截面EBSD衍射花样;
图13是电极片的截面花样解标定;
图中:100.底座,1.夹具体,11.第一端面,12.第二端面,13.第三端面,14.第四端面,2.开槽,3.挡板,31.工作端,32.承载面,33.手柄,4.定位螺孔,5.固定螺孔,6.螺柱。
具体实施方式
下面结合附图对本发明的原理和特征进行描述,所举实施例只用于解释本发明,并非用于限定本发明的范围。
如图1-图7所示为本实施例的一种EBSD测试样品台,其包括夹具体1和底座100,夹具体1通过其底端设置在底座100上,具体地,夹具体1底端设置有定位螺孔4,夹具体1通过一螺柱6与定位螺孔4相配合连接在底座100上,螺柱6的设置还能够实现夹具体1在底座100上的高度可调节,便于有效调节工作距离,以便提高背散射电子衍射的信号量,提高解析能力;
所述夹具体1为直角梯形的四棱柱,所述夹具体1的四个侧端面沿其周向依次为第一端面11、第二端面12、第三端面13、第四端面14,所述第一端面11作为夹具体1的工作面,其与夹具体1的底端呈70°夹角,所述夹具体1上开有至少一开槽2,所述开槽2分别与第一端面11、第二端面12、第三端面13相连通;本实施例中的夹具体1上开有3个开槽2,其中上下两开槽与第一端面11呈95°夹角,中间一开槽与第一端面11呈85°夹角,采用不同高度的开槽便于有效调节工作距离,以便提高背散射电子衍射的信号量,提高解析能力;
另外,与所述夹具体1相配合的还设置有挡板3,所述挡板3设置于所述开槽2中并与夹具体1可分离式连接,且挡板3的一侧端面作为工作端31,挡板3的上表面作为薄型样品的承载面32,所述挡板3的工作端31与所述第一端面11相平齐,且齐于第一端面11,挡板3相对于其工作端31的另一端设置有手柄33,便于样品的取放;夹具体1底端设有两个固定螺孔5,两固定螺孔5分别设置在定位螺孔4两侧,固定螺孔5为盲孔结构并上连至开槽2的位置,夹具体1通过螺钉与固定螺孔5相配合,螺钉抵制在挡板3的底端,用于将挡板3固定在开槽2中,为了更好的固定挡板3,采用一个或多个螺钉,确保挡板3的工作端31与所述第一端面11相平行且,齐于第一端面11,同时利于多次将同一试样固定在同一档位置,重复定位效果好。挡板3在开槽2内为间隙配合,目的是为了挡板3在夹具体1中的取放操作,挡板3的工作端31设有一补偿角α,即工作端31向挡板3的底端面方向偏折一定角度,补偿角α设为5°,如图7所示,配合开槽2与第一端面11的夹角设计,用于保证该工作端31与所述第一端面11相平齐,进而保证截面EBSD测试效果。
本实施例中的夹具体1的高度设为25mm,所述开槽2的宽度为2mm,挡板厚度为1mm。
本实施例EBSD测试样品台的应用:
将本实施例的EBSD测试样品台应用于日立U8230冷场扫描电镜中,用于薄型样品的截面的EBSD测试,本实施例具体用于1mm厚硅片的截面EBSD测试。
具体操作步骤如下:
将1mm厚硅片裁切成长1cm宽1.5cm的小片,对其将厚度面采用2000目的砂纸打磨1h,然后用3000目的砂纸打磨抛光。将抛光好的样品,用镊子夹住,避免镊子与样品检测面接触(镊子与检测面接触会形成较深的划痕),放置时,使样品厚度面与第一端面11相平行,且齐于第一端面11,然后固定在底座100,这样放置后就会保证样品检测面与水平方向的夹角为70°,进样日立8230冷场发射电镜进行EBSD衍射进行有效探测,在电压25-30KV,束流25-30μA,工作距离10-25mm。
本实施例用于1mm厚硅片的EBSD检测,样品的截面扫描电镜图、EBSD衍射花样和花样解标定分别见图8-图10。
另外将本实施例用于电极片的截面EBSD测试,其中待测正极电极片的厚度的规格参数为:0.1um-10um;具体操作步骤如下:
1.将电极片样品采用导电胶固定粘结在挡板3的承载面32上,然后置于Gatan685PESC II精密蚀刻镀膜仪中在电压为5kv作用下,双枪氩离子抛光作用1-2h,然后在电压为3kv作用下,双枪氩离子抛光作用30min-1h;
2.将第一步中抛光好的固定的极片挡板3的工作端31与所述第一端面11相平行,且齐于第一端面11,然后固定在底座100,然后固定在底座100,这样放置后就会保证样品检测面与水平方向的夹角为70°,进样日立8230冷场发射电镜进行EBSD衍射进行有效探测,在电压25-30KV,束流25-30μA,工作距离10-25mm。可以用此样品台EBSD检测正极电极片截面中正极材料颗粒扫描电镜图、EBSD衍射花样和花样解标定见图11-图13。
Claims (9)
1.一种EBSD测试样品台,包括夹具体(1)和底座(100),夹具体(1)通过其底端设置在底座(100)上,其特征在于,所述夹具体(1)为直角梯形的四棱柱,所述夹具体(1)的四个侧端面沿其周向依次为第一端面(11)、第二端面(12)、第三端面(13)、第四端面(14),所述第一端面(11)作为夹具体(1)的工作面,其与夹具体(1)的底端呈70°夹角,所述夹具体(1)上开有至少一开槽(2),所述开槽(2)分别与第一端面(11)、第二端面(12)、第三端面(13)相连通;与所述夹具体(1)相配合的还设置有挡板(3),所述挡板(3)设置于所述开槽(2)中并与夹具体(1)可分离式连接,且挡板(3)的一侧端面作为工作端(31),挡板(3)的上表面作为薄片型样品的承载面(32),所述薄片型样品的厚度设为0.1um-5mm,所述挡板(3)的工作端(31)与所述第一端面(11)相平齐,薄片型样品置于挡板的承载面时,样品检测面与水平方向的夹角为70°。
2.根据权利要求1所述的EBSD测试样品台,其特征在于,所述夹具体(1)的高度不大于25mm。
3.根据权利要求1所述的EBSD测试样品台,其特征在于,所述开槽(2)的宽度为1-5mm。
4.根据权利要求1所述的EBSD测试样品台,其特征在于,所述挡板(3)的工作端(31)设有一补偿角α,开槽(2)与第一端面(11)的夹角设为β,β=90°±α。
5.根据权利要求4所述的EBSD测试样品台,其特征在于,α≤5°。
6.根据权利要求1所述的EBSD测试样品台,其特征在于,所述夹具体(1)底端设置有定位螺孔(4)及至少一固定螺孔(5),夹具体(1)通过螺柱与定位螺孔(4)相配合连接在底座(100)上,夹具体(1)通过螺钉与固定螺孔(5)相配合用于将挡板(3)固定在开槽(2)中。
7.根据权利要求1所述的EBSD测试样品台,其特征在于,所述挡板(3)相对于其工作端(31)的另一端设置有手柄(33)。
8.根据权利要求1所述的EBSD测试样品台,其特征在于,所述薄片型样品与挡板(3)之间通过导电胶带或导电银浆固定粘结相连。
9.一种如权利要求1-8任一项所述的EBSD测试样品台的应用,其特征在于,应用于日立SU8000系列冷场电镜中,用于薄片型样品的截面EBSD测试。
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