CN103698178A - Preparation method for thin-film sample for high-resolution transmission electron microscope - Google Patents
Preparation method for thin-film sample for high-resolution transmission electron microscope Download PDFInfo
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Abstract
The invention discloses a preparation method for processing a thin-film sample for a high-resolution transmission electron microscope by adopting an ion polishing system. The preparation method is characterized in that the thin-film sample for the high-resolution transmission electron microscope is prepared by arranging an observed position on a special sample at the middle part of an oppositely-bonded test sample by means of opposite bonding, and cooperating with a reasonable ion polishing process, thus realizing high-resolution transmission electron microscope observation on a special sample organization structure. The preparation method for the thin-film sample for the high-resolution transmission electron microscope for the special sample has following advantages: preparation for the thin-film sample for the high-resolution transmission electron microscope for the special sample (for example, a sample with a surface deterioration layer or a sample with a crack tip) is realized, and the preparation method is fast in sample preparation, expense-saving, high in success rate, and simple and practicable.
Description
Technical field
The invention belongs to the technology of preparing of electron microscope film sample, relate to the preparation method of film sample for a kind of high-resolution-ration transmission electric-lens.
Background technology
At present the understanding of Fine Texture of Material and structure is mainly realized by transmission electron microscopy.Transmission electron microscopy sample preparation is more complicated and have certain limitation.Conventional method for making sample is to cut with line the thin slice that 0.1-0.3mm is thick, then with sand paper, is milled to thickness and is less than 50 μ m, goes out 3mm diameter sequin afterwards, then by the method for electropolishing or ion milling, sample is thinned to perforation with rushing sample device.The method cannot realize the Micro-Structure Analysis of sample ad-hoc location.
Summary of the invention
The object of the invention is to propose the preparation method that a kind of high-resolution-ration transmission electric-lens that can realize the Micro-Structure Analysis of sample ad-hoc location is used film sample.Technical solution of the present invention is: 1) comprising on the part of observed position, cut block sample, and observed position is placed on cut block sample, block sample is of a size of: long: 0.5～2.2mm, wide: 0.5～1mm: thick: 0.2～0.5mm, 2) by block sample by grow with on the thick surface forming to a sticky batching corresponding with block sample same material and size; 3) two surface finish at thickness direction by block sample, are finally milled to 20～30 μ m with 1000# sand paper, form block sample and composition to sticky thin slice; 4) will be bonded at single hole annular to sticky thin slice carries online; 5) by being stained with, the single hole annular of sticky thin slice is carried to a net being placed on and on Ion Beam Thinner, being thinned to perforation.Ion milling technological parameter is: 1) ion beam voltage 5kV, and ion beam is with respect to being 10 ° to the pitch angle of sticky thin slice, the attenuate time is 30～100min; 2) ion beam voltage 4kV, ion beam is with respect to being 8 ° to the pitch angle of sticky thin slice, the attenuate time is 15～40min; 3) ion beam voltage 3kV, ion beam is with respect to being 5 ° to the pitch angle of sticky thin slice, the attenuate time is 8～30min; 4) ion beam voltage 2kV, ion beam is with respect to being 3 ° to the pitch angle of sticky thin slice, attenuate time 5～20min; 5) ion beam voltage 1kV, ion beam, with respect to being 2 ° to the pitch angle of sticky thin slice, being thinned to perforation and making film sample.
Described is comprising the block sample that cuts two same sizes on the part of observed position, to sticking into sticky thin slice.
Described Ion Beam Thinner be thinned to perforation, the order that is divided into (5kV, 10 °), (4kV, 8 °), (3kV, 5 °), (2kV, 3 °), (1kV, 2 °) is thinned to perforation successively, the time of each attenuate is determined according to the composition of material.
The diameter of bore that described single hole annular is carried net is preferably 1～2mm.
The advantage that the present invention has and beneficial effect: 1), by sticky mode, observation place is placed in to the center of block sample, realizes the high-resolution-ration transmission electric-lens of particular sample micromechanism is observed; 2), by the Proper Match at ion beam voltage and angle of inclination, guaranteeing, under the prerequisite of attenuate quality, to have shortened the sample preparation cycle; 3) successively decreasing successively of ion beam energy and angle, can effectively suppress the damage of ion beam to sample.4) sample preparation low-yield, low-angle attenuate parameter of last stage, can reduce the surface contamination of film sample, guarantees the surface quality of film sample.5) particular sample high-resolution-ration transmission electric-lens provided by the invention is with in the preparation method of film sample, and ion milling is total consuming time in 4h, ion milling time shorten over half.
