CN108169265A - A kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film - Google Patents
A kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film Download PDFInfo
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- CN108169265A CN108169265A CN201711379373.4A CN201711379373A CN108169265A CN 108169265 A CN108169265 A CN 108169265A CN 201711379373 A CN201711379373 A CN 201711379373A CN 108169265 A CN108169265 A CN 108169265A
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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
A kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film intercepts wire sample and stretches fixation；A pair of of molybdenum annulus is affixed on wire up and down, wire is made to expose from molybdenum annulus hollow part, the wire cut outside molybdenum ring completes encapsulation；Packaged molybdenum ring is put on the sample stage of Ion Beam Thinner, 1 ~ 5Kev of ion energy, 1 ° ~ 10 ° of Ion beam incident angles are thinned, the situation that observation sample is thinned, after wire occurs perforating or disconnect from centre, you can sample is taken out to obtain Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film.The present invention is easy to operate, and success rate is high, and sample preparation is at low cost, can also avoid the deformation occurred in sample making course, pollution, it is decrystallized the problems such as, significantly reduce sample access, the difficulty preserved；It can be widely applied to prepare the wire longitudinal section sample of superfine diameter.
Description
Technical field
The invention belongs to TEM sample preparation fields, provide a kind of Gas in Ultra-thin Metal Wires（Minimum diameter 0.05mm）Longitudinal section
Method prepared by transmission electron microscope film sample.
Background technology
Transmission electron microscope is the important means for observing metal material microstructure.It is preceding using transmission electron microscope observing material structure
Carry is to prepare qualified film sample.The method for preparing transmissive film sample is mainly electrolysed double spray, focused ion beam cutting
Method, Ion beam modulating etc..
Prepare Gas in Ultra-thin Metal Wires（Diameter≤0.3mm）Film sample is difficult.1）The double spray reductions of electrolysis, sample preparation folder
A diameter of Φ 3.0mm of tool, undersized sample can not shelter from the hole in fixture, in the double spray process of electrolysis, sample
Stabilization is cannot keep in two electrolyte columns, leads to sample easily deformed damaged；Simultaneously because photoelectric sensor system can not be utilized
It automatically determines whether to perforate, sample preparation procedure can be caused uncontrolled.Sample is prepared using the methods of plating, splicing, bonding,
It also is difficult to ensure sample quality.In addition, preservation after sample preparation, observation there are difficulty it is higher the problem of.2）Focused ion
Beam reduction（FIB）, need expensive special equipment（Scanning electron microscope equipped with ion gun, mechanical arm）, the sample preparation time is long, takes
With costliness；It is minimum for size（Diameter≤0.3mm）Sample clamping, in sampling process it is all more difficult, in addition, focused ion beam
Can lead to occur amorphous structure in sample in sample making course, cause structure observation, material analysis erroneous judgement.3）Ion beam is thinned
Method, fixture be for standard size preparation of samples, fine wire sample directly carry out ion beam bombardment can cause wire from
Centre fracture, causes subsequent samples, transfer process difficult, also there are sample vulnerable to pollution, is difficult to be fixed on TEM sample platform
The problems such as upper.
Invention content
The technical issues of solution：The invention reside in the systems for providing a kind of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope film sample
Preparation Method.Using the stationary fixture of design and thin slice molybdenum ring, realize to Gas in Ultra-thin Metal Wires（Minimum diameter 0.05mm）Encapsulation；
It is thinned using ion beam and prepares qualified TEM film samples.Sample can carry out transmission electron microscope structure observation, electron diffraction spot
Analysis
Technical solution：A kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film, preparation process are：1）Sample
It intercepts and fixed：Interception wire sample simultaneously stretches fixation；2）Molybdenum ring seal fills：A pair of of molybdenum annulus is affixed on wire up and down,
Wire is made to expose from molybdenum annulus hollow part, the wire cut outside molybdenum ring completes encapsulation；3）Ion beam is thinned：It will envelope
The molybdenum ring installed is put on the sample stage of Ion Beam Thinner, 1 ~ 5Kev of ion energy, and 1 ° ~ 10 ° of Ion beam incident angles are thinned,
The situation that observation sample is thinned, after wire occurs perforating or disconnect from centre, you can sample is taken out to obtain Gas in Ultra-thin Metal Wires
Longitudinal section transmission electron microscope sample film.
When above-mentioned sample is fixed, first one end of wire is fixed and limited, is stretched, then the steel wire other end is limited
It is and fixed.
Preferably, when above-mentioned ion beam is thinned, ion beam incident angle is 3 °.
Preferably, when above-mentioned ion beam is thinned, ion beam energy 3Kev.
Preferably, a diameter of 3mm of above-mentioned molybdenum ring, thickness are not more than 40 μm.
