CN107121446B - A kind of Cross-section transmission tem sample mechanical pre-thinning method - Google Patents
A kind of Cross-section transmission tem sample mechanical pre-thinning method Download PDFInfo
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- CN107121446B CN107121446B CN201710278227.6A CN201710278227A CN107121446B CN 107121446 B CN107121446 B CN 107121446B CN 201710278227 A CN201710278227 A CN 201710278227A CN 107121446 B CN107121446 B CN 107121446B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/2202—Preparing specimens therefor
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Abstract
The present invention relates to a kind of Cross-section transmission tem sample mechanical pre-thinning methods.This method holds sand paper grinding after sample to be sticked to the center of stainless steel steel column end face together with nut collar.By using the digital display dial gauge multimetering nut collar thickness being fixed on the base to guarantee that the thickness of sample is parallel with top and bottom in process of lapping.Turn-over when buck is to close to original thickness half, and after the same method by buck to 0.03mm.Using method determined by the present invention, the pre- thinned size that sample making course can be overcome to occur is not in place or mill leaks situation.It also avoids sample wearing into wedge shape simultaneously, to obtain damaging the pre- thinned sample that small, thickness is qualified, top and bottom are parallel.Method of the present invention is applicable not only to the pre- of the Cross-section transmission sample at research interface and is thinned, and can equally be well applied to block materials, has many advantages, such as that at low cost, success rate is high.
Description
Technical field
The present invention relates to a kind of by transmission electron microscope sample mechanical pre-thinning to the method for required size, especially suitable for
Cross section transmission electron microscope sample mechanical pre-thinning can equally be well applied to the mechanical pre-thinning of the transmission electron microscope sample of block materials,
Belong to transmission electron microscope sample preparation field.
Background technique
Transmission electron microscope (TEM) is the effective tool of observation and analysis of material pattern, tissue and structure.The system of sample
It is standby that conclusive effect is played in the research of electron micrology.Focused ion beam (FIB) can prepare preferable transmission electron microscope
Sample, but its equipment is expensive, prepares sample cost height, it can not be universal in all scientific research institutions.Therefore, traditional method
Such as it is electrolysed double sprays, ion milling, ultra-thin section are still main transmission electron microscope sample preparation method.These methods are in sample preparation
In the process, it requires sample to be thinned in advance certain thickness.Such as when studying block materials, need sample being thinned to 60 in advance
μm~80 μm of backlash at the small sample of Φ 3, then can prepare preferable transmissive test using the methods of the double sprays of electrolysis.But
For research coating, the cross-sectional sample of coating and making Nano surface sample, sample preparation difficulty is greater than block materials.Such as document
(Chen Chunhuan appoints preparation [J] Physico-chemical tests-physics fascicle of the making Nano surface material cross-section transmission electron microscope samples such as auspicious inscription,
2009,45 (11): 680-683.0) used in method be prepared for preferable cross section sample.But this method is in ion milling
There is still a need for sample is thinned to 30 μm or so in advance before.For diameter be Φ 3 semicircle during the grinding process, it is difficult to ensure that sample
Top and bottom it is parallel, be easy buck wedgewise.Secondly, 30 μm or so of thickness is difficult to control, traditional measurement method
It is to remove sample after the thickness of experience estimation sample, uses the thickness of micrometer caliper measurement sample.And sample is removing survey
The damage of sample is be easy to cause during amount.Other methods are for example placed on buck on polished machine extremely using dedicated fixture
Required thickness, but still can not more be accurately controlled the thickness of sample, also will appear that buck size is not in place, sample
The not parallel problem in top and bottom.Therefore, it is horizontal for preparation how to obtain the parallel mechanical pre-thinning sample in accurate size, top and bottom
Section TEM sample is a very crucial step.
Summary of the invention
It is proposed of the invention is encountered for mechanical be thinned to during 0.030mm or so in advance of Cross-section transmission sample
Pre- thinned size is blocked up or buck perforation, sample are lost and sample top and bottom are not parallel etc. it is pre- be thinned it is low success rate of
Problem proposes a kind of pre- thinned method of feasible Cross-section transmission tem sample.