Accompanying drawing explanation
The high resolution picture of the GH4169 high temperature alloy grinding skin metamorphic layer that Fig. 1 the present invention successfully observes.
The high resolution picture picture of the M50NiL steel grinding skin metamorphic layer that Fig. 2 the present invention successfully observes.
The M50NiL steel contact fatigue that Fig. 3 the present invention successfully observes is cheated the high resolution picture of the most advanced and sophisticated tissue of sub-surface crack.
Embodiment
The preparation method who the invention provides a kind of high-resolution-ration transmission electric-lens film sample of particular sample, preparation process is as follows:
Cut block sample comprising on the sample of observed position, block sample is of a size of: long: 0.5～2.2mm, and wide: 0.5～1mm: thick: 0.2～0.5mm; Observed position is placed in simultaneously block sample by grow and the thick surperficial center forming near;
Cut the batching that a size is identical with observed block sample with material;
By the observed surface of block sample with batching to sticky, form sticky sample;
Two surface uniform polishings by sticky sample thickness direction, are finally milled to 20～30 μ m with 1000# sand paper, form sticky thin slice;
To be bonded at single hole annular to sticky thin slice carries online;
By being stained with, a single hole annular year net for sticky thin slice is placed on Ion Beam Thinner and is thinned to perforation, make film sample.
Ion milling technological parameter is as follows:
Ion beam voltage 5kV, 10 °, ion beam and sample inclination angle, attenuate time 30～100min;
Ion beam voltage 4kV, 8 °, ion beam and sample inclination angle, attenuate time 15～40min;
Ion beam voltage 3kV, 5 °, ion beam and sample inclination angle, attenuate time 8～30min;
A, ion beam voltage 2kV, 3 °, ion beam and sample inclination angle, attenuate time 5～20min;
B, ion beam voltage 1kV, 2 °, ion beam and sample inclination angle, be thinned to perforation.
The present invention's Ion Beam Thinner used, is preferably Gatan691 at present.
The ion milling time is relevant with material.For alloy in lightweight, the attenuate time takes the circumstances into consideration to reduce.
The external diameter that the present invention's single hole annular used is carried net is 3mm, and diameter of bore is 1～2mm preferably.
High-resolution-ration transmission electric-lens provided by the invention is with in the preparation method of film sample, and before ion milling, sample can pass through pit instrument attenuate sample central part area thickness, further to shorten the ion milling time.
Embodiment 1
The high resolution electron microscopy film sample of preparing high temperature alloy GH4169 sheet material grinding skin metamorphic layer.Sample making course is as follows: 1) on GH4169 sheet material, cut two block samples, block sample is of a size of: long: 2.2mm, wide: 1mm: thick: 0.3mm, and by grinding skin be placed in block sample by grow with the thick surface forming on; 2) by two block samples to sticky, two grinding skins that sticky face are to GH4169 sheet material wherein; 3) by two surface uniform polishings to sticky sample thickness direction, finally with 1000# sand paper, be milled to 22.7 μ m, form sticky thin slice; 4) will sticky thin slice be bonded to annular the carrying on the net of single hole that diameter of bore is 1mm; 5) by being stained with, the single hole annular of sticky thin slice is carried to a net being placed on and on Ion Beam Thinner, being thinned to perforation.
Ion milling technological parameter is: 1) ion beam voltage 5kV, and ion beam is with respect to being 10 ° to the pitch angle of sticky thin slice, the attenuate time is 90min; 2) ion beam voltage 4kV, ion beam is with respect to being 8 ° to the pitch angle of sticky thin slice, the attenuate time is 25min; 3) ion beam voltage 3kV, ion beam is with respect to being 5 ° to the pitch angle of sticky thin slice, the attenuate time is 15min; 4) ion beam voltage 2kV, ion beam is with respect to being 3 ° to the pitch angle of sticky thin slice, attenuate time 8min; 5) ion beam is with respect to being 2 ° to the pitch angle of sticky thin slice, and film sample is made in attenuate time 5min perforation.
With JEOL JEM-2010 type high-resolution-ration transmission electric-lens, observe GH4169 grinding skin film sample, its high resolution picture as shown in Figure 1.
