CN111351694A - Preparation method of metallographic specimen without water seepage and stain edge microstructure - Google Patents
Preparation method of metallographic specimen without water seepage and stain edge microstructure Download PDFInfo
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- CN111351694A CN111351694A CN202010361318.8A CN202010361318A CN111351694A CN 111351694 A CN111351694 A CN 111351694A CN 202010361318 A CN202010361318 A CN 202010361318A CN 111351694 A CN111351694 A CN 111351694A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000005498 polishing Methods 0.000 claims abstract description 42
- 238000000227 grinding Methods 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000004140 cleaning Methods 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 14
- 239000000565 sealant Substances 0.000 claims abstract description 13
- 230000007797 corrosion Effects 0.000 claims abstract description 9
- 238000005260 corrosion Methods 0.000 claims abstract description 9
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 229910003460 diamond Inorganic materials 0.000 claims abstract description 7
- 239000010432 diamond Substances 0.000 claims abstract description 7
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 6
- HQFCOGRKGVGYBB-UHFFFAOYSA-N ethanol;nitric acid Chemical compound CCO.O[N+]([O-])=O HQFCOGRKGVGYBB-UHFFFAOYSA-N 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- VUZPGEIXNYGDJN-UHFFFAOYSA-N 1-nitroethanol Chemical compound CC(O)[N+]([O-])=O VUZPGEIXNYGDJN-UHFFFAOYSA-N 0.000 claims 1
- 239000000956 alloy Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 6
- 238000001514 detection method Methods 0.000 description 4
- 238000001223 reverse osmosis Methods 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000002344 surface layer Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000000861 blow drying Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 239000002085 irritant Substances 0.000 description 1
- 231100000021 irritant Toxicity 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005464 sample preparation method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
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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
- G01N1/32—Polishing; Etching
-
- 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
- G01N1/34—Purifying; Cleaning
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention belongs to the technical field of metallographic specimen treatment, and particularly relates to a preparation method of a metallographic specimen without a water seepage stained edge microstructure. Comprises mechanical grinding and polishing: polishing the sample after hot inlaying until no visible scratches exist on the polished surface; liquid seal interface: uniformly coating the liquid sealant on the interface between the sample to be tested and the embedding material, standing at room temperature for 20-40min to allow the liquid sealant to naturally penetrate and fill, and naturally drying; mechanical polishing: grinding diamond paste or Al2O3Directly extruding polishing paste on a grinding device, dropwise adding clear water on the inner side of the sample to keep the polishing surface moist, and slowly moving the sample along the reverse direction of the rotation of the grinding disc; cleaning, metallographic corrosion and the like. The sample prepared by the invention can eliminate the phenomenon of edge water seepage and stain when the microstructure of the metallographic sample is observed, obviously improves the image definition of the edge microstructure, and has simple and easy operation and stable effect.
Description
Technical Field
The invention belongs to the technical field of metallographic specimen treatment, and particularly relates to a preparation method of a metallographic specimen without a water seepage stained edge microstructure.
Background
The metallographic observation has important significance for the detection and evaluation of the microstructure of the metal material. In metallographic examination, the situation that the microstructure of the surface layer of the material needs to be observed and evaluated is often met. In order to avoid the appearance of edge chamfering caused by directly grinding and polishing the sample, a metallographic embedding method is generally used for observing the metallographic structure of the edge of the surface layer. However, the interface between the edge of the sample and the insert has an irremovable physical gap, and after polishing, corrosion and blow-drying, the residual moisture in the interface gap can seep out of the surface, and particularly, the water seepage phenomenon is more serious for porous materials with loose surfaces. The water seeped out of the surface can cause serious pollution to the appearance of the microstructure at the edge of the sample, and the observation of the metallographic structure at the edge of the surface layer is greatly influenced.
In order to solve the problem, the existing solution is to perform repeated polishing treatment, and to perform corrosion drying by using high-wind-speed hot air, so as to prolong the drying time and shorten the observation and photographing time. In addition, the method can avoid dripping clear water in the mechanical polishing process and replace the clear water with high-volatility ethanol so as to solve the phenomenon of reverse osmosis water fouling. The method greatly consumes manpower and material resources (the using amount of ethanol is large), has unstable effect, can only improve fouling, and is difficult to completely solve and avoid.
Disclosure of Invention
The invention aims to provide a preparation method of a metallographic specimen of an edge microstructure without water seepage and stain, successfully solves the phenomenon of serious stain of the edge microstructure appearance caused by reverse osmosis of residual moisture in a gap of a specimen interface, obviously improves the image definition of the edge microstructure, and has the advantages of simple and easy operation and comprehension and stable effect.
