CN110487823B - 一种粉末颗粒透射电子显微镜试样的制备方法 - Google Patents

一种粉末颗粒透射电子显微镜试样的制备方法 Download PDF

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CN110487823B
CN110487823B CN201910743711.0A CN201910743711A CN110487823B CN 110487823 B CN110487823 B CN 110487823B CN 201910743711 A CN201910743711 A CN 201910743711A CN 110487823 B CN110487823 B CN 110487823B
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孙崇锋
席生岐
李建平
郭永春
杨忠
朱蕊花
白亚平
高圆
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Abstract

本发明属于透射电子显微镜（TEM）样品制备技术领域,具体涉及一种粉末颗粒透射电子显微镜试样的制备方法。本发明要提供一种粉末颗粒透射电子显微镜试样的制备方法，以克服现有技术存在的工艺复杂、制备TEM样品薄区范围小和制样成本高的问题。为了达到上述目的，本发明提供的解决方案是：通过在不含磁性的支撑泡沫结构中镶嵌粉末颗粒进而离子减薄获得具有较多薄区的TEM样品。该方法简单易行、成本低，可获得具有较多薄区的TEM粉末样品。本发明适用于各种常规颗粒，颗粒粒径尺寸为亚微米、微米或亚毫米级；同时，本发明具有通用性，不仅适合金属颗粒，也适合非金属颗粒。