Embodiment 2
The high resolution electron microscopy film sample of preparing ultra-high strength steel M50NiL sheet material grinding skin metamorphic layer.Sample making course is as follows: 1) on ultra-high strength steel M50NiL sheet material, cut two block samples, block sample is of a size of: long: 2.2mm, wide: 1mm: thick: 0.3mm, and by grinding skin be placed in block sample by grow with the thick surface forming on; 2) by two block samples to sticky, two grinding skins that sticky face are to M50NiL sheet material wherein; 3) by two surface uniform polishings to sticky sample thickness direction, finally with 1000# sand paper, be milled to 21.2 μ m, form sticky thin slice; 4) will sticky thin slice be bonded to annular the carrying on the net of single hole that diameter of bore is 1mm; 5) by being stained with, the single hole annular of sticky thin slice is carried to a net being placed on and on Ion Beam Thinner, being thinned to perforation.
Ion milling technological parameter is: 1) ion beam voltage 5kV, and ion beam is with respect to being 10 ° to the pitch angle of sticky thin slice, the attenuate time is 100min; 2) ion beam voltage 4kV, ion beam is with respect to being 8 ° to the pitch angle of sticky thin slice, the attenuate time is 30min; 3) ion beam voltage 3kV, ion beam is with respect to being 5 ° to the pitch angle of sticky thin slice, the attenuate time is 18min; 4) ion beam voltage 2kV, ion beam is with respect to being 3 ° to the pitch angle of sticky thin slice, attenuate time 12min; 5) ion beam is with respect to being 2 ° to the pitch angle of sticky thin slice, and film sample is made in attenuate time 7min perforation.
With JEOL JEM-2010 type high-resolution-ration transmission electric-lens, observe M50NiL grinding skin film sample, its high resolution picture fruit as shown in Figure 2.
Embodiment 3
Prepare ultra-high strength steel M50NiL contact fatigue and cheat the high resolution electron microscopy film sample of sub-surface crack tip end surface metamorphic layer.Sample making course is as follows: 1), near ultra-high strength steel M50NiL contact fatigue hole, cut a block sample, block sample is of a size of: long: 2.2mm, wide: 1mm: thick: 0.4mm, and by observation place be placed in block sample by grow with the thick surface forming on; 2) block sample by grow with on the thick surface forming to a sticky batching corresponding with block sample same material and size, form gluing sample; 3) by two surface uniform polishings to sticky sample thickness direction, finally with 1000# sand paper, be milled to 24.5 μ m, form sticky thin slice; 4) will sticky thin slice be bonded to annular the carrying on the net of single hole that diameter of bore is 1mm; 5) by being stained with, the single hole annular of sticky thin slice is carried to a net being placed on and on Ion Beam Thinner, being thinned to perforation.
Ion milling technological parameter is: 1) ion beam voltage 5kV, and ion beam is with respect to being 10 ° to the pitch angle of sticky thin slice, the attenuate time is 100min; 2) ion beam voltage 4kV, ion beam is with respect to being 8 ° to the pitch angle of sticky thin slice, the attenuate time is 40min; 3) ion beam voltage 3kV, ion beam is with respect to being 5 ° to the pitch angle of sticky thin slice, the attenuate time is 30min; 4) ion beam voltage 2kV, ion beam is with respect to being 3 ° to the pitch angle of sticky thin slice, attenuate time 15min; 5) ion beam voltage 1kV, ion beam is with respect to being 2 ° to the pitch angle of sticky thin slice, film sample is made in attenuate time 2min perforation.
With JEOL JEM-2010 type high-resolution-ration transmission electric-lens, observe M50NiL grinding skin film sample, crack tip high resolution picture as shown in Figure 3.
