CN105334095A - Sample preparation method and device for metal material transmission electron microscope with diameter of less than 3 mm - Google Patents
Sample preparation method and device for metal material transmission electron microscope with diameter of less than 3 mm Download PDFInfo
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- CN105334095A CN105334095A CN201510859253.9A CN201510859253A CN105334095A CN 105334095 A CN105334095 A CN 105334095A CN 201510859253 A CN201510859253 A CN 201510859253A CN 105334095 A CN105334095 A CN 105334095A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2866—Grinding or homogeneising
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
- G01N2001/2873—Cutting or cleaving
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Abstract
The invention discloses a sample preparation method and a sample preparation device for a metal material transmission electron microscope with the diameter of less than 3 mm. The sample preparation device comprises a barrel and a barrel cover, wherein a first blind taper hole is formed in the middle part of the inner bottom side of the barrel; the barrel cover is arranged at the upper end of the barrel; a second blind taper hole and a pouring opening are formed in the middle part of the inner side of the barrel cover; the barrel wall is of a cavity; a water inlet and a water outlet are formed in the outer wall of the cavity. The sample preparation method comprises the following steps: vertically placing a metal material with the cross section diameter of less than 3 mm in the sample preparation device; introducing cooling water into the cavity; pouring molten metal Sn for solidifying. According to the sample preparation method and the sample preparation device, metal materials with the cross section diameters of between 0.5 and 3 mm can be adapted to the barrel for thickening and sample preparing, so that the sample preparation method and the sample preparation device have universality; the solidifying time can be shortened by adopting out-of-barrel cooling; meanwhile, the influence on the structure of the metal material caused by over-high temperature of the solution of the molten metal Sn is avoided; moreover, the metal material is self-positioned by the two tapered blind taper holes; therefore, the sample preparation method and the sample preparation device have the advantages that the positioning is accurate, the pouring thickness uniformity is ensured, the structure is simple, the device is light, convenient and compact, the manufacturing cost is low and the like.
Description
Technical field
The present invention relates to method for making sample and device that a kind of diameter is less than 3mm metal material transmission electron microscope, belong to material analysis test metal material sample preparation technology field.
Background technology
Material microstructure characterizes the pattern comprising tissues observed, the crystal structure determining phase and analyzes its chemical composition.Transmission electron microscope is at the defect of research material, tiny precipitated phase and utilize in ordered state of the direct display material Atom of high resoltion lattice image or atomic group etc. and have vital role.But transmission electron microscopy sample preparation process relative complex, and there is certain requirement.Usually require that the diameter of section of sample is greater than 3mm, and part metals material is after large deformation amount, macroscopic cross section is generally less than 3mm, and the sample that preparation is applicable to transmission electron microscope observing is often very difficult.At present, in laboratory, the main method adopted is focused ion beam In situcut, adopt the electron microscopic sample that focused ion beam In situcut can be of moderate size, thickness is suitable, but cost is high, length consuming time, and requires higher to human users, people also try to find the method that sample for use in transmitted electron microscope prepared by other applicable small bore metal material, publication number is the preparation method disclosing a kind of finer wire transmission electron microscope longitudinal section sample in the Chinese patent application of CN104792595A, finer wire sample shear mainly becomes length to be the first sample of 5 ~ 10mm by it, solidification glue is injected in the mould that bottom is smooth, mold bottom is laid in by equally spaced for first sample, heating makes it solidify, then the sample and mould that are cured is separated, sample is ground to turn-over grinding behind steel wire diameter 1/2 place, be milled to after thickness 85 ~ 100um is, the sequin that diameter is is gone out with piercer, the sample summary of the invention of transmission electron microscope observing is finally suitable for the thinning acquisition of two spray.But the large and sample of workload is easy to worn outly to be difficult to firmly evenly because area is excessive during this method mechanical reduction.The Chinese patent application of publication number CN103335872A discloses the successful preparation achieving diameter 1mm filament sample longitudinal section film by the two spray method of electrolysis and diameter 3mm aperture sample folder, but this method operation easier is large, and the filament of φ 1mm can only be used for, sample specification is single, does not have versatility.Publication number is that the Chinese patent of CN102841005A proposes to adopt the method for nickel plating to make the method for sample for use in transmitted electron microscope to the finer wire of 0.9 ~ 3mm, but the method carries out surface treatment to sample, and length consuming time, cost is high.
Summary of the invention
The technical problem to be solved in the present invention is: the method for making sample providing a kind of diameter of section to be less than 3mm metal material transmission electron microscope and sample preparation device, may be used for the metal material that cross section is 0.5 ~ 3mm, there is versatility, consuming time short, to solve problems of the prior art.