Description

一种粉末颗粒透射电子显微镜试样的制备方法
技术领域：
本发明属于透射电子显微镜（TEM）样品制备技术领域, 具体涉及一种粉末颗粒透射电子显微镜试样的制备方法。
背景技术：
透射电子显微镜在材料科学与工程等相关科学研究方面应用较多，TEM样品制备在电子显微学研究工作中起到了非常重要的技术支撑作用。由于电子易散射或被物体吸收，其穿过TEM试样时存在穿透力低的特点，因而样品的厚度会显著影响TEM试样的成像质量。想要得到满意的TEM观察效果，首先要制备出好的薄膜样品。因而，在TEM试样上获得具有较大面积的超薄区域（薄区厚度小于100nm）是进行有效TEM观察（尤其是高分辨透射电子显微镜HRTEM观察）的前提条件。
根据材料样品的形状和尺寸，可以将其分为：块体材料、纳米材料（纳米薄膜、纳米线和纳米颗粒）和常规粉末材料（粉末颗粒粒径在亚微米、微米甚至亚毫米尺度）。对于常规粉末材料，其颗粒粒度通常在亚毫米、微米、亚微米尺度，粉末颗粒粒度较大，之前通常使用捞粉法制备TEM试样进行透射观察，由于颗粒尺寸较大，粉末颗粒的边缘几乎不存在薄区或者薄区非常小，很难获得满意的TEM观察效果。因而，获得较大面积的薄区且薄区厚度进一步降低成为粉末材料TEM试样制备的重要技术难题。
目前，除了捞粉法制备粉末材料TEM试样，还可以将粉末通过树脂等有机物对粉末颗粒进行包埋，进而对包埋的粉末进行离子减薄；或者对粉末颗粒进行化学/电镀，进而对镶嵌有样品粉末颗粒的薄膜进行离子减薄。以上两种方式最终都可以获得具有一定厚度的薄区。然而，以上两种方法都存在各自的不足之处。一、树脂材料和粉末颗粒，尤其是无机非金属和金属颗粒的润湿性很差，导致粉末颗粒和树脂的界面强度很低，甚至存在较大裂纹。颗粒与树脂基体之间低的界面强度和裂纹，导致在离子减薄孔洞周围（即薄区周围）很容易发生脱落，最终获得薄区的镶嵌颗粒较少，进而制样成功率不高/制样效果较差。二、电镀和化学镀制备粉末颗粒TEM试样方法可以在一定程度上克服上述树脂材料和粉末颗粒界面机械咬合强度低的问题，国外的R.D. Field、H.L. Fraser、A.M. Ritter、M.F. Henry、北京科技大学的胡本芙教授等人及团队分别通过在铜板上固定粉末颗粒，进行化学镀和电镀，最终获得镶嵌有粉末颗粒的薄膜，从而进行离子减薄，获得了具有一定薄区的粉末颗粒TEM试样。对于化学镀和电镀两种方法，镀层为金属薄膜，其与粉末颗粒（主要指无机非金属和金属粉末颗粒）的界面结合强度尚可，但是化学镀和电镀过程工艺复杂、影响因素相对较多、成本相对高。
发明内容：
本发明要提供一种粉末颗粒透射电子显微镜试样的制备方法，以克服现有技术存在的工艺复杂、影响因素较多和成本高的问题。
为了达到上述目的，本发明提供的解决方案是：
一种粉末颗粒透射电子显微镜试样的制备方法，包括以下步骤：
1）根据粉末颗粒的粒径尺寸选择平均孔洞尺寸略大于颗粒平均粒径的不含磁性的支撑泡沫结构，泡沫金属网的厚度为0.1mm-1mm，剪取可获得至少一个φ3mm面积的泡沫方形网备用；
2）取少量样品粉末均匀洒落在泡沫网上，粉末层厚度为泡沫网厚度的1/5-1/4为宜；
3）将泡沫网放于平台上，敲击或震动平台，使得粉末颗粒逐渐漏入泡沫网的孔洞中；
4）用镊子轻拿内部镶嵌有粉末颗粒的泡沫网，加压将泡沫网压扁；
5）压缩泡沫网按在砂纸上打磨，获得薄片；
6）将薄片放于TEM试样打孔器中，获得圆形薄片；
7）对圆形薄片进行离子减薄，即可获得薄区质量良好的TEM试样。
上述步骤5）中，薄片厚度为20μm-50μm。
上述步骤1）中，支撑泡沫结构是泡沫铜或者镍网。
与现有技术相比，本发明的优点是：
1、方法简单，通过镶嵌粉末颗粒进而离子减薄获得具有较多薄区的TEM粉末样品。镶嵌粉末过程中使用立体中空的泡沫金属铜或者镍网，它们本身具有较多孔隙可以容纳较多粉末颗粒，可以对粉末样品进行初步过滤，使较多较小的粉末颗粒进入孔洞并在后面加压过程中镶嵌于其中；其次，这两种金属网具有优异的塑韧性，可以对嵌在压缩后金属网状结构中的颗粒起到较好的机械咬合作用，防止粉末颗粒在后期的离子减薄过程中被离子束轰击掉落，这种机械咬合作用显著强于树脂、塑性较好的铝箔等对粉末颗粒的机械咬合作用。
2、相比于传统捞粉法，该方法中增加了离子减薄这一过程，对于除纳米尺度以外的颗粒，只有通过离子减薄才能获得较好薄区，直接捞粉很难有薄区供TEM观察。
3、本方法制备工艺简单，所用设备为通用设备，因此生产成本低。
4、本发明适用于各种常规颗粒，颗粒粒径尺寸为亚微米、微米或亚毫米级。具有通用性，不仅适合金属颗粒，也适合非金属颗粒。
附图说明：
图1是传统捞粉法获得的TEM照片；
图2是采用本发明方法获得的TEM照片；
图3是采用本发明方法获得的HRTEM照片。
具体实施方式：
下面将结合附图和实施例对本发明做详细地描述。
实施例1：
一种粉末颗粒透射电子显微镜试样的制备方法，包括以下具体步骤：
1）根据粉末颗粒的粒径尺寸选择平均孔洞尺寸略大于颗粒平均粒径的泡沫铜结构（注意：在进行TEM观察时候，具有磁性的样品会导致电子束散射，进而使得TEM照片清晰度变差），泡沫网的厚度为1mm，剪取5×5mm面积（经过后处理后可以获得至少一个φ3mm的TEM试样即可）的泡沫网备用；
2）使用棉棒粘取少量样品粉末，均匀洒落在泡沫网上，粉末层厚度为泡沫网厚度的1/4；
3）将载有少量样品粉末的泡沫网放于平台上，敲击平台，掌握好敲击力度，既使得粉末颗粒逐渐漏入泡沫网的孔洞中，又不至于粉末洒落与泡沫网之外的平台上；
4）用镊子轻拿内部镶嵌有粉末颗粒的泡沫网，将其放于液压钳上，加上50MPa的压强，将泡沫网压扁，使泡沫网结构紧紧的包住粉末颗粒或者使得粉末颗粒紧密镶嵌于压实的泡沫网中；
5）将镶嵌有粉末颗粒的压缩泡沫网按在砂纸上打磨，最终获得厚度为20μm的薄片；
6）将打磨后的薄片放于TEM试样打孔器中，获得φ3mm的圆形薄片；
7）对打孔器获得的圆形薄片进行离子减薄，即可获得薄区质量良好的TEM试样。
实施例2：
一种粉末颗粒透射电子显微镜试样的制备方法，包括以下具体步骤：
1）根据粉末颗粒的粒径尺寸选择平均孔洞尺寸略大于颗粒平均粒径的泡沫铜结构（注意：在进行TEM观察时候，具有磁性的样品会导致电子束散射，进而使得TEM照片清晰度变差），泡沫网的厚度为0.5mm，剪取5×5mm面积的泡沫网备用；
2）使用棉棒粘取少量样品粉末，均匀洒落在泡沫网上，粉末层厚度为泡沫网厚度的1/4；
3）将载有少量样品粉末的泡沫网放于平台上，敲击平台，掌握好敲击力度，既使得粉末颗粒逐渐漏入泡沫网的孔洞中，又不至于粉末洒落与泡沫网之外的平台上；
4）用镊子轻拿内部镶嵌有粉末颗粒的泡沫网，将其放于液压钳上，加上2MPa的压强，将泡沫网压扁，使泡沫网结构紧紧的包住粉末颗粒或者使得粉末颗粒紧密镶嵌于压实的泡沫网中；
5）将镶嵌有粉末颗粒的压缩泡沫网按在砂纸上打磨，最终获得厚度为40μm的薄片；
6）将打磨后的薄片放于TEM试样打孔器中，获得φ3mm的圆形薄片；
7）对打孔器获得的圆形薄片进行离子减薄，即可获得薄区质量良好的TEM试样。
上述实施例1为最佳实施例，通过实验，可以发现：参见图1，对于具有较大粒径的粉末颗粒，传统捞粉法获得的TEM试样薄区极少，获得的明场像不够清晰，难以进行高分辨透射电子显微镜（HRTEM）操作；使用本发明中的方法，获得的TEM照片如图2所示，可以发现，该方法中的试样经过镶嵌→机械减薄→离子减薄后，获得粉末颗粒的薄区较大，可以获得清晰的TEM明场像，同时可以进一步进行清晰地HRTEM观察，如图3所示。

