CN102854048B - Preparation method of transmitting sample with crack tip - Google Patents
Preparation method of transmitting sample with crack tip Download PDFInfo
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- CN102854048B CN102854048B CN201210389124.4A CN201210389124A CN102854048B CN 102854048 B CN102854048 B CN 102854048B CN 201210389124 A CN201210389124 A CN 201210389124A CN 102854048 B CN102854048 B CN 102854048B
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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 material analysis techniques field, especially a kind of crack tip preparation of transmission samples.
Background technology
In conventional material analysis process, film sample preparation adopts ion milling and twin-jet electropolishing polishing two kinds of technological means; wherein ion milling needs to use Ion Beam Thinner; ion current is bombarded sample surfaces continuously with a certain incident angle; sample surfaces atom is continuously sputtered; finally obtain required film sample, this technology is more serious to sample surfaces damage; It is less that another shortcoming is exactly thin district, twin-jet electropolishing polishing needs to use two spray instrument, by electrolytic solution by two side nozzles, obtain a spray speed moderate, two post liquid are symmetrical and in the state of straight line, insert specimen holder and carry out polishing, thus reach the effect of thinning sample, this technology is in the more difficult grasp of thinning 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, it is thinning that ion beam is carried out in the crack tip region that this preparation method can will observe it accurately, easily, crack tip region is made to carry out high-resolution imaging, prepare in sample preserves complete to sample surfaces simultaneously, and preparation process is simple to operate, and control accuracy is high, prepare transmission sample success ratio high, can autotelic thinning wanted viewing area.
Crack tip preparation of transmission samples of the present invention, its step is as follows:
1) sample with crackle is carried out electron beam patterning in two-beam focused ion beam system, find the crack tip that sample surfaces will be observed;
2) at crack tip area deposition Pt, for protecting the carrying out of the crack tip that will observe;
3) sample stage is rotated, 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 in horizontal level, adopts ion beam to carry out V-type cutting to crack tip Pt sedimentary province along etching place;
5) stretch into mechanical arm, the needle point at mechanical arm top is contacted with crack tip Pt sedimentary province, utilizes Pt to deposit, needle point and V-type crack tip Pt sedimentary province are welded and fixed;
6) the V-type crack tip Pt sedimentary province place of etching is carried out ion beam cutting, V-type crack tip Pt sedimentary province is separated completely with sample, obtains crack tip V-type sample;
7) by 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;
8) copper mesh being welded with crack tip V-type sample is vertically placed in specimen holder, then sample stage is rotated that ion gun and sample are in is vertical, ion beam carries out to crack tip V-type sample thinning.
Further, in step 4), described V-type cutting comprises carries out ion beam cutting along etching place, side, sedimentary province, by sample stage centered by sedimentary province, rotate 180 °, along sedimentary province, opposite side etching place carries out ion beam cutting, then sample stage is gone back to original position.
Further, in step 2) in, be rectangle in the shape of crack tip area deposition Pt, deposit thickness is 0.8 ~ 1.2 μm.
Further, in step 2) in, be trapezoidal in the shape of crack tip area deposition Pt, deposit thickness is 0.8 ~ 1.2 μm.
Further, in step 3), the degree of depth carrying out etching at crack tip Pt sedimentary province periphery is 8 ~ 10 μm.
Further, in step 3), in sample stage anglec of rotation α and step 8), sample stage anglec of rotation b is equal, and described sample stage anglec of rotation α is 45 ° ~ 55 °.
Further, described sample stage anglec of rotation α is 52 ° or 54 °.
Further, in step 8), ion beam thinning process carries out to its sample as follows:
A) sample stage is gone to 52.5 ° ~ 53 °, thinning to carrying out on the upside of crack tip V-type sample, electric current is 2nA ~ 4nA; Sample stage is gone to 55 ° ~ 55.5 ° again, carry out thinning to downside with same current, make crack tip V-type thickness of sample be 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 thinning on the downside of crack tip V-type sample, makes crack tip V-type thickness of sample be 150 ~ 300 nanometers;
C) carry out segmentation to the downside of the most advanced and sophisticated V-type samples of the bending crack obtained in step b) thinning, electric current is 50pA, until crack tip V-type sample is formed 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, it is thinning that ion beam is carried out in the crack tip region will observed it accurately, crack tip region is made to carry out high-resolution imaging, prepare in sample preserves complete to sample surfaces simultaneously, preparation process is simple to operate, control accuracy is high, prepares transmission sample success ratio high, can autotelic thinning wanted viewing area;
2, crack tip preparation of transmission samples of the present invention adopts and adopts V-type cutting technique when preparing crack tip, this cutting technique is preserved complete to preparing sample surfaces surface, the crack tip V-type sample formed after cutting is carrying out the thinning formation film sample of ion beam, control accuracy is high, prepare transmission sample success ratio high, can autotelic thinning wanted viewing area.