The purpose of the invention can be realized by the following technical scheme:
a preparation method of a metallographic specimen without water seepage and stain edge microstructures comprises the following steps,
(1) mechanical grinding and polishing: polishing the sample after hot inlaying until no visible scratches exist on the polished surface;
preferably, the sample is used 400 times after hot-setting#、800#、1000#、1500#、2500#And (4) polishing the silicon carbide metallographic abrasive paper in different passes.
(2) And a liquid seal interface:
uniformly coating the liquid sealant on the interface between the sample to be tested and the embedding material, standing at room temperature for 20-40min to allow the liquid sealant to naturally penetrate and fill, and naturally drying;
preferably, the liquid sealant comprises the following components in parts by weight:
the invention adds the process step of liquid seal interface to process the sample to be tested, observes the microstructure of the sample to be tested through a metallographic microscope and measures the quality of the edge image, and can find that the interface has no water seepage and stain, the microstructure image is clean and clear, and the detection and evaluation accuracy of the subsequent microstructure of the metal material is obviously improved. The method can be effectively applied to the metallographic observation and detection of the microstructure of the metal surface layer, such as surface coating, physical interface gap, intergranular oxide layer and the like.
Further preferably, the liquid sealant comprises the following components in percentage by weight,
the solution obtained in the formula has the advantages of optimal liquid sealing effect, short curing time and no defects of shrinkage residual stress, cracking and the like after curing.
Further preferably, the coating amount of the liquid sealing agent needs to completely cover the interface gap, and the transverse diffusion amount is optimally 0.5-2mm on two sides of the interface. Therefore, the coating amount is ensured to be enough to fill the gap after curing and shrinking, and meanwhile, the difficulty of subsequent mechanical polishing caused by excessive coating is avoided.
(3) And mechanical polishing:
grinding diamond paste or Al2O3Directly extruding polishing paste on a grinding device, dropwise adding clear water on the inner side of the sample to keep the polishing surface moist, and slowly moving the sample along the reverse direction of the rotation of the grinding disc;
preferably, the grinding paste is diamond grinding paste with the grain size of 2.5 μm; the polishing paste is Al with the grain diameter of less than 1 mu m2O3Polishing paste; the grinding disc rotating speed is 1000 r/min. If the rotating speed is too high, the speed of frictional heat generation is increased, the heat dissipation of the polishing surface is not facilitated, the surface is oxidized and darkened, and scratches of the polishing surface are increased and are difficult to remove due to the fact that the rotating speed is too high. The polishing time is prolonged due to the excessively low rotating speed, and the difficulty of the scratch removing process is increased.
(4) And cleaning:
washing the sample in the step (3) with clear water, then placing the sample in ethanol for cleaning, and drying the sample with cold air;
(5) corrosion of the metallic phase
And (4) placing the sample in the step (4) in a nitric acid ethanol solution for corrosion for 5-8s, quickly cleaning the sample with water after the color of the surface becomes dark, then cleaning with ethanol, and finally quickly drying the surface of the sample with hot air.
Preferably, the volume ratio of nitric acid to ethanol in the nital solution is 4%.
The invention has the beneficial effects that:
1. the invention realizes the permeation filling of the residual interface gap by adopting the liquid sealing agent to carry out liquid sealing on the interface of the sample and the embedding material, successfully solves the phenomenon that the edge microstructure appearance is seriously stained due to the reverse osmosis of the residual moisture in the interface gap, achieves the aim of clearly observing the surface metallographic microstructure, and realizes the simple, convenient, rapid and stable detection of the sample.
2. The liquid sealant adopted by the osmotic filling of the invention is safe, harmless, not easy to volatilize, non-irritant, small in single dosage, and capable of being stored for a long time and used for many times.
3. The method has the advantages of simple and convenient operation, easy control, good effect, simple and easily obtained used equipment, short experimental time, low experimental requirement and simple and convenient experimental steps.
Drawings
FIG. 1 is a topographical view of a surface microstructure of a sample at 100 times magnification, wherein FIG. 1A is a comparative example and FIG. 1B is the invention.
Fig. 2 is a surface microstructure topography of a sample magnified 500 times, where fig. 2A is a comparative example and fig. 2B is the invention.
Detailed Description
The invention will now be further illustrated by reference to the following examples:
example 1:
1) preparation of the liquid sealant:
taking the following raw materials in percentage by weight:
mixing the above materials, and stirring to obtain liquid sealant.
2) Mechanical grinding and polishing: and (3) grinding the cut 18CrNiMo7-6 sample by using 400#, 800#, 1000#, 1500# and 2500# silicon carbide metallographic abrasive paper in different passes in sequence until no visible scratches are formed on the surface.
3) Liquid seal interface: and uniformly coating the prepared liquid sealant on the interface of the sample and the embedding material until the interface is completely covered, ensuring that the solution diffusion quantity on the two sides of the interface is 1mm, standing at room temperature for 30min, naturally permeating and filling the solution, and naturally drying.