The technical scheme that the present invention takes is: a kind of diameter is less than the method for making sample of 3mm metal material transmission electron microscope, comprises the following steps:
(1) sample is filled: metal material diameter of section being less than 3mm is vertically placed on the drum of sample preparation device and the middle part of bung;
(2) potting syrup processed: low-melting-point metal Sn is put into graphite crucible and be heated to more than 232 DEG C by batch-type furnace and make it melt;
(3) by step (2) molten metal Sn solution casting in the drum in step (1), be covered with around metal material, after the metal Sn around metal material is solidified, it is taken out from sample preparation device, obtain the metal material sample that diameter of section is greater than 3mm;
(4) the technologic material sample wire cutting machine in step (3) is cut out the thick thin slice of 1mm;
(5) thin slice in step (4) is mechanical grinding to below 100um;
(6) the thin slice piercer after polishing is gone out the sequin that diameter is 3mm, during punching, guarantee that initial metal material is centrally located at piercer punch-center;
(7) sequin just after punching loads in the fixture of the two spray instrument of electrolysis, and it is thinning to carry out twin-jet electropolishing, namely obtains the sample for TEM (transmission electron microscope) analysis.
Preferably, before sample preparation, at the inner side of above-mentioned sample preparation device drum coating releasing material, thus prevent together with metal Sn solution is set in sample preparation device, conveniently stripped.
Preferably, blind taper hole one and the blind taper hole two of formed objects fixing metal material is respectively equipped with in the drum bottom centre of sample preparation device and bung medial center, metal material two ends are inserted in two blind taper holes respectively, two blind taper hole vertical directions keep coaxial, guarantee that cross section is fixed on the center of sample preparation device drum at the metal material being less than 3mm, thus make the thickness of the metal Sn of metal material sample surrounding set even.
Preferably, at the barrel of above-mentioned sample preparation device drum, the cavity passing into chilled water is set, in described step (3), pass into the metal Sn of chilled water to cast carry out cooled and solidified, when molten metal Sn solution pours into around metal material, the temperature of metal Sn solution in drum reduces by the chilled water of cavity immediately makes it solidify, thus avoid the too high microstructure to metal material of molten metal Sn solution temperature to have an impact, accelerate the speed that metal Sn solution solidifies simultaneously, shorten experimental period.
A kind of diameter is less than the sample preparation device of 3mm metal material transmission electron microscope, comprise drum and bung, the blind taper hole one placing sample is provided with in the middle part of bottom side in described drum, upper end is provided with bung, described bung middle inside is provided with the blind taper hole two placing sample, and is provided with sprue gate, and its barrel of wall is the cavity of hollow structure, described cavity comprises outer wall and inwall, and described outer wall is provided with the water inlet and water delivering orifice that are communicated with cavity.
Preferably, be threaded connection between above-mentioned bung and drum, can install fast, convenient to operation.
Preferably, above-mentioned water inlet is arranged on outer wall near top side, described water delivering orifice is arranged on outer wall near bottom side, contrary with water inlet direction, chilled water enters from drum one side bottom, flows out from opposite side top, can be more evenly good to inwall cooling, cooling effect is better, and the sample performance after cast is better.
Preferably, above-mentioned blind taper hole one and blind taper hole two internal diameter size, from 0.5 ~ 3mm transition, can meet the requirement of the metal material TEM sample preparation being less than 3mm.
Preferably, above-mentioned sprue gate is the through hole that bung cylindrical arranges two symmetrical platforms and inner wall and formed, and adopts two sprue gates of this structure, can realize cast fast, and is convenient to turn bung and loads and unloads.
The present invention can increase thick to more than 3mm by the pair cross-section metal material that is less than 3mm fast, reach the size being applicable to preparing sample for use in transmitted electron microscope, metal material between the 0.5 ~ 3mm of cross section is fixed on the center of bucket in experimental provision, then from sprue gate by around molten metal Sn solution casting to metal material, simultaneously in outer barrel, logical recirculated water cools.
Beneficial effect of the present invention: compared with prior art, can adapt to diameter of section in drum of the present invention is that metal material between 0.5 ~ 3mm carries out overstriking sample preparation, there is versatility, it is short that employing carries out cooling time place metal Sn solution can solidified outside drum, avoid the too high tissue to metal material of molten metal Sn solution temperature to have an impact simultaneously, and two of taper blind taper holes carry out self-align to metal material, there is accurate positioning, ensure the Sn metal thickness homogeneity of surrounding set, and it is simple that the present invention also has structure, device is light small and exquisite, easy to loading and unloading, convenient operation and control, cost of manufacture is low, the advantage such as time saving and energy saving.
