CN102854048A - Preparation method of transmitting sample with crack tip - Google Patents
Preparation method of transmitting sample with crack tip Download PDFInfo
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- CN102854048A CN102854048A CN2012103891244A CN201210389124A CN102854048A CN 102854048 A CN102854048 A CN 102854048A CN 2012103891244 A CN2012103891244 A CN 2012103891244A CN 201210389124 A CN201210389124 A CN 201210389124A CN 102854048 A CN102854048 A CN 102854048A
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Abstract
The invention relates to the technical field of material analysis, and particularly relates to a preparation method of a transmitting sample with a crack tip. The preparation method comprises the steps of a) performing electron beam imaging on a sample with cracks in a double-beam focused ion beam system, and finding the to-be-absorbed crack tip on the surface of the sample; b) depositing Pt in the crack tip area, and playing a protection role on the to-be-absorbed area; c) cutting the sample with the crack tip by means of V-shaped cutting; and d) welding the cut sample with the crack tip on a copper mesh, and performing ion beam thinning until the transparent transmitting sample is formed. Via the preparation method of the transmitting sample with the crack tip disclosed by the invention, the ion beam thinning can be accurately performed on the to-be-absorbed crack tip area, so that high-resolution imaging can be performed in the crack tip area; the preparation process is simple in operation and high in control accuracy; and the prepared transmitting sample is high in quality and high in success rate.
Description
Technical field
The present invention relates to the material analysis technical field, especially a kind of crack tip preparation of transmission samples.
Background technology
Ion milling and two kinds of technological means of twin-jet electropolishing polishing are adopted in the film sample preparation in the conventional material analysis process, wherein ion milling need to use Ion Beam Thinner, ion current is bombarded sample surfaces continuously with a certain incident angle, make the continuously sputter of sample surfaces atom, obtain at last needed film sample, this technology is more serious to the sample surfaces damage; It is less that another shortcoming is exactly thin district, the twin-jet electropolishing polishing needs to use two spray instrument, electrolytic solution is passed through two side nozzles, it is moderate to obtain a spray speed, two post liquid are symmetrical and at the state of straight line, the insertion specimen holder polishes, thereby reaches the effect of attenuate sample, and this technology is in the relatively more difficult grasp of attenuate later stage.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of crack tip preparation of transmission samples, this preparation method can be accurately, easily the ion beam attenuate is carried out in its crack tip zone that will observe, make the crack tip zone can carry out high-resolution imaging, prepare simultaneously in the sample process and sample surfaces to be preserved complete, preparation process is simple to operate, and control accuracy is high, preparation transmission sample success ratio is high, can want viewing area by autotelic attenuate.
Crack tip preparation of transmission samples of the present invention, its step is as follows:
1) will in the two-beam focused ion beam system, carry out electron beam patterning, the crack tip that finds sample surfaces to observe with the sample of crackle;
2) at crack tip area deposition Pt, be used for protecting the crack tip that will observe;
3) with the sample stage rotation, make ion gun and sample be in plumbness, and carry out semiclosed etching at crack tip Pt sedimentary province periphery;
4) sample stage is placed horizontal level, adopt ion beam that crack tip Pt sedimentary province is carried out the V-type cutting along the etching place;
5) stretch into mechanical arm, the needle point at mechanical arm top is contacted with crack tip Pt sedimentary province, utilize the Pt deposition, needle point and V-type crack tip Pt sedimentary province are welded and fixed;
6) V-type crack tip Pt sedimentary province is not carried out the ion beam cutting in the etching place, V-type crack tip Pt sedimentary province is separated fully with sample, obtain crack tip V-type sample;
7) with copper mesh imaging under electron beam, put down mechanical arm, crack tip V-type sample is welded on the copper mesh of horizontal positioned, with ion beam needle point and crack tip V-type sample are cut off, regain mechanical arm;
The copper mesh that 8) will be welded with crack tip V-type sample vertically places specimen holder, and it is vertical ion gun and sample to be in the sample stage rotation again, and crack tip V-type sample is carried out the ion beam attenuate.