Accompanying drawing explanation
The crack tip that Fig. 1 will observe for sample surfaces is at electron beam patterning figure;
Fig. 2 is the enlarged drawing after both sides, crack tip Pt protected location and left side etch;
Fig. 3 is crack tip enlarged drawing after deposition model pattern adopts V-type to cut;
Fig. 4 is the enlarged drawing that crack tip welds with mechanical arm;
Fig. 5 is welded on enlarged drawing on copper mesh after crack tip and sample separation;
Fig. 6 is that crack tip adopts the enlarged drawing in ion beam cutting in Mill for-depth pattern;
Fig. 7 is the enlarged drawing of crack tip in ion beam thinning process;
Fig. 8 be crack tip ion beam is thinning complete after enlarged drawing.
Embodiment
In order to make the object, technical solutions and advantages of the present invention clearly, below the preferred embodiments of the present invention are described in detail.
Embodiment one
Be illustrated in figure 1 crack tip that sample surfaces will observe at electron beam patterning figure; Be illustrated in figure 2 both sides, crack tip Pt protected location and left side etch after enlarged drawing; Be illustrated in figure 3 crack tip enlarged drawing after deposition model pattern adopts V-type to cut; Be illustrated in figure 4 the enlarged drawing that crack tip welds with mechanical arm; Enlarged drawing on copper mesh is welded on after being illustrated in figure 5 crack tip and sample separation; Be illustrated in figure 6 the enlarged drawing of crack tip in Mill for-depth pattern employing ion beam; Enlarged drawing after being illustrated in figure 7 that crack tip is thinning and completing; Fig. 8 be crack tip ion beam is thinning complete after enlarged drawing.Crack tip preparation of transmission samples of the present invention, prepared transmission sample is chosen as Ti alloy, and its step is as follows:
1) sample with crackle is carried out electron beam patterning in two-beam focused ion beam system, find the crack tip that sample surfaces will be observed; Preferred two-beam focused ion beam system selects German ZEISS two-beam focused ion beam system;
2) at crack tip area deposition platinum Pt, playing the protective effect to wanted observation area, is rectangle in the shape of crack tip area deposition Pt, and the specification of rectangle is 15 × 5 μm, and deposit thickness is 1 μm;
3) by sample stage anglec of rotation α be 45 ° ~ 55 °, preferred sample stage anglec of rotation α is 52 °, ion gun and sample is in vertical, etches respectively in two long sides of crack tip Pt sedimentary province and a short side, and the etching transversal section degree of depth is 8 μm;
4) sample stage being placed in horizontal level, carrying out ion beam cutting, now in order to avoid depositing again along transversal section place, length side, sedimentary province, adopt deposition model pattern, by 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, namely rotate-180 ° or 180 °;
5) stretch into mechanical arm, by needle point and crack tip Pt sedimentary province end thereof contacts, utilize Pt to deposit, needle point and sample of cutting are welded and fixed;
6) carry out ion beam cutting by the right side of its V-type sample, make its complete and sample separation, adopt deposition model pattern, avoid depositing again;
7) copper mesh imaging under electron beam of will put well, puts down mechanical arm, is welded on the copper mesh of horizontal positioned by its most advanced and sophisticated V-type sample, then needle point and sample is cut off with ion beam, regains mechanical arm;
8) copper mesh being welded with crack tip V-type sample is vertically placed in specimen holder, sample stage is rotated 53 °, under Mill for-depth pattern, ion beam carries out to crack tip V-type sample thinning.
In step 8), ion beam thinning process carries out to its sample as follows:
A) sample stage is gone to 52.5 ° ~ 53 °, preferably sample stage is gone to 53 °, thinning to carrying out on the upside of crack tip V-type sample, electric current is 2nA; Again sample stage is gone to 55 °, carry out thinning to downside with same current, make crack tip V-type thickness of sample be 200 ~ 300 nanometers;
B) sample stage is gone to 55.5 ° or 56 °, electric current is 120pA, carries out thinning on the downside of crack tip V-type sample, crack tip V-type thickness of sample is made to be 150 ~ 300 nanometers, when thickness is close to 200nm, sample meeting flexural deformation, now under electron beam during imaging, crackle appearance is very clear;
C) carry out segmentation to the downside of the most advanced and sophisticated V-type sample of the bending crack obtained in step b) thinning, electric current is 50pA, until crack tip V-type sample is formed 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) sample with crackle is carried out electron beam patterning in two-beam focused ion beam system, find the crack tip that sample surfaces will be observed; Preferred two-beam focused ion beam system selects German ZEISS two-beam focused ion beam system;
2) at crack tip area deposition Pt, play the protective effect to wanted observation area, the shape of crack tip area deposition Pt is trapezoidal, and deposit thickness is approximately 1 μm;
3) by sample stage anglec of rotation α be 45 ° ~ 55 °, preferred sample stage anglec of rotation α is 54 °, ion gun and sample is in vertical, and along crack tip Pt sedimentary province, trapezoidal two long sides and a short side etch, and the etching transversal section degree of depth is 10 μm;
4) sample stage is placed in horizontal level, sample stage is placed in horizontal level, under deposition model pattern, adopt ion beam to carry out V-type cutting to crack tip Pt sedimentary province along etching place;
5) stretch into mechanical arm, by needle point and sample P t protected location end thereof contacts, utilize Pt to deposit, needle point and sample of cutting are welded and fixed;
6) carry out ion beam cutting by the right side of its V-type sample, make its complete and sample separation.Adopt deposition model pattern, avoid depositing again;
7) copper mesh imaging under electron beam of will put well before, puts down mechanical arm, is welded on the copper mesh of horizontal positioned by its most advanced and sophisticated V-type sample.With ion beam, needle point and sample are cut off again, regain mechanical arm;
8) copper mesh being welded with crack tip V-type sample is vertically placed in specimen holder, then sample stage is rotated 53 °, under Mill for-depth pattern, ion beam carries out to crack tip V-type sample thinning.
