CN101236143A - Method for preparing scanning electron microscope sample by ion beam bombing - Google Patents
Method for preparing scanning electron microscope sample by ion beam bombing Download PDFInfo
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- 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
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Abstract
A preparing method of a scanning electron microscope sample bombarded by ion beams relates to the preparing of the scanning electron microscope sample. The method is as follows: argon gas is continuously charged in under the condition of microvac 2x10<-3>Pa, the argon gas is ionized through an ion gun under the action of a high voltage field to obtain ion beams bombarding the surface of the sample, and the sample simultaneously rotates in 360 DEG to ensure an even bombarding on the surface of the sample. The included angle between the surface of the sample and the ion beams is generally a range from 7 DEG to 12 DEG, the bombarding voltage of the ion gun is a range from 4 kilovolt to 7 kilovolt, and the ion beams fall into a range from 0.4 milliampere to 0.5 milliampere. The method which is free of the impact of the sample material electrical property and does not bring about stress and strain to the sample during the bombarding process of the ion beams and also has no damage on the self crystal structure of the material is suitable for microscopic shape and appearance analysis of metals and nonmetal materials.
Description
Technical field
The present invention relates to the preparation of scanning electron microscope sample, particularly adopt the ion beam bombardment legal system to be equipped with the scanning electron microscope sample.
Background technology
Scanning electron microscope is to carry out microscopic appearance in the material science research to analyze indispensable means.Yet the preparation of sample is particularly important, and method of sample preparation and process are to ensure the important channel that obtains complete real information.
What people generally used usually is metallographic method and electrolytic etching method.Metallographic method to soft material and the artificial manufacturing defect of simple metal material, can make airborne dust granules be inlaid in the sample easily, and experimental result is created smoke screens to do.Metallographic method is powerless especially to the preparation of electronic information material " integrated chip " micron order circuit and solder joint sample.
Introduced traditional sample preparation methods in " material structure Electronic Micro-Analysis " [publishing house of work University Of Tianjin such as Liu Wenxi 1989]; as can be known; electrolytic etching method only limits to metal material; alloy and simple metal to the different chemical element need select several chemical reagent to be mixed with electrolytic solution, and the post-processed of waste liquid also relates to the constraint of Law on Environmental Protection.The temperature of electrolytic solution and the selection of voltage and current parameter play an important role to preparation high-quality sample, therefore need pay a large amount of time and sample is groped.The active easily migration of some element in the electrolytic corrosion process sample can cause the experimental program that misleads the back of losing of information.
Summary of the invention
The present invention proposes to adopt the ion beam bombardment legal system to be equipped with the scanning electron microscope sample, be not subjected to the influence of sample material electrical property, promptly no matter whether material conducts electricity, whether crystal structure complicated, all can prepare and meet the sample that scanning electron microscope requires, and in the ion beam bombardment process, can not bring stress and strain to sample, to material self crystal structure not damaged, be suitable for the microscopic appearance analysis of metal and nonmetal various types of materials.
The concrete grammar that the ion beam bombardment legal system is equipped with the scanning electron microscope sample is: at condition of high vacuum degree 2 * 10
-3Under the Pa condition, utilize argon gas (inert gas) to obtain argon ion by ion gun ionization under the high-voltage electric field effect, sample is constantly charged into argon gas by the bombardment process, the argon ion line that ionization is formed bombards specimen surface, sample stage self 360 degree rotations simultaneously obtain evenly bombardment to ensure specimen surface.
Angle between specimen surface and the ion beam current (inclination angle) selects 7 degree to 12 degree scopes usually, and ion gun bombarding voltage (Kv) is selected 4 kilovolts to 7 kilovolt range, and line is 0.4 to 0.5 milliampere of scope.
During the ion bombardment, can ensure that the low-temperature sensitive sample carries out the ion bombardment at subzero 30 degree environment, and can not destroy the structure of low-temperature sensitive material by the cooled with liquid nitrogen device of sample stage installation.