Further, in step 4), the cutting of described V-type comprises carries out the ion beam cutting along sedimentary province one side etching place, with sample stage centered by sedimentary province, Rotate 180 ° carries out the ion beam cutting along sedimentary province opposite side etching place, sample stage is gone back to original position again.
Further, in step 2) in, at the rectangle that is shaped as of crack tip area deposition Pt, deposit thickness is 0.8～1.2 μ m.
Further, in step 2) in, trapezoidal being shaped as of crack tip area deposition Pt, deposit thickness is 0.8～1.2 μ m.
Further, in step 3), the degree of depth of carrying out etching at crack tip Pt sedimentary province periphery is 8～10 μ m.
Further, sample stage anglec of rotation b equates that described sample stage anglec of rotation α is 45 °～55 ° in sample stage anglec of rotation α and the step 8) in step 3).
Further, described sample stage anglec of rotation α is 52 ° or 54 °.
Further, in step 8), it is as follows that its sample is carried out the ion beam thinning process:
A) sample stage is gone to 52.5 °～53 °, crack tip V-type sample upside is carried out attenuate, electric current is 2nA～4nA; Sample stage is gone to 55 °～55.5 ° again, downside is carried out attenuate with same current, making crack tip V-type thickness of sample is 300～500 nanometers;
B) sample stage is gone to sample stage and go to 55.5 ° or 56 °, electric current is 120pA～240pA, carries out attenuate at crack tip V-type sample downside, and making crack tip V-type thickness of sample is 150～300 nanometers;
C) downside of the most advanced and sophisticated V-type sample of the bending crack that obtains in step b) sample carried out the segmentation attenuate, electric current is 50pA, until crack tip V-type sample forms transparent.
Beneficial effect of the present invention is:
1, crack tip preparation of transmission samples of the present invention adopts focused ion beam FIB technology, accurately the ion beam attenuate is carried out in its crack tip zone that will observe, make the crack tip zone can carry out high-resolution imaging, preparing simultaneously in the sample process preserves complete to sample surfaces, preparation process is simple to operate, control accuracy is high, and preparation transmission sample success ratio is high, can want viewing area by autotelic attenuate;
2, crack tip preparation of transmission samples of the present invention adopts and adopt the V-type cutting technique when the preparation crack tip, this cutting technique is preserved complete to preparation sample surfaces surface, the crack tip V-type sample that forms after the cutting is carrying out ion beam attenuate formation film sample, control accuracy is high, preparation transmission sample success ratio is high, can want viewing area by autotelic attenuate.
Description of drawings
Fig. 1 is that the crack tip that will observe of sample surfaces is at electron beam patterning figure;
Fig. 2 is the enlarged drawing after etching is carried out in both sides, crack tip Pt protected location and left side;
Fig. 3 is crack tip enlarged drawing after deposition model pattern adopts V-type to cut;
Fig. 4 is the enlarged drawing of crack tip and mechanical arm welding;
Fig. 5 is welded on enlarged drawing on the copper mesh after crack tip and the sample separation;
Fig. 6 is the enlarged drawing of crack tip in the cutting of Mill for-depth pattern employing ion beam;
Fig. 7 is the enlarged drawing of crack tip in the ion beam thinning process;
Fig. 8 is the enlarged drawing of crack tip after the ion beam attenuate is finished.
Embodiment
In order to make the purpose, technical solutions and advantages of the present invention clearer, the below is described in detail the preferred embodiments of the present invention.