Claims (4)
1. the preparation method of film sample for a high-resolution-ration transmission electric-lens, it is characterized in that: 1) on the sample of observed position, cut block sample comprising, block sample is of a size of: long: 0.5～2.2mm, wide: 0.5～1mm: thick: 0.2～0.5mm, observed position is placed in simultaneously block sample by grow and the thick surperficial center forming near; 2) block sample by grow with on the thick surface forming to a sticky batching corresponding with block sample same material and size, form gluing sample; 3) by two surface uniform polishings to sticky sample thickness direction, finally with 1000# sand paper, be milled to 20～30 μ m, form sticky thin slice; 4) will be bonded at single hole annular to sticky thin slice carries online; 5) by being stained with, a single hole annular year net for sticky thin slice is placed on Ion Beam Thinner and is thinned to perforation, ion milling technological parameter is: 1) ion beam voltage 5kV, and ion beam is with respect to being 10 ° to the pitch angle of sticky thin slice, the attenuate time is 30～100min; 2) ion beam voltage 4kV, ion beam is with respect to being 8 ° to the pitch angle of sticky thin slice, the attenuate time is 15～40min; 3) ion beam voltage 3kV, ion beam is with respect to being 5 ° to the pitch angle of sticky thin slice, the attenuate time is 8～30min; 4) ion beam voltage 2kV, ion beam is with respect to being 3 ° to the pitch angle of sticky thin slice, attenuate time 5～20min; 5) ion beam voltage 1kV, ion beam, with respect to being 2 ° to the pitch angle of sticky thin slice, being thinned to perforation and making film sample.
2. the preparation method of film sample for a kind of high-resolution-ration transmission electric-lens according to claim 1, is characterized in that, described is comprising the block sample that cuts two same sizes on the sample of observed position, to sticking into sticky sample.
3. the preparation method of film sample for a kind of high-resolution-ration transmission electric-lens according to claim 1, it is characterized in that, described Ion Beam Thinner be thinned to perforation, be divided into 5kV, 10 °, 4kV, 8 °, 3kV, 5 °, 2kV, 3 °, 1kV, the order of 2 ° is thinned to perforation successively, and the time of each attenuate is determined according to material composition.
4. the preparation method of film sample for a kind of high-resolution-ration transmission electric-lens according to claim 1, is characterized in that, the diameter of bore that described single hole annular is carried net is preferably 1～2mm.
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| CN105628468A (en) * | 2015-12-28 | 2016-06-01 | 西安电子科技大学 | Method for preparing GaN-based heterojunction transparent film transmission electron microscope sectional sample |
| CN106645243A (en) * | 2016-12-23 | 2017-05-10 | 北京有色金属研究总院 | Preparation method of large-particle powder transmission electron microscope sample |
| CN107014652A (en) * | 2017-04-14 | 2017-08-04 | 广西大学 | A kind of annular contained network for transmission electron microscope is with cross-sectional sample to viscous device |
| CN107478668A (en) * | 2017-08-15 | 2017-12-15 | 合肥工业大学 | A kind of preparation method of heterogeneous alloy EBSD analyses test sample |
| CN108169265A (en) * | 2017-12-20 | 2018-06-15 | 东南大学 | A kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film |
| CN108918211A (en) * | 2018-05-08 | 2018-11-30 | 西京学院 | A kind of metallic film/amorphous alloy cross-sectional Transmission sample preparation methods |
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| CN105628468A (en) * | 2015-12-28 | 2016-06-01 | 西安电子科技大学 | Method for preparing GaN-based heterojunction transparent film transmission electron microscope sectional sample |
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| CN107478668A (en) * | 2017-08-15 | 2017-12-15 | 合肥工业大学 | A kind of preparation method of heterogeneous alloy EBSD analyses test sample |
| CN108169265A (en) * | 2017-12-20 | 2018-06-15 | 东南大学 | A kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film |
| CN108918211A (en) * | 2018-05-08 | 2018-11-30 | 西京学院 | A kind of metallic film/amorphous alloy cross-sectional Transmission sample preparation methods |
| CN109682848A (en) * | 2018-12-29 | 2019-04-26 | 国合通用测试评价认证股份公司 | A kind of preparation method of the transmissive film sample of Mg-RE-Zn system magnesium alloy |
| CN110514493A (en) * | 2019-08-21 | 2019-11-29 | 西安交通大学 | A kind of electrochemical cleaning and thining method of transmission electron microscope sample |
| CN113218980A (en) * | 2021-04-27 | 2021-08-06 | 苏州鲲腾智能科技有限公司 | High-resolution method for synchronously acquiring and analyzing structure and component information of integrated circuit |
| CN115266268A (en) * | 2022-07-29 | 2022-11-01 | 中国核动力研究设计院 | UO with high fuel consumption 2 Preparation method of nuclear fuel transmission electron microscope sample |
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Application publication date: 20140402 |