In step 8), ion beam thinning process carries out to its sample as follows:
A) sample stage is gone to 53 °, thinning to carrying out on the upside of crack tip V-type sample, electric current range of choice is 2nA ~ 4nA, and preferred electric current is 2nA; Again sample stage is gone to 55 °, carry out thinning to downside with same current, make crack tip V-type thickness of sample be 200 ~ 300 ran;
B) sample stage is gone to 55.5 ° or 56 °, electric current is 120pA, carries out thinning on the downside of crack tip V-type sample, crack tip V-type thickness of sample is made to be 150 ~ 300 nanometers, when thickness is close to 200nm, sample meeting flexural deformation, now under electron beam during imaging, crackle appearance is very clear;
C) carry out segmentation to the downside of the most advanced and sophisticated V-type sample of the bending crack obtained in step b) thinning, electric current is 50pA, until crack tip V-type sample is formed transparent.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by referring to the preferred embodiments of the present invention, invention has been described, but those of ordinary skill in the art is to be understood that, various change can be made to it in the form and details, and not depart from the spirit and scope of the present invention that appended claims limits.
Claims (7)
1. a crack tip preparation of transmission samples, is characterized in that: its step is as follows:
1) sample with crackle is carried out electron beam patterning in two-beam focused ion beam system, find the crack tip that sample surfaces will be observed;
2) at crack tip area deposition Pt, for protecting the carrying out of the crack tip that will observe;
3) sample stage is rotated, 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 in horizontal level, adopts ion beam to carry out V-type cutting to crack tip Pt sedimentary province along etching place;
5) stretch into mechanical arm, the needle point at mechanical arm top is contacted with crack tip Pt sedimentary province, utilizes Pt to deposit, needle point and V-type crack tip Pt sedimentary province are welded and fixed;
6) the V-type crack tip Pt sedimentary province place of etching is carried out ion beam cutting, V-type crack tip Pt sedimentary province is separated completely with sample, obtains crack tip V-type sample;
7) by 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;
8) copper mesh being welded with crack tip V-type sample is vertically placed in specimen holder, then sample stage is rotated that ion gun and sample are in is vertical, ion beam carries out to crack tip V-type sample thinning;
In step 8), ion beam thinning process carries out to its sample as follows:
A) sample stage is gone to 52.5 ° ~ 53 °, thinning to carrying out on the upside of crack tip V-type sample, electric current is 2nA ~ 4nA; Sample stage is gone to 55 ° ~ 55.5 ° again, carry out thinning to downside with same current, make crack tip V-type thickness of sample be 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 thinning on the downside of crack tip V-type sample, makes crack tip V-type thickness of sample be 150 ~ 300 nanometers;
C) carry out segmentation to the downside of the most advanced and sophisticated V-type sample of the bending crack obtained in step b) thinning, electric current is 50pA, until crack tip V-type sample is formed transparent.
2. crack tip preparation of transmission samples as claimed in claim 1, it is characterized in that: in step 4), described V-type cutting comprises carries out ion beam cutting along etching place, side, sedimentary province, by sample stage centered by sedimentary province, rotate 180 °, along sedimentary province, opposite side etching place carries out ion beam cutting, then 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, be rectangle in the shape of crack tip area deposition Pt, deposit thickness is 0.8 ~ 1.2 μm.
4. crack tip preparation of transmission samples as claimed in claim 2, is characterized in that: in step 2) in, be trapezoidal in the shape of crack tip area deposition Pt, deposit thickness is 0.8 ~ 1.2 μm.
5. the crack tip preparation of transmission samples as described in claim 3 or 4, is characterized in that: in step 3), and the degree of depth carrying out etching at crack tip Pt sedimentary province periphery is 8 ~ 10 μm.
6. crack tip preparation of transmission samples as claimed in claim 5, is characterized in that: in step 3), in sample stage anglec of rotation α and step 8), sample stage anglec of rotation b is equal, and described sample stage anglec of rotation α is 45 ° ~ 55 °.
7. crack tip preparation of transmission samples as claimed in claim 6, is characterized in that: described sample stage anglec of rotation α is 52 ° or 54 °.
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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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| 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 |
| 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 |
| 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 |
| CN107643309B (en) * | 2017-08-31 | 2020-04-07 | 武汉钢铁有限公司 | 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 |
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 |
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| 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 |
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