The ion beam bombardment method has overcome the defective of metallographic method and electrolytic etching method existence.The great advantage of its method is that the atomic layer that has material surface " degrades " function.Can clean slightly making uncleanly surfacing, also machine work (grinding hardened layer) " degrading " in layer can be exposed " fresh " matrix that the researcher wants the observation aspect.To containing microfissure and stress corrosion cracking (SCC), and contain the special sample that stress produces strain and be fit to ion beam bombardment equally, make its crack tip clear-cut.
The sample that the ion beam bombardment legal system is equipped with EBSD (EBSD) requirement demonstrates unique effect.Investigation of materials person knows that crystal orientation is present in the phase transformation of the deformation of material, material and the recrystallization process of material, the crystal orientation that the researcher pays close attention to material in order to the production technology of control material to reach the physical property that the user requires.Use the ion beam bombardment method can obtain desirable (EBSD) sample, ion beam can be removed any residue of sample surfaces and show the intercrystalline interface is clear, and the crystal structure of sample is not had influence.
The ion beam bombardment legal system is equipped with the research that scanning electron microscope sample technology can be widely used in materials such as electric aluminum foil, magnalium, diamond thin, integrated chip, ore deposit rock, glass fibre, and therefrom obtains the information of lot of materials crystal structure aspect.
Embodiment
Sample requires: cleaning surfaces, smooth, oil stains-less.
Method of operating: at first sample is positioned on the sample stage, bombardment chamber vacuum tightness reaches 2 * 10
-3Meet ion bombardment condition of work during Pa.Sample is constantly charged into argon gas by the bombardment process, sample stage self 360 degree rotations simultaneously.
Determine angle between sample and the ion beam (inclination angle), select ion gun bombarding voltage (Kv) and ion beam current (mA), determine bombardment time according to experiment purpose, empirical evidence hard material bombardment time is longer, and the soft material bombardment time will be lacked.
| Title material | Inclination angle (degree) | Voltage (Kv) | Ion beam current (mA) | Bombardment time (hour) |
| (soft attitude) fine aluminium | 12 | 5 | 0.4 | 2 |
| (hard attitude) fine aluminium | 12 | 6 | 0.5 | 6 |
| Magnesium alloy | 7 | 4.5 | 0.4 | 0.3-0.5 |
| Diamond thin | 10 | 7 | 0.6 | 10 |
| Integrated chip | 10 | 4 | 0.4 | 0.5 |
| The ore deposit rock | 12 | 5 | 0.5 | 1 |
| Glass fibre | 7 | 4.5 | 0.4 | 0.5 |
| Ferroalloy | 12 | 5 | 0.4 | 3 |
| Nickel alloy | 12 | 6 | 0.5 | 2 |
| Titanium alloy | 10 | 6 | 0.5 | 4 |
| Aldary | 10 | 4.5 | 0.4 | 1.5 |
| The PVC plastics | 12 | 4.5 | 0.4 | 1 |
Claims (2)
1, a kind of method of preparing scanning electron microscope sample by ion beam bombing is characterized in that, at condition of high vacuum degree 2 * 10
-3Under the Pa condition, constantly charge into argon gas, argon gas obtains the argon ion line by ion gun ionization under the high-voltage electric field effect and bombards specimen surface, sample stage self 360 degree rotations simultaneously, angle between specimen surface and the ion beam current selects 7 degree to 12 degree scopes usually, the ion gun bombarding voltage is selected 4 kilovolts to 7 kilovolt range, and line is 0.4 to 0.5 milliampere of scope.
2, the method for preparing scanning electron microscope sample by ion beam bombing as claimed in claim 1 is characterized in that, the temperature when sample stage reduces the ion bombardment by the cooled with liquid nitrogen device of installing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101008753A CN101236143A (en) | 2008-02-25 | 2008-02-25 | Method for preparing scanning electron microscope sample by ion beam bombing |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008101008753A CN101236143A (en) | 2008-02-25 | 2008-02-25 | Method for preparing scanning electron microscope sample by ion beam bombing |
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| CN101236143A true CN101236143A (en) | 2008-08-06 |
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| CNA2008101008753A Pending CN101236143A (en) | 2008-02-25 | 2008-02-25 | Method for preparing scanning electron microscope sample by ion beam bombing |
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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 | Tilt angle amount calculation device, sample stage, charged particle beam device, and program |
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Open date: 20080806 |