Such reality that the technical solution of the invention is as follows:
A kind of Cross-section transmission tem sample mechanical pre-thinning method, including diameter be the semicircle sample strip of 3mm, sample,
Washer, stainless steel steel column, the digital display dial gauge being fixed on the base, it is characterised in that the following steps are included:
Step 1: the semicircle sample strip that diameter is 3mm is cut from sample using wire cutting, two semicircle sample strips are used
It is heating and curing by Gatan G2 resin to viscous, and 80~120 DEG C of solidification temperature, curing time 1 hour；
Step 2: the sample strip for being 3mm by the diameter after resin solidification, with the examination under low speed saw cut with a thickness of 0.8mm
Sample；
Step 3: production outer diameter 20mm, internal diameter 6mm, thickness 0.8mm, the washer that material is No. 45 steel；
Step 4: the stainless steel cylinder that production both ends of the surface parallelism tolerance is 0.008mm；
Step 5: stainless steel cylinder being placed on warm table and is heated to 135 DEG C, keeps Gatan paraffin melting, is diameter
3mm, the sample with a thickness of 0.8mm and washer are sticked to the end face of stainless steel steel column, and sample is located at the inside of washer, with tweezers pressure
It is flat；
Step 6: after cementing admittedly, sample and gasket are ground together with 8 word of sandpa-per painting by hand, sand paper number is with sample thickness
Reduction and increase；The digital display dial gauge measurement gasket thickness being fixed on the base is continued on in process of lapping, is padded by measurement
The thickness of piece guarantees the thickness of sample；When measurement, the end face of stainless steel cylinder is set as zero point, measures the number of several points on gasket
Value is inclined to prevent sample mill to observe, and guarantees the depth of parallelism of sample top and bottom；Buck to about with a thickness of 0.4mm when, according to gold
Preparation step fine grinding, the polishing of phase sample；
Step 7: coherent stainless steel cylinder, gasket, sample are put into the beaker for filling acetone, clear with ultrasound
Washing machine cleans and shakes lower sample and gasket；
Step 8: cementing sample and gasket turn-over according to step 5, according to step 6 by sample be fabricated into a thickness of
0.030mm is cleaned according to step 7, obtains qualified sample.
Compared with prior art, it is an advantage of the invention that it will be apparent that being mainly manifested in:
1, sample is placed in the inside of washer, and the two is sticked on stainless steel cylinder using Gatan paraffin, later with tweezers point
Side pressure flat sample and washer make its firm pasting；
2, the depth of parallelism that the digital display dial gauge measurement washer being fixed on the base guarantees sample is continued on in process of lapping
And thickness；
3, the sand paper number that grinding uses increases with the reduction of sample thickness.After buck is to desired size,
Polishing is immersed in the beaker for filling acetone, is put into ultrasonic cleaning and is shaken lower sample.
Detailed description of the invention
The present invention shares 4 width of attached drawing.Wherein:
Fig. 1 is the semicircle sample strip that diameter is 3mm；
Fig. 2 be a pile diameter be 3mm, the sample with a thickness of 0.8mm；
Fig. 3 is that sample and gasket are pasted onto the schematic diagram on stainless steel cylinder；
Fig. 4 is with the digital display dial gauge measurement sample thickness schematic diagram being fixed on the base.
In figure, 1, the semicircle sample strip of diameter 3mm, 2, sample, 3, washer, 4, stainless steel steel column, 5, be fixed on the base
Digital display dial gauge.