Advantageous effect：The present invention is easy to operate, and success rate is high, and sample preparation is at low cost（Only 1/10th of FIB）.It can also avoid
The deformation that occurs in sample making course, pollution, it is decrystallized the problems such as, significantly reduce sample access, the difficulty preserved；It can be extensive
It is used to prepare superfine diameter（0.05~0.3mm）Wire longitudinal section sample.
Description of the drawings
Fig. 1 is fixture structure schematic diagram；1- bolts, 2- steel wires, 3- grooves；
Fig. 2 is the sample drawing for preparing completion；
Fig. 3 is filament thin film transmission electron microscope sample drawing, is sample observation result in embodiment 1.Wherein A）Low power number is observed
Under sample, B）The bright field image of wire sample, C）With the electron diffraction pattern in region.
Fig. 4 is filament thin film transmission electron microscope sample drawing.
Specific embodiment
The invention will be further elaborated by the following examples.The present embodiment is based on the technical solution of the present invention
Under implemented, give detailed embodiment and process, but the scope of the present invention is not limited to following embodiments.
Embodiment 1：Cold-drawn deformation pearlite steel wire（Diameter 0.05mm）The preparation of longitudinal section film sample
1）Sample intercepts：3 sections of steel wire samples are intercepted, per segment length about 20cm.
2）Sample is fixed：Steel wire one end is fixed on the bolt of fixture side, across the groove on fixture, stretched to another
Side, and across the groove of opposite side, then be fixed on the bolt of fixture opposite side.Other two sample is also in the same way
It is fixed.Fixing device is shown in Fig. 1.
3）Molybdenum ring seal fills：Molybdenum ring is placed on the fine wire of three laid out in parallel, is adhesively fixed with glue；Treat that glue coagulates
After Gu, molybdenum ring is pasted in the another side of metal, makes to expose a steel wire in molybdenum annular distance；Cut the metal outside molybdenum ring
Silk.
4）Ion beam is thinned：The sample that molybdenum ring seal installs is put on the sample stage of Ion Beam Thinner, using reasonably from
Parameter is thinned in beamlet（1 ~ 5Kev of ion energy, 1 ° ~ 10 ° of Ion beam incident angles）It is thinned.Time interval length is thinned to be set as
10~20min。
5）After wire occurs perforating or disconnect from centre, you can take out sample, for tem analysis.
6）During Fig. 3 sample makings, final ion beam incident angle is 3 °, energy 3Kev.Sample surfaces are without damage, thin area
The amorphous area that edge is not damaged by ion beam.
7）During Fig. 4 sample makings, final ion beam incident angle is 8 °, energy 5Kev.Thin area edge exists by ion
The amorphous area of beam damage, while surface damage is apparent.
Embodiment 2：Cold-drawn deformation pearlite steel wire（Diameter 0.15mm）The preparation of longitudinal section film sample
1）Sample intercepts：3 sections of steel wire samples are intercepted, per segment length about 20cm.
2）Sample is fixed：Steel wire one end is fixed on the bolt of fixture side, across the groove on fixture, stretched to another
Side, and across the groove of opposite side, then be fixed on the bolt of fixture opposite side.Other two sample is also in the same way
It is fixed.Fixing device is shown in Fig. 1.
3）Molybdenum ring seal fills：Molybdenum ring is placed on the fine wire of three laid out in parallel, is adhesively fixed with glue；Treat that glue coagulates
After Gu, molybdenum ring is pasted in the another side of metal, makes to expose a steel wire in molybdenum annular distance；Cut the metal outside molybdenum ring
Silk.
4）Ion beam is thinned：The sample that molybdenum ring seal installs is put on the sample stage of Ion Beam Thinner, using reasonably from
Parameter is thinned in beamlet（3 ~ 5Kev of ion energy, 3 ° ~ 10 ° of Ion beam incident angles）It is thinned.Time interval length is thinned to be set as
20~35min。
5）After wire occurs perforating or disconnect from centre, you can take out sample, for tem analysis.
Embodiment 3：Cold-drawn deformation pearlite steel wire（Diameter 0.30mm）The preparation of longitudinal section film sample
1）Sample intercepts：3 sections of steel wire samples are intercepted, per segment length about 20cm.
2）Sample is fixed：Steel wire one end is fixed on the bolt of fixture side, across the groove on fixture, stretched to another
Side, and across the groove of opposite side, then be fixed on the bolt of fixture opposite side.Other two sample is also in the same way
It is fixed.Fixing device is shown in Fig. 1.
3）Molybdenum ring seal fills：Molybdenum ring is placed on the fine wire of three laid out in parallel, is adhesively fixed with glue；Treat that glue coagulates
After Gu, molybdenum ring is pasted in the another side of metal, makes to expose a steel wire in molybdenum annular distance；Cut the metal outside molybdenum ring
Silk.