Embodiment one
Be illustrated in figure 1 as crack tip that sample surfaces will observe at electron beam patterning figure; Be illustrated in figure 2 as the enlarged drawing after etching is carried out in both sides, crack tip Pt protected location and left side; Be illustrated in figure 3 as crack tip enlarged drawing after deposition model pattern adopts V-type to cut; Be illustrated in figure 4 as the enlarged drawing of crack tip and mechanical arm welding; Be welded on enlarged drawing on the copper mesh after being illustrated in figure 5 as crack tip and sample separation; Be illustrated in figure 6 as the enlarged drawing of crack tip in Mill for-depth pattern employing ion beam; Be illustrated in figure 7 as the enlarged drawing after the crack tip attenuate is finished; Fig. 8 is the enlarged drawing of crack tip after the ion beam attenuate is finished.Crack tip preparation of transmission samples of the present invention, prepared transmission sample is chosen as the Ti alloy, and its step is as follows:
1) will in the two-beam focused ion beam system, carry out electron beam patterning, the crack tip that finds sample surfaces to observe with the sample of crackle; Preferred two-beam focused ion beam system is selected German ZEISS two-beam focused ion beam system;
2) at crack tip area deposition platinum Pt, play the protective effect to want observation area, at the rectangle that is shaped as of crack tip area deposition Pt, the specification of rectangle is 15 * 5 μ m, and deposit thickness is 1 μ m;
3) be 45 °～55 ° with sample stage anglec of rotation α, preferred sample stage anglec of rotation α is 52 °, and it is vertical that ion gun and sample are in, and carries out etching in two long sides and a short side of crack tip Pt sedimentary province respectively, and the etching transversal section degree of depth is 8 μ m;
4) sample stage is placed horizontal level, carrying out the ion beam cutting along place, sedimentary province length one side transversal section, this moment is for fear of depositing again, adopt deposition model pattern, with sample stage centered by sedimentary province, Rotate 180 °, repeat previous step at opposite side, form V-type; Again sample stage is gone back to original position, i.e.-180 ° or 180 ° of rotations;
5) stretch into mechanical arm, with needle point and crack tip Pt sedimentary province one end in contact, utilize the Pt deposition, needle point and the sample of cutting are welded and fixed;
6) its V-type sample right side is carried out the ion beam cutting, make it fully and sample separation, adopt deposition model pattern, avoid depositing again;
7) with copper mesh imaging under electron beam of putting well, put down mechanical arm, its most advanced and sophisticated V-type sample is welded on the copper mesh of horizontal positioned, with ion beam needle point and sample are cut off again, regain mechanical arm;
The copper mesh that 8) will be welded with crack tip V-type sample vertically places specimen holder, with 53 ° of sample stage rotations, under Mill for-depth pattern crack tip V-type sample is carried out the ion beam attenuate.
In step 8), it is as follows that its sample is carried out the ion beam thinning process:
A) sample stage is gone to 52.5 °～53 °, preferably sample stage is gone to 53 °, crack tip V-type sample upside is carried out attenuate, electric current is 2nA; Sample stage is gone to 55 ° again, downside is carried out attenuate with same current, making crack tip V-type thickness of sample is 200～300 nanometers;
B) sample stage is gone to 55.5 ° or 56 °, electric current is 120pA, carries out attenuate at crack tip V-type sample downside, making crack tip V-type thickness of sample is 150～300 nanometers, and when thickness during near 200nm, sample can flexural deformation, this moment, during imaging, the crackle appearance was very clear under electron beam;
C) downside of the most advanced and sophisticated V-type sample of the bending crack that obtains in the step b) carried out the segmentation attenuate, electric current is 50pA, until crack tip V-type sample forms transparent.
Embodiment two
Crack tip preparation of transmission samples of the present invention, prepared transmission sample is chosen as magnesium alloy, and its step is as follows:
1) will in the two-beam focused ion beam system, carry out electron beam patterning, the crack tip that finds sample surfaces to observe with the sample of crackle; Preferred two-beam focused ion beam system is selected German ZEISS two-beam focused ion beam system;
2) at crack tip area deposition Pt, play the protective effect to want observation area, being shaped as of crack tip area deposition Pt is trapezoidal, and deposit thickness is approximately 1 μ m;
3) be 45 °～55 ° with sample stage anglec of rotation α, preferred sample stage anglec of rotation α is 54 °, and it is vertical that ion gun and sample are in, and carries out etching along crack tip Pt sedimentary province trapezoidal two long sides and a short side, and the etching transversal section degree of depth is 10 μ m;
4) sample stage is placed horizontal level, sample stage is placed horizontal level, under deposition model pattern, adopt ion beam that crack tip Pt sedimentary province is carried out the V-type cutting along the etching place;
5) stretch into mechanical arm, with needle point and sample P t protected location one end in contact, utilize the Pt deposition, needle point and the sample of cutting are welded and fixed;
6) its V-type sample right side is carried out the ion beam cutting, make it fully and sample separation.Adopt deposition model pattern, avoid depositing again;
7) mechanical arm is put down in the copper mesh imaging under electron beam that will put well before, and its most advanced and sophisticated V-type sample is welded on the copper mesh of horizontal positioned.With ion beam needle point and sample are cut off again, regain mechanical arm;
The copper mesh that 8) will be welded with crack tip V-type sample vertically places specimen holder, with 53 ° of sample stage rotations, under Mill for-depth pattern crack tip V-type sample is carried out the ion beam attenuate again.