Specific embodiment
A kind of Cross-section transmission tem sample mechanical pre-thinning method as shown in Figure 1, Figure 2, Figure 3, Figure 4, including diameter
For the semicircle sample strip 1 of 3mm, sample 2, washer 3, stainless steel steel column 4, the digital display dial gauge 5 being fixed on the base, feature exists
In the following steps are included:
Step 1: the semicircle sample strip 1 that diameter is 3mm is cut from sample using wire cutting, by two semicircle sample strips 1
It is heating and curing to viscous with Gatan G2 resin, 80~120 DEG C of solidification temperature, curing time 1 hour；
Step 2: the sample strip for being 3mm by the diameter after resin solidification, with the examination under low speed saw cut with a thickness of 0.8mm
Sample 2；
Step 3: production outer diameter 20mm, internal diameter 6mm, thickness 0.8mm, the washer 3 that material is No. 45 steel；
Step 4: the stainless steel cylinder 4 that production both ends of the surface parallelism tolerance is 0.008mm；
Step 5: stainless steel cylinder 4 being placed on warm table and is heated to 135 DEG C, keeps Gatan paraffin melting, is diameter
3mm, the sample 2 with a thickness of 0.8mm and washer 3 are sticked to the end face of stainless steel steel column 4, and sample is located at the inside of washer, uses tweezers
It flattens；
Step 6: after cementing admittedly, sample 2 and gasket 3 are ground together with 8 word of sandpa-per painting by hand, sand paper number is with sample thickness
The reduction of degree and increase；The digital display dial gauge 5 being fixed on the base is continued on in process of lapping and measures gasket thickness, by measurement
The thickness of gasket 3 guarantees the thickness of sample 2；When measurement, the end face of stainless steel cylinder 4 is set as zero point, measures number on gasket 3
The numerical value of point is inclined to prevent sample mill to observe, and guarantees the depth of parallelism of 2 top and bottom of sample；Sample 2 is ground to about with a thickness of 0.4mm
When, according to preparation step fine grinding, the polishing of metallographic sample；
Step 7: coherent stainless steel cylinder 4, gasket 3, sample 2 are put into the beaker for filling acetone, with ultrasound
Cleaning machine cleans and shakes lower sample 2 and gasket 3；
Step 8: cementing sample 2 and 3 turn-over of gasket according to step 5, according to step 6 by sample 2 be fabricated into a thickness of
0.030mm is cleaned according to step 7, obtains qualified sample 2.
Claims (1)
1. a kind of Cross-section transmission tem sample mechanical pre-thinning method, semicircle sample strip (1), sample including diameter for 3mm
(2), washer (3), stainless steel steel column (4), the digital display dial gauge (5) being fixed on the base, it is characterised in that the following steps are included:
Step 1: the semicircle sample strip (1) that diameter is 3mm is cut from sample using wire cutting, by two semicircle sample strips (1)
It is heating and curing to viscous with Gatan G2 resin, 80~120 DEG C of solidification temperature, curing time 1 hour；
Step 2: the sample strip for being 3mm by the diameter after resin solidification, with the sample under low speed saw cut with a thickness of 0.8mm
(2)；
Step 3: production outer diameter 20mm, internal diameter 6mm, thickness 0.8mm, the washer (3) that material is No. 45 steel；
Step 4: the stainless steel cylinder (4) that production both ends of the surface parallelism tolerance is 0.008mm；
Step 5: stainless steel cylinder (4) is placed on warm table and is heated to 135 DEG C, keeps Gatan paraffin melting, is diameter
3mm, the sample (2) with a thickness of 0.8mm and washer (3) are sticked to the end face of stainless steel steel column (4), and sample is located at the inside of washer,
It is flattened with tweezers；
Step 6: after cementing admittedly, sample (2) and gasket (3) are ground together with 8 word of sandpa-per painting by hand, sand paper number is with sample thickness
The reduction of degree and increase；Digital display dial gauge (5) the measurement gasket thickness being fixed on the base is continued on in process of lapping, by surveying
The thickness of gasket (3) is measured to guarantee the thickness of sample (2)；When measurement, the end face of stainless steel cylinder (4) is set as zero point, measurement
The numerical value of the upper several points of gasket (3) is inclined to prevent sample (2) mill to observe, and guarantees the depth of parallelism of sample (2) top and bottom；Buck arrives
When about with a thickness of 0.4mm, according to preparation step fine grinding, the polishing of metallographic sample；
Step 7: coherent stainless steel cylinder (4), gasket (3), sample (2) are put into the beaker for filling acetone, with super
Sound cleaning machine cleans and shakes lower sample (2) and gasket (3)；
Step 8: sample (2) and gasket (3) turn-over are cemented according to step 5, sample (2) is fabricated into thickness according to step 6
It for 0.030mm, is cleaned according to step 7, obtains qualified sample (2).
