CN101236143A - A method for preparing scanning electron microscope samples by ion beam bombardment - Google Patents
A method for preparing scanning electron microscope samples by ion beam bombardment Download PDFInfo
- Publication number
- CN101236143A CN101236143A CNA2008101008753A CN200810100875A CN101236143A CN 101236143 A CN101236143 A CN 101236143A CN A2008101008753 A CNA2008101008753 A CN A2008101008753A CN 200810100875 A CN200810100875 A CN 200810100875A CN 101236143 A CN101236143 A CN 101236143A
- Authority
- CN
- China
- Prior art keywords
- sample
- ion beam
- scanning electron
- electron microscope
- ion
- 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.)
- Pending
Links
- 238000010884 ion-beam technique Methods 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 25
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052786 argon Inorganic materials 0.000 claims abstract description 10
- 239000007789 gas Substances 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000010849 ion bombardment Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 2
- 230000005684 electric field Effects 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000523 sample Substances 0.000 abstract description 32
- 239000000463 material Substances 0.000 abstract description 17
- 239000013078 crystal Substances 0.000 abstract description 7
- 238000004458 analytical method Methods 0.000 abstract description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 3
- 239000002184 metal Substances 0.000 abstract description 3
- 150000002739 metals Chemical class 0.000 abstract description 2
- 229910052755 nonmetal Inorganic materials 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 description 8
- 230000007797 corrosion Effects 0.000 description 5
- 238000005260 corrosion Methods 0.000 description 5
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 229910003460 diamond Inorganic materials 0.000 description 2
- 239000010432 diamond Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000001887 electron backscatter diffraction Methods 0.000 description 2
- 239000003365 glass fiber Substances 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- 239000007779 soft material Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910000640 Fe alloy Inorganic materials 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- 229910000990 Ni alloy Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 description 1
- -1 argon ions Chemical class 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000002003 electron diffraction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000004452 microanalysis Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Sampling And Sample Adjustment (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
Abstract
Description
技术领域technical field
本发明涉及扫描电子显微镜试样的制备，特别涉及采用离子束轰击法制备扫描电子显微镜试样。The invention relates to the preparation of scanning electron microscope samples, in particular to the preparation of scanning electron microscope samples by ion beam bombardment.
背景技术Background technique
扫描电子显微镜是材料科学研究中进行微观形貌分析不可缺少的手段。然而试样的制备尤为重要，试样的制备方法及过程是保障获得完整真实信息的重要途径。Scanning electron microscopy is an indispensable means for microscopic morphology analysis in material science research. However, the preparation of the sample is particularly important, and the preparation method and process of the sample are an important way to ensure complete and true information.
通常人们普遍使用的是金相法以及电解腐蚀法。金相法容易对软体材料及纯金属材料人为制造缺陷，可使空气中的粉尘颗粒镶嵌入试样中，对实验结果制造假象。金相法对电子信息材料“集成芯片”微米级电路及焊点试样的制备更是无能为力。Generally, metallographic methods and electrolytic corrosion methods are commonly used. Metallographic method is easy to artificially create defects on soft materials and pure metal materials, which can cause dust particles in the air to be embedded in the sample and create false impressions on the experimental results. Metallographic method is powerless to the preparation of electronic information material "integrated chip" micron circuit and solder joint samples.
《材料结构电子显微分析》[刘文西 等著 天津大学出版社 1989年]中介绍了传统的样品制备方法，可知，电解腐蚀法仅限于金属材料，对不同化学元素的合金及纯金属需要选择几种化学试剂配制成电解液，废液的后期处理还涉及到环境保护法的约束。电解液的温度及电压电流参数的选择对制备高质量试样起着重要作用，因此需要付出大量的时间及样品进行摸索。电解腐蚀过程试样中的某些元素活泼易迁移会造成信息的丢失误导后面的实验方案。"Material Structure Electron Microanalysis" [Liu Wenxi et al. Tianjin University Press 1989] introduced the traditional sample preparation method. It can be seen that the electrolytic corrosion method is limited to metal materials, and it is necessary to select several alloys and pure metals with different chemical elements. Various chemical reagents are prepared into electrolyte, and the post-treatment of waste liquid also involves the constraints of environmental protection laws. The temperature of the electrolyte and the selection of voltage and current parameters play an important role in the preparation of high-quality samples, so it takes a lot of time and samples to explore. Some elements in the sample during electrolytic corrosion are active and easy to migrate, which will cause the loss of information and mislead the subsequent experimental plan.