In step 8), it is as follows that its sample is carried out the ion beam thinning process:
A) sample stage is gone to 53 °, crack tip V-type sample upside is carried out attenuate, the electric current range of choice is 2nA～4nA, and preferred electric current is 2nA; Sample stage is gone to 55 ° again, downside is carried out attenuate with same current, making crack tip V-type thickness of sample is about 200～300 nanometers;
B) sample stage is gone to 55.5 ° or 56 °, electric current is 120pA, carries out attenuate at crack tip V-type sample downside, making crack tip V-type thickness of sample is 150～300 nanometers, and when thickness during near 200nm, sample can flexural deformation, this moment, during imaging, the crackle appearance was very clear under electron beam;
C) downside of the most advanced and sophisticated V-type sample of the bending crack that obtains in the step b) carried out the segmentation attenuate, electric current is 50pA, until crack tip V-type sample forms transparent.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although by invention has been described with reference to the preferred embodiments of the present invention, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (8)
1. crack tip preparation of transmission samples, it is characterized in that: its step is as follows:
1) will in the two-beam focused ion beam system, carry out electron beam patterning, the crack tip that finds sample surfaces to observe with the sample of crackle;
2) at crack tip area deposition Pt, be used for protecting the crack tip that will observe;
3) with the sample stage rotation, make ion gun and sample be in plumbness, and carry out semiclosed etching at crack tip Pt sedimentary province periphery;
4) sample stage is placed horizontal level, adopt ion beam that crack tip Pt sedimentary province is carried out the V-type cutting along the etching place;
5) stretch into mechanical arm, the needle point at mechanical arm top is contacted with crack tip Pt sedimentary province, utilize the Pt deposition, needle point and V-type crack tip Pt sedimentary province are welded and fixed;
6) V-type crack tip Pt sedimentary province is not carried out the ion beam cutting in the etching place, V-type crack tip Pt sedimentary province is separated fully with sample, obtain crack tip V-type sample;
7) with copper mesh imaging under electron beam, put down mechanical arm, crack tip V-type sample is welded on the copper mesh of horizontal positioned, with ion beam needle point and crack tip V-type sample are cut off, regain mechanical arm;
The copper mesh that 8) will be welded with crack tip V-type sample vertically places specimen holder, and it is vertical ion gun and sample to be in the sample stage rotation again, and crack tip V-type sample is carried out the ion beam attenuate.
2. crack tip preparation of transmission samples as claimed in claim 1, it is characterized in that: in step 4), the cutting of described V-type comprises carries out the ion beam cutting along sedimentary province one side etching place, with sample stage centered by sedimentary province, Rotate 180 °, carry out the ion beam cutting along sedimentary province opposite side etching place, again sample stage is gone back to original position.
3. crack tip preparation of transmission samples as claimed in claim 2 is characterized in that: in step 2) in, at the rectangle that is shaped as of crack tip area deposition Pt, deposit thickness is 0.8～1.2 μ m.
4. crack tip preparation of transmission samples as claimed in claim 2 is characterized in that: in step 2) in, trapezoidal being shaped as of crack tip area deposition Pt, deposit thickness is 0.8～1.2 μ m.
5. such as claim 3 or 4 described crack tip preparation of transmission samples, it is characterized in that: in step 3), the degree of depth of carrying out etching at crack tip Pt sedimentary province periphery is 8～10 μ m.
6. crack tip preparation of transmission samples as claimed in claim 5 is characterized in that: sample stage anglec of rotation b equates that described sample stage anglec of rotation α is 45 °～55 ° in sample stage anglec of rotation α and the step 8) in step 3).
7. crack tip preparation of transmission samples as claimed in claim 6, it is characterized in that: described sample stage anglec of rotation α is 52 ° or 54 °.
