CN85105786A - 超微试样超薄片的制备 - Google Patents

超微试样超薄片的制备 Download PDF

Info

Publication number
CN85105786A
CN85105786A CN 85105786 CN85105786A CN85105786A CN 85105786 A CN85105786 A CN 85105786A CN 85105786 CN85105786 CN 85105786 CN 85105786 A CN85105786 A CN 85105786A CN 85105786 A CN85105786 A CN 85105786A
Authority
CN
China
Prior art keywords
sample
preparation
thin slice
negative electrode
ultra micro
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN 85105786
Other languages
English (en)
Other versions
CN85105786B (zh
Inventor
方克明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
University of Science and Technology Beijing USTB
Original Assignee
University of Science and Technology Beijing USTB
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by University of Science and Technology Beijing USTB filed Critical University of Science and Technology Beijing USTB
Priority to CN85105786A priority Critical patent/CN85105786B/zh
Publication of CN85105786A publication Critical patent/CN85105786A/zh
Publication of CN85105786B publication Critical patent/CN85105786B/zh
Expired legal-status Critical Current

Links

Images

Landscapes

  • Sampling And Sample Adjustment (AREA)

Abstract

本发明属于一种现代物理测试制样的新技术，是采用电镀的方法镶嵌超微试样，然后进行两面磨抛处理，制成的试样既薄又不损坏超微物体的组织结构，适合于微米数量级且脆性大的样品制备。其制成的样品薄片可以小于2000进行透射电镜测试时图象清晰，为利用现代物理测试仪对超微物体的微观分析研究提供了方便。

Description

本发明是一种现代物理测试制样的新技术。
随着现代科学技术的发展，新开拓的技术领域愈来愈广泛，同时对微观世界的研究也愈来愈重视，如要探查空气污染的尘埃的成份结构;要搞清物质合成时形成的新相;要分析钢中及其他合金中微量元素夹杂物等等，开展这方面的研究借助于现代物理测试仪器十分有效，但是由于研究的对象往往在微米数量级范围，所以在制备样品时，尤其是在制备透射电镜所需小于2000 超薄样品时十分困难。目前这种样品的制备一般采用离子溅射法，将样品打穿，然后利用孔边缘的薄层进行测试，但是这时的薄层不一定是所要研究的部位，另外溅射过程，试样温度升高和去掉了样品的一部分，致使所要研究的部位有可能被破坏掉。此方法不适用于超微和脆性试样。
本发明的目的在于克服上述方法的不足，制备的样品既薄又不破坏其组织的完整，适合于各种材料且大于5微米的微小物体，为超微物体制成超薄样品提供了一种新方法。
超微物体制成超薄样品的方法是在显微镜或扫描电镜下对需要制备的试样进行鉴定和选择，然后把试样（4）单层地放置在一个事先抛光的金属平台（2）上，将试样和平台一起水平放置在电镀槽（1）中。（见附图1）电镀液（3）含有四甲基氯化胺1-5%、三乙醇胺5-10%、丙三醇5-10%，余量为甲醇。镀液温度保持在10℃-18℃。载有试样的金属平台作为阴极，另一金属作为阳极（5）同样水平放置在电镀槽中，接通直流电，其阴极电流密度在3-10mA/cm2之间，此时阳极溶解，阴极平台上的试样被镀上一层金属膜，待电镀将试样全部覆盖后，取出阴极，磨抛掉试样的一半。在磨抛过的平面上再镀一层金属，然后取出试样磨抛掉另一面，直至所需厚度。这时继续将带有金属基体的试样作为阳极进行电解（见附图2），样品薄片随阳极溶解而从金属基体上脱落下来。
实施例：将球墨铸铁中离析出来的直径为20μm的球状石墨单层地放置在阴极铜台上进行电镀，镀后试样镶入金属铜中，再经过二面抛光制成薄片，在透射电镜下可清楚地看到每一球状石墨的真正核心（见照片1）与其薄片的衍射图象（见照片2）。

Claims (6)

1、一种超微试样超薄片的制备方法，其特征在于用电镀的方法镶样，
a)阴极电流密度范围是3-10mA/cm2。
b)镀液温度保持在10℃-18℃。
c)镀液成份为：四甲基氯化铵1-5%、三乙醇胺5-10%、丙三醇5-10%，余量为甲醇。
2、如权利要求1所述方法，其特征在于超微试样单层地镶嵌在阴极载物台上。
3、如权利要求1、2所述的方法，其特征在于阴极载物台水平放置在镀槽中。
4、如权利要求3所述的阴极载物台，其特征在于表面抛光。
5、如权利要求，1、2所述方法，其特征在于将镶好的试样进行磨抛处理，然后在此抛光面镀上一层金属继续磨抛另一面，直接制成小于2000
Figure 85105786_IMG2
的样品薄片。
6、如权利要求5所述的方法，其特征在于将制成的样品薄片作为阳极进行电解，样品薄片随阳极溶解脱落而取出。
CN85105786A 1985-07-30 1985-07-30 超微试样超薄片的制备 Expired CN85105786B (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN85105786A CN85105786B (zh) 1985-07-30 1985-07-30 超微试样超薄片的制备