4）Ion beam is thinned：The sample that molybdenum ring seal installs is put on the sample stage of Ion Beam Thinner, using reasonably from
Parameter is thinned in beamlet（3 ~ 5Kev of ion energy, 3 ° ~ 10 ° of Ion beam incident angles）It is thinned.Time interval length is thinned to be set as
30~45min。
5）After wire occurs perforating or disconnect from centre, you can take out sample, for tem analysis.
Claims (5)
1. a kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film, it is characterised in that preparation process is：1）
Sample is intercepted and is fixed：Interception wire sample simultaneously stretches fixation；2）Molybdenum ring seal fills：A pair of of molybdenum annulus is affixed on wire up and down
On, wire is made to expose from molybdenum annulus hollow part, the wire cut outside molybdenum ring completes encapsulation；3）Ion beam is thinned：
Packaged molybdenum ring is put on the sample stage of Ion Beam Thinner, 1 ~ 5Kev of ion energy, 1 ° ~ 10 ° progress of Ion beam incident angles
It is thinned, the situation that observation sample is thinned, after wire occurs perforating or disconnect from centre, you can sample is taken out to obtain ultra-fine gold
Belong to silk longitudinal section transmission electron microscope sample film.
2. a kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film according to claim 1, feature
When being that the sample is fixed, first one end of wire is fixed and limited, is stretched, then the steel wire other end is limited and consolidated
It is fixed.
3. a kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film according to claim 1, feature
When being that ion beam is thinned, ion beam incident angle is 3 °.
4. a kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film according to claim 1, feature
When being that ion beam is thinned, ion beam energy 3Kev.
5. a kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film according to claim 1, feature
It is a diameter of 3mm of molybdenum ring, thickness is not more than 40 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711379373.4A CN108169265A (en) | 2017-12-20 | 2017-12-20 | A kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film |
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| CN201711379373.4A CN108169265A (en) | 2017-12-20 | 2017-12-20 | A kind of preparation method of Gas in Ultra-thin Metal Wires longitudinal section transmission electron microscope sample film |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117405719A (en) * | 2023-12-14 | 2024-01-16 | 崇义章源钨业股份有限公司 | Thin film material section scanning electron microscope sample preparation device |
Citations (5)
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|---|---|---|---|---|
| CN102841005A (en) * | 2012-09-20 | 2012-12-26 | 东南大学 | Preparation method for thin steel wire transmission electron microscope sample |
| CN103698178A (en) * | 2013-12-12 | 2014-04-02 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for thin-film sample for high-resolution transmission electron microscope |
| CN104792595A (en) * | 2015-04-23 | 2015-07-22 | 江苏省沙钢钢铁研究院有限公司 | Preparation method of thin steel wire longitudinal sectional electronic microscopic sample |
| CN105334095A (en) * | 2015-12-01 | 2016-02-17 | 贵州大学 | Sample preparation method and device for metal material transmission electron microscope with diameter of less than 3 mm |
| CN105973674A (en) * | 2016-07-01 | 2016-09-28 | 中国科学院地质与地球物理研究所 | Preparation method of transmission electron microscope sample with large area of thin region |
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- 2017-12-20 CN CN201711379373.4A patent/CN108169265A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102841005A (en) * | 2012-09-20 | 2012-12-26 | 东南大学 | Preparation method for thin steel wire transmission electron microscope sample |
| CN103698178A (en) * | 2013-12-12 | 2014-04-02 | 中国航空工业集团公司北京航空材料研究院 | Preparation method for thin-film sample for high-resolution transmission electron microscope |
| CN104792595A (en) * | 2015-04-23 | 2015-07-22 | 江苏省沙钢钢铁研究院有限公司 | Preparation method of thin steel wire longitudinal sectional electronic microscopic sample |
| CN105334095A (en) * | 2015-12-01 | 2016-02-17 | 贵州大学 | Sample preparation method and device for metal material transmission electron microscope with diameter of less than 3 mm |
| CN105973674A (en) * | 2016-07-01 | 2016-09-28 | 中国科学院地质与地球物理研究所 | Preparation method of transmission electron microscope sample with large area of thin region |
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| 姜训勇 等: "细金属丝透射电镜试样的制备", 《理化检验-物理分册》 * |
| 徐炜 等: "透射电镜用掺杂钨丝薄膜试样制备的新方法", 《稀有金属》 * |
| 董林 等: "丝材及粒材的透射电镜试样制备方法", 《理化检验-物理分册》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117405719A (en) * | 2023-12-14 | 2024-01-16 | 崇义章源钨业股份有限公司 | Thin film material section scanning electron microscope sample preparation device |
| CN117405719B (en) * | 2023-12-14 | 2024-03-05 | 崇义章源钨业股份有限公司 | Thin film material section scanning electron microscope sample preparation device |
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Application publication date: 20180615 |