Accompanying drawing explanation
Fig. 1 is structural representation of the present invention;
Fig. 2 is the plan structure schematic diagram of invention;
Fig. 3 is the structural representation of lid door of the present invention;
Fig. 4 be lid door of the present invention look up structural representation.
In figure: 1-drum, 2-bung, 3-cavity, 4-outer wall, 5-inwall, 6-water inlet, 7-water delivering orifice, blind taper hole two, the 10-sprue gate of the blind taper hole of 8-one, 9-, 11-platform.
Embodiment
Below in conjunction with accompanying drawing and specific embodiment, invention is described further.
Embodiment 1: a kind of diameter is less than the method for making sample of 3mm metal material transmission electron microscope, comprises the following steps:
(1) sample is filled: metal material diameter of section being less than 3mm is vertically placed on the drum of sample preparation device and the middle part of bung;
(2) potting syrup processed: low-melting-point metal Sn is put into graphite crucible and be heated to more than 232 DEG C by batch-type furnace and make it melt;
(3) by step (2) molten metal Sn solution casting in the drum in step (1), be covered with around metal material, after the metal Sn around metal material is solidified, it is taken out from sample preparation device, obtain the metal material sample that diameter of section is greater than 3mm;
(4) the technologic material sample wire cutting machine in step (3) is cut out the thick thin slice of 1mm;
(5) thin slice in step (4) is mechanical grinding to below 100um;
(6) the thin slice piercer after polishing is gone out the sequin that diameter is 3mm, during punching, guarantee that initial metal material is centrally located at piercer punch-center;
(7) sequin just after punching loads in the fixture of the two spray instrument of electrolysis, and it is thinning to carry out twin-jet electropolishing, namely obtains the sample for TEM (transmission electron microscope) analysis.
Preferably, before sample preparation, at the inner side of above-mentioned sample preparation device drum coating releasing material, thus prevent together with metal Sn solution is set in sample preparation device, conveniently stripped.
Preferably, blind taper hole one and the blind taper hole two of formed objects fixing metal material is respectively equipped with in the drum bottom centre of sample preparation device and bung medial center, metal material two ends are inserted in two blind taper holes respectively, two blind taper hole vertical directions keep coaxial, guarantee that cross section is fixed on the center of sample preparation device drum at the metal material being less than 3mm, thus make the thickness of the metal Sn of metal material sample surrounding set even.
Preferably, at the barrel of above-mentioned sample preparation device drum, the cavity passing into chilled water is set, in described step (3), pass into the metal Sn of chilled water to cast carry out cooled and solidified, when molten metal Sn solution pours into around metal material, the temperature of metal Sn solution in drum reduces by the chilled water of cavity immediately makes it solidify, thus avoid the too high microstructure to metal material of molten metal Sn solution temperature to have an impact, accelerate the speed that metal Sn solution solidifies simultaneously, shorten experimental period.
Embodiment 2: as shown in Fig. 1 ~ Fig. 4, a kind of diameter is less than the sample preparation device of 3mm metal material transmission electron microscope, comprise drum 1 and bung 2, be provided with the blind taper hole 1 placing sample in described drum 1 in the middle part of bottom side, upper end is provided with bung 2, and described bung 2 middle inside is provided with the blind taper hole 29 placing sample, and be provided with sprue gate 10, its barrel of wall is the cavity 3 of hollow structure, and described cavity 3 comprises outer wall 4 and inwall 5, and described outer wall 4 is provided with the water inlet 6 and water delivering orifice 7 that are communicated with cavity 3.
Preferably, be threaded connection between above-mentioned bung 1 and drum 1, can install fast, convenient to operation.
Preferably, above-mentioned water inlet 6 is arranged on outer wall 4 near top side, described water delivering orifice 7 is arranged on outer wall 4 near bottom side, contrary with water inlet 6 direction, chilled water enters from drum one side bottom, flows out from opposite side top, can be more evenly good to inwall cooling, cooling effect is better, and the sample performance after cast is better.
Preferably, above-mentioned blind taper hole 1 and blind taper hole 29 internal diameter size, from 0.5 ~ 3mm transition, can meet the requirement of the metal material TEM sample preparation being less than 3mm.
Preferably, above-mentioned sprue gate 10 is that bung 2 cylindrical arranges the through hole formed inside two symmetrical platforms 11 and inwall 5, and platform is formed by milling cylindrical, adopts two sprue gates of this structure, can realize fast pouring into a mould, and is convenient to turn bung and loads and unloads.