发明内容Contents of the invention
本发明提出采用离子束轰击法制备扫描电子显微镜试样，不受试样材料电性能的影响，即无论材料是否导电、晶体结构是否复杂，均可制备出符合扫描电镜要求的试样，并且在离子束轰击过程中不会给试样带来应力和应变，对材料自身晶体结构无损伤，适合于金属及非金属各类材料的微观形貌分析。The present invention proposes to use the ion beam bombardment method to prepare the scanning electron microscope sample, which is not affected by the electrical properties of the sample material, that is, no matter whether the material is conductive or not, and the crystal structure is complex, the sample that meets the requirements of the scanning electron microscope can be prepared. The ion beam bombardment process will not bring stress and strain to the sample, and will not damage the crystal structure of the material itself. It is suitable for microscopic morphology analysis of various metal and non-metal materials.
离子束轰击法制备扫描电子显微镜试样的具体方法是：在高真空度2×10-3Pa条件下，利用氩气(惰性气体)通过离子枪在高压电场作用下电离获得氩离子，试样被轰击过程不断充入氩气，使电离形成的氩离子束流轰击到试样表面，同时样品台自身360度旋转，以保障试样表面获得均匀轰击。The specific method for preparing scanning electron microscope samples by ion beam bombardment is: under the condition of high vacuum degree of 2×10 -3 Pa, use argon (inert gas) to ionize under the action of high voltage electric field through ion gun to obtain argon ions. During the bombardment process, argon gas is continuously filled, so that the argon ion beam formed by ionization bombards the surface of the sample, and at the same time, the sample stage itself rotates 360 degrees to ensure that the surface of the sample is bombarded uniformly.
试样表面与离子束流之间的夹角(倾角)通常选择7度至12度范围，离子枪轰击电压(Kv)选择4千伏至7千伏范围，束流在0.4至0.5毫安范围。The included angle (tilt angle) between the sample surface and the ion beam is usually in the range of 7 degrees to 12 degrees, the ion gun bombardment voltage (Kv) is selected in the range of 4 kV to 7 kV, and the beam current is in the range of 0.4 to 0.5 mA .
离子轰击时，可以通过样品台安装的液氮冷却装置，保障低温敏感试样在零下30度环境进行离子轰击，而不会破坏低温敏感材料的结构。During ion bombardment, the liquid nitrogen cooling device installed on the sample stage can ensure that the low temperature sensitive sample is subjected to ion bombardment in an environment of minus 30 degrees without destroying the structure of the low temperature sensitive material.
离子束轰击法克服了金相法以及电解腐蚀法存在的缺陷。其方法的最大优点是具有将材料表面的原子层“剥蚀”功能。可将粗造不清洁的表面平整清洗，也可将机加工(研磨硬化层)一层一层的“剥蚀掉”，裸露出研究者想要观察层面的“新鲜”基体。对含有微观裂纹及应力腐蚀裂纹，以及含有应力产生应变的特殊试样同样适合离子束轰击，使其裂纹尖端轮廓清晰。The ion beam bombardment method overcomes the defects of the metallographic method and the electrolytic corrosion method. The biggest advantage of its method is that it has the function of "ablating" the atomic layer on the surface of the material. The rough and unclean surface can be cleaned evenly, or the machining (grinding hardened layer) can be "eroded" layer by layer, exposing the "fresh" substrate of the layer that the researcher wants to observe. It is also suitable for ion beam bombardment for special samples containing microscopic cracks and stress corrosion cracks, as well as stress-induced strains, so that the crack tip outline is clear.