8. crack tip preparation of transmission samples as claimed in claim 7 is characterized in that: in step 8), it is as follows that its sample is carried out the ion beam thinning process:
A) sample stage is gone to 52.5 °～53 °, crack tip V-type sample upside is carried out attenuate, electric current is 2nA～4nA; Sample stage is gone to 55 °～55.5 ° again, downside is carried out attenuate with same current, making crack tip V-type thickness of sample is 300～500 nanometers;
B) sample stage is gone to sample stage and go to 55.5 ° or 56 °, electric current is 120pA～240pA, carries out attenuate at crack tip V-type sample downside, and making crack tip V-type thickness of sample is 150～300 nanometers;
C) downside of the most advanced and sophisticated V-type sample of the bending crack that obtains in the step b) carried out the segmentation attenuate, electric current is 50pA, until crack tip V-type sample forms transparent.
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| CN201210389124.4A CN102854048B (en) | 2012-10-15 | 2012-10-15 | Preparation method of transmitting sample with crack tip |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792583A (en) * | 2014-01-17 | 2015-07-22 | 中芯国际集成电路制造(上海)有限公司 | Preparation method of TEM sample |
| CN105842045A (en) * | 2016-03-22 | 2016-08-10 | 西安交通大学 | Method for preparation of large-size transmission sample with focused ion beam |
| CN105865862A (en) * | 2016-03-25 | 2016-08-17 | 江苏省沙钢钢铁研究院有限公司 | Making method of three-dimensional atom probe sample |
| CN107643309A (en) * | 2017-08-31 | 2018-01-30 | 武汉钢铁有限公司 | The analysis method of electrical steel surface coating |
| CN112881439A (en) * | 2021-03-09 | 2021-06-01 | 洪启集成电路(珠海)有限公司 | OLED TEM sample preparation method and OLED TEM sample |
| CN114486324A (en) * | 2022-01-30 | 2022-05-13 | 上海季丰电子股份有限公司 | Preparation method of transmission electron microscope sample |
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| EP1209737A2 (en) * | 2000-11-06 | 2002-05-29 | Hitachi, Ltd. | Method and apparatus for specimen fabrication |
| JP2008298797A (en) * | 2008-09-01 | 2008-12-11 | Hitachi Ltd | Sample preparing device |
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2012
- 2012-10-15 CN CN201210389124.4A patent/CN102854048B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1209737A2 (en) * | 2000-11-06 | 2002-05-29 | Hitachi, Ltd. | Method and apparatus for specimen fabrication |
| JP2008298797A (en) * | 2008-09-01 | 2008-12-11 | Hitachi Ltd | Sample preparing device |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104792583A (en) * | 2014-01-17 | 2015-07-22 | 中芯国际集成电路制造(上海)有限公司 | Preparation method of TEM sample |
| CN104792583B (en) * | 2014-01-17 | 2018-06-26 | 中芯国际集成电路制造(上海)有限公司 | A kind of preparation method of TEM sample |
| CN105842045A (en) * | 2016-03-22 | 2016-08-10 | 西安交通大学 | Method for preparation of large-size transmission sample with focused ion beam |
| CN105842045B (en) * | 2016-03-22 | 2018-12-07 | 西安交通大学 | A kind of processing method using focused ion beam preparation large scale transmission sample |
| CN105865862A (en) * | 2016-03-25 | 2016-08-17 | 江苏省沙钢钢铁研究院有限公司 | Making method of three-dimensional atom probe sample |
| CN105865862B (en) * | 2016-03-25 | 2018-12-14 | 江苏省沙钢钢铁研究院有限公司 | A kind of preparation method of three-dimensional atom probe sample |
| CN107643309A (en) * | 2017-08-31 | 2018-01-30 | 武汉钢铁有限公司 | The analysis method of electrical steel surface coating |
| CN112881439A (en) * | 2021-03-09 | 2021-06-01 | 洪启集成电路(珠海)有限公司 | OLED TEM sample preparation method and OLED TEM sample |
| CN114486324A (en) * | 2022-01-30 | 2022-05-13 | 上海季丰电子股份有限公司 | Preparation method of transmission electron microscope sample |
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