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN85105786A CN85105786B (zh) 1985-07-30 1985-07-30 超微试样超薄片的制备

Publications (2)

Publication Number Publication Date
CN85105786A true CN85105786A (zh) 1987-01-28
CN85105786B CN85105786B (zh) 1987-03-18

Family

ID=4794706

Family Applications (1)

Application Number Title Priority Date Filing Date
CN85105786A Expired CN85105786B (zh) 1985-07-30 1985-07-30 超微试样超薄片的制备

Country Status (1)

Country Link
CN (1) CN85105786B (zh)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100593706C (zh) * 2007-03-29 2010-03-10 上海大学 电解法提取钢中超细夹杂物的方法
CN105865869A (zh) * 2016-04-05 2016-08-17 山东大学 一种异质界面材料电镜观察样品制备方法
CN109490347A (zh) * 2018-10-12 2019-03-19 中国航发北京航空材料研究院 一种钛铝合金粉末透射样品的制备方法
CN113432943A (zh) * 2021-06-17 2021-09-24 攀钢集团攀枝花钢铁研究院有限公司 一种岩矿样透射光片的制备方法

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100593706C (zh) * 2007-03-29 2010-03-10 上海大学 电解法提取钢中超细夹杂物的方法
CN105865869A (zh) * 2016-04-05 2016-08-17 山东大学 一种异质界面材料电镜观察样品制备方法
CN105865869B (zh) * 2016-04-05 2019-02-12 山东大学 一种异质界面材料电镜观察样品制备方法
CN109490347A (zh) * 2018-10-12 2019-03-19 中国航发北京航空材料研究院 一种钛铝合金粉末透射样品的制备方法
CN113432943A (zh) * 2021-06-17 2021-09-24 攀钢集团攀枝花钢铁研究院有限公司 一种岩矿样透射光片的制备方法

Also Published As

Publication number Publication date
CN85105786B (zh) 1987-03-18

Similar Documents

Publication Publication Date Title
Samuels Metallographic polishing by mechanical methods
Heilmann et al. Sliding wear and transfer
CN105865869B (zh) 一种异质界面材料电镜观察样品制备方法
Huang et al. Electrodeposition of a protective copper/nickel deposit on the magnesium alloy (AZ31)
Lechtman A pre-Columbian technique for electrochemical replacement plating of gold and silver on copper objects
Konieczny et al. The influence of cast method and anodizing parameters on structure and layer thickness of aluminium alloys
Torabinejad et al. Tribological behavior of electrodeposited Ni-Fe multilayer coating
CN85105786A (zh) 超微试样超薄片的制备
Chang et al. Electrodeposition of Ni–P Alloys From a Sulfamate Electrolyte: Relationship Between Bath pH and Structural Characteristics
Braunovic et al. Surface analysis of fretting damage in electrical contacts of aluminum with different contact materials
Leidheisee et al. Bright Nickel Plating on Metallic Single Crystals in the Absence of Addition Agent
CN105300761B (zh) 小尺寸金属材料的tem电解双喷薄膜样品的制备方法
CN109490347A (zh) 一种钛铝合金粉末透射样品的制备方法
Sekar Effect of saccharin and thiourea on electrodeposition of cobalt and characteristics of deposits
Roy et al. New combination of polishing and etching technique for revealing grain structure of an annealed aluminum (AA1235) alloy.
Schwartz et al. A Positive‐Replica Technique for Electron Microscopy
Niu et al. Cross‐section metal sample preparations for transmission electron microscopy by electro‐deposition and electropolishing
Cherneva et al. Characterisation of mechanical properties of electrochemically deposited thin silver layers
Jegan Pulse eletrodeposition of Ni/nano-Al2O3 composite coatings on cast iron cylinder liner
Giallourakis et al. A cryogenic fracture technique for characterizing zinc-coated steels
Cleghorn et al. Some Structural Properties of Bright Gold Electrodeposits
CN218567027U (zh) 一种便于阳极化制膜的铝及铝合金金相样品
CN112378722B (zh) 一种铝/过渡层/铅合金/PbO2复合棒的金相样品快速制备方法
Fazel et al. The influence of temperature on tribological behaviour of Ni-SiC Electrodeposited coating
Kirchoff et al. Thinning of aluminum powder particles for transmission electron microscopy

Legal Events

Date Code Title Description
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
PB01 Publication
C06 Publication
C13 Decision
GR02 Examined patent application
C14 Grant of patent or utility model
GR01 Patent grant
C19 Lapse of patent right due to non-payment of the annual fee
CF01 Termination of patent right due to non-payment of annual fee