Above-mentioned, preferred inwall 5 diameter 6mm, high 10mm, wall thickness 3mm, the thick 3mm in bottom, outer diameter 15mm, high 15mm, wall thickness 3mm, bung diameter 10mm, high 3mm.
Embodiment 3: first in sample preparation device drum inwall brush one deck release materials, then the first sample that metal material diameter of section being less than 3mm cuts into 7 ~ 10mm length is vertically fixed on the center of sample preparation device drum and bung, after sample fixes, low-melting-point metal Sn is put into graphite crucible by experiment the batch-type furnace of room join more than 232 DEG C and make it melt, after the metal Sn fusing in crucible, it being taken out from batch-type furnace with crucible tongs is placed on asbestos gauge, break because of Local cooling to prevent crucible, during with the crucible that crucible tongs gripping is scorching hot, must by the sharp first preheating of pincers, then with spoon, the metal Sn solution in crucible is scooped out, from sample preparation device, the sprue gate of bung is by around metal Sn solution casting to metal material, in order to avoid the too high tissue to metal material of molten metal Sn solution temperature has an impact, logical cooling circulating water in built-in bucket wall cavity simultaneously on drum, after being solidified to the surrounding of metal material metal Sn dissolution homogeneity to be melted, it is taken out from sample preparation device, the thick thin slice of 1mm is cut out with wire cutting machine, be mechanical grinding to below 100um, the sequin that diameter is 3mm is gone out with piercer, guarantee during punching that initial metal material is positioned at disk center, then sequin is loaded in the fixture of the two spray instrument of electrolysis, the thinning mode of the two spray of employing obtains the sample for TEM (transmission electron microscope) analysis.
Embodiment 4: sample is the 82B high-carbon steel finer wire after drawing, and diameter 0.5mm, is organized as sorbite, with wire cutting machine, sample is cut to the first sample of length 10mm;
Samples vertical is fixed on the center of experimental provision drum and bung (inwall has brushed release materials);
Low-melting-point metal Sn is put into graphite crucible by experiment the batch-type furnace of room be heated to more than 232 DEG C and make it melt;
Being taken out from batch-type furnace by molten metal Sn solution with crucible tongs is placed on asbestos gauge, simultaneously logical cooling circulating water in outer barrel;
With spoon, the metal Sn solution in crucible is scooped out, from the sprue gate of sample preparation device middle cover door by around metal Sn solution casting to metal material;
It takes out after being solidified to the surrounding of metal material equably by molten metal Sn from sample preparation device;
Cut out the thick thin slice of 1mm with wire cutting machine, be mechanical grinding to below 100um, go out with piercer the sequin that diameter is 3mm, during punching, guarantee that initial metal material is positioned at disk center;
Loaded by sequin in the fixture of the two spray instrument of electrolysis, it is thinning to carry out twin-jet electropolishing;
Namely the sample for TEM (transmission electron microscope) analysis is obtained.
Embodiment 5:
Sample is the 82B high-carbon steel finer wire after drawing, and diameter 2.9mm, is organized as sorbite, with wire cutting machine, sample is cut to the first sample that length is 6mm;
Samples vertical is fixed on the center of bucket in experimental provision (inwall has been brushed and smeared material);
Low-melting-point metal Sn is put into graphite crucible by experiment the batch-type furnace of room be heated to more than 232 DEG C and make it melt;
Being taken out from batch-type furnace by molten metal Sn solution with crucible tongs is placed on asbestos gauge, and experimental provision is led to cooling circulating water;
With spoon, the metal Sn solution in crucible is scooped out, from the sprue gate of sample preparation device middle cover door by around metal Sn solution casting to metal material;
It takes out after being solidified to the surrounding of metal material equably by molten metal Sn from sample preparation device;
Cut out the thick thin slice of 1mm with wire cutting machine, be mechanical grinding to below 100um, go out with piercer the sequin that diameter is 3mm, during punching, guarantee that initial metal material is positioned at disk center;
Loaded by sequin in the fixture of the two spray instrument of electrolysis, it is thinning to carry out twin-jet electropolishing;
Namely the sample for TEM (transmission electron microscope) analysis is obtained.
The above; be only the specific embodiment of the present invention; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; change can be expected easily or replace; all should be encompassed within protection scope of the present invention, therefore, protection scope of the present invention should be as the criterion with the protection domain of described claim.