4) Mechanical polishing: and (3) selecting diamond grinding paste with the granularity of 2.5 mu m to be smeared on the surface of the polishing cloth, selecting the rotating speed of a polishing machine to be 1000r/min, slowly moving the sample along the reverse direction of the rotation of the grinding disc while polishing, and dropwise adding clear water until a bright mirror-image polishing surface is obtained.
5) Cleaning: and after polishing, quickly washing the surface of the sample by using clear water, then washing by using ethanol, and drying by using cold air.
6) Metallographic corrosion: and placing the dried metallographic sample in a 4% nitric acid ethanol solution in volume ratio to corrode for 5-8s, quickly cleaning the metallographic sample with water after the surface color becomes dark, then cleaning with ethanol, and quickly drying the surface of the metallographic sample with high-speed hot air.
And obtaining the metallographic specimen with no water seepage and stain edge microstructure by using the processed specimen.
Comparative example 1
1) Mechanical grinding and polishing: and (3) grinding the cut 18CrNiMo7-6 sample by using 400#, 800#, 1000#, 1500# and 2500# silicon carbide metallographic abrasive paper in different passes in sequence until no visible scratches are formed on the surface.
2) Mechanical polishing: and (3) selecting diamond grinding paste with the granularity of 2.5 mu m to be smeared on the surface of the polishing cloth, selecting the rotating speed of a polishing machine to be 1000r/min, slowly moving the sample along the reverse direction of the rotation of the grinding disc while polishing, and dropwise adding clear water until a bright mirror-image polishing surface is obtained.
3) Cleaning: and after polishing, quickly washing the surface of the sample by using clear water, then washing by using ethanol, and drying by using cold air.
4) Metallographic corrosion: and placing the dried metallographic sample in a 4% nitric acid ethanol solution in volume ratio to corrode for 5-8s, quickly cleaning the metallographic sample with water after the surface color becomes dark, then cleaning with ethanol, and quickly drying the surface of the metallographic sample with high-speed hot air.
The microstructure of the sample to be measured is observed through a metallographic microscope, and the depth of the edge water seepage and fouling area is measured, and the result is shown in the following table:
the comparison of the data shows that the metallographic sample preparation method designed by the invention can effectively avoid the water reverse osmosis phenomenon of the edge interface during the observation of the microstructure, thereby obviously improving the image definition of the edge microstructure, and having simple and easy operation and stable effect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention, and the present invention should not be limited by the disclosure of the preferred embodiments. Therefore, it is intended that all equivalents and modifications which do not depart from the spirit of the invention disclosed herein are deemed to be within the scope of the invention.
Claims (6)
1. A preparation method of a metallographic specimen without water seepage and stain edge microstructures comprises the following steps,
(1) mechanical grinding and polishing: polishing the sample after hot inlaying until no visible scratches exist on the polished surface;
(2) and a liquid seal interface:
uniformly coating the liquid sealant on the interface between the sample to be tested and the embedding material, standing at room temperature for 20-40min to allow the liquid sealant to naturally penetrate and fill, and naturally drying;
(3) and mechanical polishing:
grinding diamond paste or Al2O3Directly extruding polishing paste on a grinding device, dropwise adding clear water on the inner side of the sample to keep the polishing surface moist, and slowly moving the sample along the reverse direction of the rotation of the grinding disc;
(4) and cleaning:
washing the sample in the step (3) with clear water, then placing the sample in ethanol for cleaning, and drying the sample with cold air;
(5) corrosion of the metallic phase
And (4) placing the sample in the step (4) in a nitric acid ethanol solution for corrosion for 5-8s, quickly cleaning the sample with water after the color of the surface becomes dark, then cleaning with ethanol, and finally quickly drying the surface of the sample with hot air.
2. The method of claim 1, wherein: in the step (1), the samples are sequentially used for 400 after being hot-inlaid#、800#、1000#、1500#、2500#And (4) polishing the silicon carbide metallographic abrasive paper in different passes.
3. The method of claim 1, wherein: the liquid sealant in the step (2) comprises the following components in parts by weight:
4. the method of claim 1, wherein: the grinding paste in the step (3) is diamond grinding paste with the granularity of 2.5 mu m; the polishing paste is Al with the grain diameter of less than 1 mu m2O3And (7) polishing paste.
5. The method for preparing the alloy material according to claim 1, wherein the grinding disc rotating speed of the step (3) is 1000 r/min.
6. The method according to claim 1, wherein the volume ratio of nitric acid to ethanol in the nitroethanol solution in the step (5) is 4%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113155564A (en) * | 2021-04-15 | 2021-07-23 | 唐山钢铁集团有限责任公司 | Analysis method for inclusions causing sand hole defects of stamping parts |
| CN115184112A (en) * | 2022-07-13 | 2022-10-14 | 国标（北京）检验认证有限公司 | Preparation method of osmium target material microstructure sample |
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