CN107121446A - 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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- CN107121446A CN107121446A CN201710278227.6A CN201710278227A CN107121446A CN 107121446 A CN107121446 A CN 107121446A CN 201710278227 A CN201710278227 A CN 201710278227A CN 107121446 A CN107121446 A CN 107121446A
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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 method.Sample is bonded at hand-held sand paper behind the center of stainless steel steel column end face together with nut collar and ground by this method.By using the digital display dial gauge multimetering nut collar thickness being fixed on base to ensure that the thickness of sample is parallel with top and bottom in process of lapping.Buck is to close to turn-over during 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 grinds leakage situation.Also avoid sample wearing into wedge shape simultaneously, so as to obtain the damage pre- thinned sample that small, thickness is qualified, top and bottom are parallel.Method of the present invention is applicable not only to study the pre- of the Cross-section transmission sample at interface and is thinned, and can equally be well applied to block materials, has the advantages that cost is low, success rate is high.
Description
Technical field
The present invention relates to it is a kind of by transmission electron microscope sample mechanical pre-thinning to the method for required size, be particularly suitable for use in
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 technology
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, it is high to prepare sample cost, can not be popularized in all scientific research institutions.Therefore, traditional method
It is still main transmission electron microscope sample preparation method to be such as electrolysed double sprays, ion milling, ultra-thin section.These methods are in sample preparation
During, it is required for sample being thinned in advance certain thickness.Such as when studying block materials, it is necessary to which sample is thinned into 60 in advance
μm~80 μm of backlash into Φ 3 small sample, then can prepare preferable transmissive test using the methods of the double sprays of electrolysis.But
For the cross-sectional sample of research coating, coating and making Nano surface sample, its sample preparation difficulty is more 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)：The method used in 680-683.0) is prepared for preferable cross section sample.But this method is in ion milling
Still need to be thinned to sample into 30 μm or so in advance before.For a diameter of Φ 3 semicircle in process of lapping, it is difficult to ensure that sample
Top and bottom it is parallel, easily by buck wedgewise.Secondly, 30 μm or so of thickness is difficult control, traditional measuring method
It is to remove sample after estimating the thickness of sample by experience, the thickness of sample is measured using micrometer caliper.And sample is removing survey
The damage of sample is easily caused during amount.Other methods are for example placed on buck on polished machine extremely using special fixture
Required thickness, but still can not more be accurately controlled the thickness of sample, also occurs that buck size is not in place, sample
The problem of top and bottom are not parallel.Therefore, the parallel mechanical pre-thinning sample in accurate size, top and bottom how is obtained horizontal for preparing
Section TEM sample is a very crucial step.
The content of the invention
The proposition of the present invention, runs into for pre- be thinned to during 0.030mm or so of Cross-section transmission sample machinery
Pre- thinned size is blocked up or buck perforation, sample are lost, and sample top and bottom it is 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.
The technical solution of the present invention is such reality：
A kind of Cross-section transmission tem sample mechanical pre-thinning method, including a diameter of 3mm semicircle sample strip, sample,
Packing ring, stainless steel steel column, the digital display dial gauge being fixed on base, it is characterised in that comprise the following steps：
Step one：A diameter of 3mm semicircle sample strip is cut from sample using wire cutting, two semicircle sample strips are used
It is heating and curing by Gatan G2 resins to viscous, 80~120 DEG C of solidification temperature, 1 hour hardening time；
Step 2：By the sample strip of a diameter of 3mm after resin solidification, with the examination that thickness is 0.8mm under low speed saw cut
Sample；
Step 3：Make the packing ring that external diameter 20mm, internal diameter 6mm, thickness 0.8mm, material are No. 45 steel；
Step 4：Make the stainless steel cylinder that both ends of the surface parallelism tolerance is 0.008mm；
Step 5：Stainless steel cylinder is placed on warm table and is heated to 135 DEG C, makes Gatan paraffin melting, a diameter of
3mm, thickness are bonded at the end face of stainless steel steel column for 0.8mm sample and packing ring, and sample is located at the inside of packing ring, uses tweezers pressure
It is flat；
Step 6：After cementing admittedly, sample and pad are together ground with the word of sandpa-per painting 8 by hand, sand paper number is with sample thickness
Reduction and increase；The digital display dial gauge measurement gasket thickness being fixed on base is continued on in process of lapping, is padded by measurement
The thickness of piece ensures the thickness of sample；During measurement, the end face of stainless steel cylinder is set as the number of several points on zero point, measurement pad
Value is inclined to prevent sample mill to observe, it is ensured that the depth of parallelism of sample top and bottom；Buck to about thickness be 0.4mm when, according to gold
The preparation process fine grinding of phase sample, polishing；
Step 7：Coherent stainless steel cylinder, pad, sample are put into the beaker for filling acetone, it is clear with ultrasound
Washing machine is cleaned and shakes lower sample and pad；
Step 8：Sample is cemented with pad turn-over according to step 5, sample is fabricated into thickness according to step 6 is
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：
1st, sample is placed in the inside of packing ring, and both are bonded on stainless steel cylinder using Gatan paraffin, afterwards with tweezers point
Side pressure flat sample and packing ring, make its firm pasting；
2nd, the depth of parallelism that the digital display dial gauge measurement packing ring being fixed on base ensures sample is continued on in process of lapping
And thickness；
3rd, the sand paper number that grinding is used increases with the reduction of sample thickness.After buck is to desired size,
Polishing, immersion is filled in the beaker of acetone, is put into ultrasonic cleaning and is shaken lower sample.