Claims (9)
1. diameter is less than a method for making sample for 3mm metal material transmission electron microscope, it is characterized in that: comprise the following steps:
(1) sample is filled: metal material diameter of section being less than 3mm is vertically placed on the drum of sample preparation device and the middle part of bung;
(2) potting syrup processed: low-melting-point metal Sn is put into graphite crucible and be heated to more than 232 DEG C by batch-type furnace and make it melt;
(3) step (2) molten metal Sn solution is poured in the drum in step (1) by sprue gate, be covered with around metal material, after the metal Sn around metal material is solidified, it is taken out from sample preparation device, obtain the metal material sample that diameter of section is greater than 3mm;
(4) the technologic material sample wire cutting machine in step (3) is cut out the thick thin slice of 1mm;
(5) thin slice in step (4) is mechanical grinding to below 100um;
(6) the thin slice piercer after polishing is gone out the sequin that diameter is 3mm, during punching, guarantee that initial metal material is centrally located at piercer punch-center;
(7) sequin just after punching loads in the fixture of the two spray instrument of electrolysis, and it is thinning to carry out twin-jet electropolishing, namely obtains the sample for TEM (transmission electron microscope) analysis.
2. a kind of diameter according to claim 1 is less than the method for making sample of 3mm metal material transmission electron microscope, it is characterized in that: before sample preparation, at the inner side of the drum bung of described sample preparation device coating releasing material.
3. a kind of diameter according to claim 1 is less than the method for making sample of 3mm metal material transmission electron microscope, it is characterized in that: the blind taper hole one and the blind taper hole two that are respectively equipped with formed objects fixing metal material in the drum bottom centre of sample preparation device and bung medial center, metal material two ends are inserted in two blind taper holes respectively, and two blind taper hole vertical directions keep coaxial.
4. a kind of diameter according to claim 1 is less than the method for making sample of 3mm metal material transmission electron microscope, it is characterized in that: the cavity passing into chilled water is set at the barrel of described sample preparation device drum, in described step (3), pass into the metal Sn of chilled water to cast carry out cooled and solidified.
5. a diameter is less than the sample preparation device of 3mm metal material transmission electron microscope, it is characterized in that: comprise drum (1) and bung (2), the blind taper hole one (8) placing sample is provided with in the middle part of described drum (1) interior bottom side, upper end is provided with bung (2), described bung (2) middle inside is provided with the blind taper hole two (9) placing sample, and be provided with sprue gate (10), its barrel of wall is the cavity (3) of hollow structure, described cavity (3) comprises outer wall (4) and inwall (5), described outer wall (4) is provided with the water inlet (6) and water delivering orifice (7) that are communicated with cavity (3).
6. a kind of diameter according to claim 5 is less than the sample preparation device of 3mm metal material transmission electron microscope, it is characterized in that: be threaded connection between described bung (1) and drum (1).
7. a kind of diameter according to claim 5 is less than the sample preparation device of 3mm metal material transmission electron microscope, it is characterized in that: described water inlet (6) is arranged on outer wall (4) near top side, described water delivering orifice (7) is arranged on outer wall (4) near bottom side, contrary with water inlet (6) direction.
8. a kind of diameter according to claim 5 is less than the sample preparation device of 3mm metal material transmission electron microscope, it is characterized in that: described blind taper hole one (8) and blind taper hole two (9) internal diameter size are from 0.5 ~ 3mm transition.
9. a kind of diameter according to claim 5 is less than the sample preparation device of 3mm metal material transmission electron microscope, it is characterized in that: described sprue gate (10) arrange the through hole that two symmetrical platforms (11) and inwall (5) inner side formed for bung (2) cylindrical.
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| CN201510859253.9A CN105334095B (en) | 2015-12-01 | 2015-12-01 | A kind of diameter is less than the method for making sample and device of 3mm metal material transmission electron microscopes |
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| CN105699151A (en) * | 2016-04-11 | 2016-06-22 | 贵州大学 | Device and method for preparing static stretching sample of steel wire with section diameter being 2-10mm |
| CN105973659A (en) * | 2016-04-11 | 2016-09-28 | 贵州大学 | Sample preparation method and device of steel wire fatigue testing specimen with cross-sectional diameter of 2-10 mm |
| CN106896014A (en) * | 2017-04-17 | 2017-06-27 | 江西省科学院应用物理研究所 | The preparation method and device of a kind of metal material cross-sectional Transmission tem sample |
| CN107824924A (en) * | 2017-11-27 | 2018-03-23 | 武汉比色光电科技有限公司 | A kind of optical device automatic coupling fixing device |
| 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 |
| CN114608924A (en) * | 2022-02-15 | 2022-06-10 | 北京钢研高纳科技股份有限公司 | Preparation method of transmission electron microscope sample of high-temperature alloy electron beam welding joint |
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| CN106896014A (en) * | 2017-04-17 | 2017-06-27 | 江西省科学院应用物理研究所 | The preparation method and device of a kind of metal material cross-sectional Transmission tem sample |
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| 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 |
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