离子束轰击法制备背散射电子衍射(EBSD)要求的试样显示出独特的功效。材料研究者知道晶体取向存在于材料的形变、材料的相变和材料的再结晶过程，研究者关注材料的晶体取向用以控制材料的生产工艺以达到使用者要求的物理性能。使用离子束轰击法可获得理想的(EBSD)样品，离子束可清除样品表面任何残留物将晶粒间界面清晰展现出来，对试样的晶体结构无影响。Ion beam bombardment preparation of samples required for backscattered electron diffraction (EBSD) shows unique efficacy. Materials researchers know that crystal orientation exists in the deformation, phase transition and recrystallization process of materials. Researchers pay attention to the crystal orientation of materials to control the production process of materials to achieve the physical properties required by users. The ideal (EBSD) sample can be obtained by ion beam bombardment. The ion beam can remove any residue on the surface of the sample and clearly display the interface between grains without affecting the crystal structure of the sample.
离子束轰击法制备扫描电子显微镜试样技术可广泛用于电子铝箔、镁铝合金、金刚石薄膜、集成芯片、矿岩、玻璃纤维等材料的研究，并从中获得大量材料晶体结构方面的信息。Ion beam bombardment method to prepare scanning electron microscope sample technology can be widely used in the research of electronic aluminum foil, magnesium aluminum alloy, diamond film, integrated chip, ore rock, glass fiber and other materials, and obtain a lot of information on the crystal structure of materials.
具体实施方式Detailed ways
试样要求：表面清洁、平整、无油迹。Sample requirements: the surface is clean, smooth and free of oil stains.
操作方法：首先将试样放置于样品台上，轰击室真空度达到2×10-3Pa时符合离子轰击工作条件。试样被轰击过程不断充入氩气，同时样品台自身360度旋转。Operation method: first place the sample on the sample stage, when the vacuum degree of the bombardment chamber reaches 2×10 -3 Pa, it meets the working conditions of ion bombardment. The sample is continuously filled with argon during the bombardment process, and the sample stage itself rotates 360 degrees.
确定样品与离子束之间夹角(倾角)，选择离子枪轰击电压(Kv)及离子束流(mA)，依据实验目的确定轰击时间，经验证明硬质材料轰击时间要长一些，软质材料轰击时间要短一些。Determine the angle (inclination) between the sample and the ion beam, select the ion gun bombardment voltage (Kv) and ion beam current (mA), and determine the bombardment time according to the purpose of the experiment. Experience has proved that the bombardment time for hard materials is longer, and for soft materials The bombardment time is shorter.
Claims (2)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101008753A CN101236143A (en) | 2008-02-25 | 2008-02-25 | A method for preparing scanning electron microscope samples by ion beam bombardment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101008753A CN101236143A (en) | 2008-02-25 | 2008-02-25 | A method for preparing scanning electron microscope samples by ion beam bombardment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101236143A true CN101236143A (en) | 2008-08-06 |
Family
ID=39919914
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2008101008753A Pending CN101236143A (en) | 2008-02-25 | 2008-02-25 | A method for preparing scanning electron microscope samples by ion beam bombardment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101236143A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105699149A (en) * | 2016-04-05 | 2016-06-22 | 工业和信息化部电子第五研究所 | Layer stripping method in chip failure analysis process |
| CN106233420A (en) * | 2014-05-09 | 2016-12-14 | 株式会社日立高新技术 | sample processing method and charged particle beam apparatus |
| CN106646746A (en) * | 2015-11-02 | 2017-05-10 | 中国兵器装备研究院 | Fine processing method for end face of optical fiber |
| CN110998780A (en) * | 2017-05-31 | 2020-04-10 | 日本制铁株式会社 | Tilt angle amount calculation device, sample stage, charged particle beam device, and program |
-
2008
- 2008-02-25 CN CNA2008101008753A patent/CN101236143A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106233420A (en) * | 2014-05-09 | 2016-12-14 | 株式会社日立高新技术 | sample processing method and charged particle beam apparatus |
| CN106233420B (en) * | 2014-05-09 | 2018-10-16 | 株式会社日立高新技术 | Sample processing method and charged particle beam apparatus |