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710278227.6A CN107121446B (en) | 2017-04-25 | 2017-04-25 | A kind of Cross-section transmission tem sample mechanical pre-thinning method |
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| CN201710278227.6A CN107121446B (en) | 2017-04-25 | 2017-04-25 | A kind of Cross-section transmission tem sample mechanical pre-thinning method |
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| CN107121446B true CN107121446B (en) | 2019-10-22 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107855923B (en) * | 2017-11-07 | 2019-11-05 | 西北工业大学 | The polishing method of organic inorganic hybridization halide perovskite semiconductor crystal |
| CN112834300B (en) * | 2020-12-31 | 2023-07-25 | 苏州热工研究院有限公司 | Preparation method of metal material transmission electron microscope slice sample |
| CN113176284A (en) * | 2021-03-22 | 2021-07-27 | 中国原子能科学研究院 | Sample preparation method suitable for radioactive small punch test and transmission electron microscope |
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| CN201442215U (en) * | 2009-04-03 | 2010-04-28 | 大连交通大学 | Mechanical pre-thinning device used for transmission electron microscopy sample preparation process |
| CN202255998U (en) * | 2011-07-30 | 2012-05-30 | 北京科技大学 | Structure for fixing transmission electron microscope thin film samples during process of pre-reduction grinding |
| CN102519771A (en) * | 2011-12-30 | 2012-06-27 | 青岛大学 | Method for preparing cross section transmission electron microscope sample |
| CN103308362A (en) * | 2013-06-14 | 2013-09-18 | 首钢总公司 | Sample preparation method of alloying hot-dip galvanized coating section transmission sample |
| CN103487303A (en) * | 2013-09-30 | 2014-01-01 | 首钢总公司 | Method for preparing cross-section transmission electron microscope sample of cold-rolled sheet |
| CN104075928A (en) * | 2014-06-13 | 2014-10-01 | 北京工业大学 | Method for mechanically thinning grinding wafer transmission electron microscope test sample |
| CN105115795A (en) * | 2015-07-20 | 2015-12-02 | 北京大学 | Preparation method of micron-size sheet transmission electron microscope cross-sectional sample |
-
2017
- 2017-04-25 CN CN201710278227.6A patent/CN107121446B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201442215U (en) * | 2009-04-03 | 2010-04-28 | 大连交通大学 | Mechanical pre-thinning device used for transmission electron microscopy sample preparation process |
| CN202255998U (en) * | 2011-07-30 | 2012-05-30 | 北京科技大学 | Structure for fixing transmission electron microscope thin film samples during process of pre-reduction grinding |
| CN102519771A (en) * | 2011-12-30 | 2012-06-27 | 青岛大学 | Method for preparing cross section transmission electron microscope sample |
| CN103308362A (en) * | 2013-06-14 | 2013-09-18 | 首钢总公司 | Sample preparation method of alloying hot-dip galvanized coating section transmission sample |
| CN103487303A (en) * | 2013-09-30 | 2014-01-01 | 首钢总公司 | Method for preparing cross-section transmission electron microscope sample of cold-rolled sheet |
| CN104075928A (en) * | 2014-06-13 | 2014-10-01 | 北京工业大学 | Method for mechanically thinning grinding wafer transmission electron microscope test sample |
| CN105115795A (en) * | 2015-07-20 | 2015-12-02 | 北京大学 | Preparation method of micron-size sheet transmission electron microscope cross-sectional sample |
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