Claims (3)

1.一种粉末颗粒透射电子显微镜试样的制备方法，其特征在于，包括以下步骤：
步骤1）、根据粉末颗粒的粒径尺寸选择平均孔洞尺寸略大于颗粒平均粒径的不含磁性的泡沫金属网，泡沫金属网的厚度为0.1mm-1mm，剪取可获得至少一个φ3mm面积的方形泡沫金属网备用；
步骤2）、取少量样品粉末均匀洒落在泡沫金属网上，粉末层厚度为泡沫金属网厚度的1/5-1/4为宜；
步骤3）、将泡沫金属网放于平台上，敲击或震动平台，使得粉末颗粒逐渐漏入泡沫金属网的孔洞中；
步骤4）、用镊子轻拿内部镶嵌有粉末颗粒的泡沫金属网，将其放于液压钳上，加压将泡沫金属网压扁；
步骤5）、压缩泡沫金属网按在砂纸上打磨，获得薄片；
步骤6）、将薄片放于TEM试样打孔器中，获得圆形薄片；
步骤7）、对圆形薄片进行离子减薄，即可获得薄区范围较大的TEM试样。
2.如权利要求1所述的粉末颗粒透射电子显微镜试样的制备方法，其特征在于：所述步骤5）中，薄片厚度为20μm-50μm。
3.如权利要求1或2所述的粉末颗粒透射电子显微镜试样的制备方法，其特征在于：所述步骤1）中，泡沫金属网是泡沫铜网或者泡沫镍网。
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