Brief description of the drawings
The shared width of accompanying drawing 4 of the present invention.Wherein：
Fig. 1 is a diameter of 3mm semicircle sample strip；
Fig. 2 is the sample that a diameter of 3mm of a pile, thickness are 0.8mm；
Fig. 3 is the schematic diagram that sample is pasted onto with pad on stainless steel cylinder；
Fig. 4 is with the digital display dial gauge measurement sample thickness schematic diagram being fixed on base.
In figure, 1, diameter 3mm semicircle sample strip, 2, sample, 3, packing ring, 4, stainless steel steel column, 5, be fixed on base
Digital display dial gauge.
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 3mm semicircle sample strip 1, sample 2, packing ring 3, stainless steel steel column 4, the digital display dial gauge 5 being fixed on base, its feature exists
In comprising the following steps：
Step one：A diameter of 3mm semicircle sample strip 1 is cut from sample using wire cutting, by two semicircle sample strips 1
It is heating and curing to viscous with Gatan G2 resins, 80~120 DEG C of solidification temperature, 1 hour hardening time；
Step 2：By the sample strip of a diameter of 3mm after resin solidification, with the examination that thickness is 0.8mm under low speed saw cut
Sample 2；
Step 3：Make the packing ring 3 that external diameter 20mm, internal diameter 6mm, thickness 0.8mm, material are No. 45 steel；
Step 4：Make the stainless steel cylinder 4 that 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, makes Gatan paraffin melting, a diameter of
3mm, thickness are bonded at the end face of stainless steel steel column 4 for 0.8mm sample 2 and packing ring 3, and sample is located at the inside of packing ring, uses tweezers
Flatten；
Step 6：After cementing admittedly, sample 2 and pad 3 are together ground with the word of sandpa-per painting 8 by hand, sand paper number is thick with sample
The reduction of degree and increase；The measurement gasket thickness of digital display dial gauge 5 being fixed on base is continued on in process of lapping, by measurement
The thickness of pad 3 ensures the thickness of sample 2；During measurement, the end face of stainless steel cylinder 4 is set as number on zero point, measurement pad 3
The numerical value of point is inclined to prevent sample mill to observe, it is ensured that the depth of parallelism of the top and bottom of sample 2；It is 0.4mm that sample 2, which is ground to about thickness,
When, according to the preparation process fine grinding of metallographic sample, polishing；
Step 7：Coherent stainless steel cylinder 4, pad 3, sample 2 are put into the beaker for filling acetone, with ultrasound
Cleaning machine cleans and shakes lower sample 2 and pad 3；
Step 8：Sample 2 is cemented with the turn-over of pad 3 according to step 5, sample 2 is fabricated into thickness according to step 6 is
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, includes a diameter of 3mm semicircle sample strip (1), sample
(2), packing ring (3), stainless steel steel column (4), the digital display dial gauge (5) being fixed on base, it is characterised in that comprise the following steps：
Step one：A diameter of 3mm semicircle sample strip (1) is cut from sample using wire cutting, by two semicircle sample strips (1)
It is heating and curing to viscous with Gatan G2 resins, 80~120 DEG C of solidification temperature, 1 hour hardening time；
Step 2：By the sample strip of a diameter of 3mm after resin solidification, with the sample that thickness is 0.8mm under low speed saw cut
(2)；
Step 3：Make the packing ring (3) that external diameter 20mm, internal diameter 6mm, thickness 0.8mm, material are No. 45 steel；
Step 4：Make the stainless steel cylinder (4) that 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, makes Gatan paraffin melting, a diameter of
3mm, thickness are bonded at the end face of stainless steel steel column (4) for 0.8mm sample (2) and packing ring (3), and sample is located at the inside of packing ring,
Flattened with tweezers；
Step 6：After cementing admittedly, sample (2) and pad (3) are together ground with the word of sandpa-per painting 8 by hand, sand paper number is thick with sample
The reduction of degree and increase；Digital display dial gauge (5) the measurement gasket thickness being fixed on base is continued on in process of lapping, by surveying
The thickness of pad (3) is measured to ensure the thickness of sample (2)；During measurement, the end face of stainless steel cylinder (4) is set as zero point, measurement
The numerical value of the upper several points of pad (3) is inclined to prevent sample (2) mill to observe, it is ensured that the depth of parallelism of sample (2) top and bottom；Buck is arrived
When about thickness is 0.4mm, according to the preparation process fine grinding of metallographic sample, polishing；
Step 7：Coherent stainless steel cylinder (4), pad (3), sample (2) are put into the beaker for filling acetone, with super
Sound cleaning machine cleans and shakes lower sample (2) and pad (3)；
Step 8：Sample (2) is cemented with pad (3) turn-over according to step 5, sample (2) is fabricated into thickness according to step 6
For 0.030mm, cleaned according to step 7, obtain qualified sample (2).
Priority Applications (1)
| 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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| CN107121446A true CN107121446A (en) | 2017-09-01 |
| CN107121446B CN107121446B (en) | 2019-10-22 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107855923A (en) * | 2017-11-07 | 2018-03-30 | 西北工业大学 | The polishing method of organic inorganic hybridization halide perovskite semiconductor crystal |
| CN112834300A (en) * | 2020-12-31 | 2021-05-25 | 苏州热工研究院有限公司 | Preparation method of sheet sample of metal material for transmission electron microscope |
| 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 |
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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 |
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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 |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107855923A (en) * | 2017-11-07 | 2018-03-30 | 西北工业大学 | The polishing method of organic inorganic hybridization halide perovskite semiconductor crystal |
| 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 |
| CN112834300A (en) * | 2020-12-31 | 2021-05-25 | 苏州热工研究院有限公司 | Preparation method of sheet sample of metal material for transmission electron microscope |
| 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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| CN107121446B (en) | 2019-10-22 |
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