| CN106646746A (en) * | 2015-11-02 | 2017-05-10 | 中国兵器装备研究院 | Fine processing method for end face of optical fiber |
| CN106646746B (en) * | 2015-11-02 | 2020-06-16 | 中国兵器装备研究院 | Fine processing method for optical fiber end face |
| CN105699149A (en) * | 2016-04-05 | 2016-06-22 | 工业和信息化部电子第五研究所 | Layer stripping method in chip failure analysis process |
| CN110998780A (en) * | 2017-05-31 | 2020-04-10 | 日本制铁株式会社 | Tilt angle amount calculation device, sample stage, charged particle beam device, and program |
| CN110998780B (en) * | 2017-05-31 | 2022-07-01 | 日本制铁株式会社 | Inclination angle amount calculation device, sample stage, charged particle beam device and program |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Feng et al. | Different role of second phase in the micro-galvanic corrosion of WE43 Mg alloy in NaCl and Na2SO4 solution | |
| Huang et al. | A high-strength and biodegradable Zn–Mg alloy with refined ternary eutectic structure processed by ECAP | |
| TW467958B (en) | Improved target for use in magnetron sputtering of aluminum for forming metalliztion films having low defect densities and methods for manufacturing and using such target | |
| US20150197848A1 (en) | Sputtering Target | |
| Wang et al. | Surface integrity of alumina machined by electrochemical discharge assisted diamond wire sawing | |
| Xue et al. | The crystallographic texture and dependent mechanical properties of the CrCoNi medium-entropy alloy by laser remelting strategy | |
| CN103572225A (en) | Production method of tantalum target and tantalum target component | |
| CN101236143A (en) | A method for preparing scanning electron microscope samples by ion beam bombardment | |
| CN103572223A (en) | Production method of tantalum target and tantalum target component | |
| CN103572224A (en) | Production method of nickel target and nickel target component | |
| JP4563966B2 (en) | Semiconductor processing apparatus member and method for manufacturing the same | |
| Hu et al. | The effect of neodymium on the microcracks generated on the Al–17.5 Si alloy surface treated by high current pulsed electron beam | |
| Kim et al. | Direct energy deposition of high strength austenitic stainless steel matrix nanocomposite with superior ductility: Microstructure, tensile properties, and deformation behavior | |
| Hsu et al. | The improved stability and corrosion resistance of the passive film on Mn-containing FeCrNiCoMnx high entropy alloys by multiple pickling | |
| Xue et al. | Influence of impurity content on corrosion behavior of Al-Zn-Mg-Cu alloys in a tropical marine atmospheric environment | |
| Li | Advanced techniques in TEM specimen preparation | |
| Ma | Comparison of different sample preparation techniques in TEM observation of microstructure of INCONEL alloy 783 subjected to prolonged isothermal exposure | |
| US10518329B2 (en) | Method of making nanocrystalline metal flakes and nanocrystalline flakes made therefrom | |
| Liu et al. | Corrosion behavior of tantalum alloying on γ‐TiAl by double‐glow plasma surface metallurgy technique | |
| Wu et al. | EBSD study of (1 1 0) orientation of iridium (Ir) coating on niobium (Nb) substrate by double glow plasma | |
| Ghorbanian et al. | Investigation of the electrolyte effects on formation of vanadium carbide via plasma electrolytic saturation method (pes) | |
| CN113529080B (en) | Coating for PCB micro milling cutter | |
| Huang et al. | Sinter-joining of W-10Ti powder to W-10Ti waste target by spark plasma sintering | |
| CN116240440A (en) | An in-situ precipitation self-strengthening and toughening MoCrTiAlC system refractory high-entropy alloy and its preparation method | |
| Mehmood et al. | Effect of electric discharge machining on material removal rate and white layer composition |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20080806 |