CN112881397A - Preparation method of steel sample for high-temperature confocal microscope observation - Google Patents
Preparation method of steel sample for high-temperature confocal microscope observation Download PDFInfo
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- CN112881397A CN112881397A CN202110202128.6A CN202110202128A CN112881397A CN 112881397 A CN112881397 A CN 112881397A CN 202110202128 A CN202110202128 A CN 202110202128A CN 112881397 A CN112881397 A CN 112881397A
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 17
- 239000010959 steel Substances 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 23
- 238000005498 polishing Methods 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000002474 experimental method Methods 0.000 claims abstract description 4
- 238000005464 sample preparation method Methods 0.000 claims abstract description 4
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 3
- 230000006835 compression Effects 0.000 claims description 6
- 238000007906 compression Methods 0.000 claims description 6
- 238000012360 testing method Methods 0.000 description 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 1
- 235000017491 Bambusa tulda Nutrition 0.000 description 1
- 241001330002 Bambuseae Species 0.000 description 1
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 1
- 239000011425 bamboo Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 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
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
-
- 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
-
- 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
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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
- G01N1/36—Embedding or analogous mounting of samples
-
- 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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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The application discloses a preparation method of a steel sample for high-temperature confocal microscope observation, which comprises the following steps: selecting a target sample, polishing the target sample after inlaying the target sample according to a conventional metallographic sample preparation method, and taking out the target sample; placing the polished surface a of the target sample on a first embedding cylinder base in a downward mode, and adding an embedding material to prepare a first embedding block; placing the surface b opposite to the surface a of the first mosaic block on the base of the second mosaic cylinder in a downward mode, and adding a mosaic material to obtain a second mosaic block; polishing the surface b of the second mosaic block until the section of the target sample is completely exposed, and automatically polishing; and taking out the processed target sample in the second mosaic block, cleaning the target sample by an ultrasonic cleaning machine, and then placing the target sample under a high-temperature confocal microscope for experiment. The method is not limited by the parallelism of the original bottom surfaces of the samples, and the samples for observing the high-temperature confocal microscope with the upper and lower parallel bottom surfaces can be prepared only by using conventional sample preparation tools and consumables.
Description
Technical Field
The invention belongs to the technical field of preparation of high-temperature metallographic samples, and particularly relates to a preparation method of a steel sample for high-temperature confocal microscope observation.
Background
At present, for a steel sample for observation of a high-temperature confocal microscope, the upper bottom surface and the lower bottom surface are required to be parallel, so that the surface of the sample can be focused clearly in the process of high-temperature metallographic observation, and the shooting quality of a high-temperature metallographic picture is ensured.
Because the steel sample for observation by the high-temperature confocal microscope is thin, the height is generally less than or equal to 3.5mm, the thin sample is not easy to be ground manually or automatically, the currently adopted method is that after the sample is embedded, one bottom surface of the sample is ground and flattened, the sample is taken out from an embedded block, then the other bottom surface is embedded, ground and polished, and then taken out, the parallelism degree of the bottom surfaces of the sample prepared by the method is seriously dependent on the parallelism degree of the upper bottom surface and the lower bottom surface of the original sample, and the parallelism correcting function is not provided, and if the upper bottom surface and the lower bottom surface of the original sample are not parallel, the sample with the parallel upper bottom surface and the parallel lower bottom surface can not be prepared.
In order to meet the sample requirements of high-temperature metallographic experiments, improve the success rate of preparing thin samples and save the sample preparation cost, a new preparation method of a sample for high-temperature confocal observation needs to be developed.
Disclosure of Invention
The invention aims to provide a preparation method of a steel sample for high-temperature confocal microscope observation, which overcomes the defects in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a steel sample for high-temperature confocal microscope observation comprises the following steps: step (1): selecting a target sample, polishing the target sample after inlaying the target sample according to a conventional metallographic sample preparation method, and taking the sample out of the inlaying block;
step (2): marking the polished surface of the target sample in the step (1) as an a surface, downwards placing the marked a surface on a base of a first embedding cylinder, adding an embedding material to prepare a first embedding block, wherein the bottom surface of the a surface of the target sample is still marked as the a surface, and the other opposite bottom surface is marked as a b surface;
and (3): placing the first mosaic block b in the step (2) on a second mosaic cylinder base in a downward mode, adding a mosaic material to prepare a second mosaic block, wherein the bottom surface of the b surface of the original first mosaic block is marked as a b surface;
and (4): polishing the surface b of the second mosaic block in the step (3) until the section of the target sample is completely exposed, and automatically polishing;
and (5): and (4) taking out the target sample in the second mosaic block processed in the step (4), cleaning the target sample by an ultrasonic cleaning machine, and then placing the target sample under a high-temperature confocal microscope for experiment.
Preferably, in the step (2), the first mosaic block is consistent with the height of the target sample.
Preferably, in the step (2), the addition amount of the embedding material satisfies the following condition:
Vx＝(V2-V1)×I
wherein: vx is the volume of the added quantity of the embedding material; v2 is the volume of the first mosaic, V1 is the volume of the target sample, and I is the mosaic compression ratio.
Preferably, select the mosaic material that the volume is V3, put into first inlay a section of thick bamboo base on, under certain mosaic condition, inlay the mosaic material and obtain the mosaic piece that the volume is V4, the compression ratio of mosaic material satisfies:
preferably, the diameter of the second embedding cylinder base is larger than that of the first embedding cylinder base.
Preferably, in the step (3): the height of the second mosaic block is more than 8 mm.
Compared with the prior art, the invention has at least the following beneficial effects:
the invention provides a method for preparing a sample for observing a high-temperature confocal microscope, which can correct the parallelism of the upper bottom surface and the lower bottom surface of the sample in the sample preparation process and enables the upper bottom surface and the lower bottom surface to be parallel. The method can prepare samples meeting the test requirements only by using common metallographic sample preparation equipment without designing a special clamp. The success rate of sample preparation is improved, and a plurality of samples can be prepared at one time according to experimental requirements.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present application, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a schematic structural diagram of a method for preparing a steel sample for high temperature confocal microscope observation according to an embodiment of the present invention;
description of reference numerals: 1. a sample; 2. a mosaic piece having a diameter of D1; 3. b, surface; 4. a surface; 5. a mosaic of diameter D2.
Detailed Description
The technical solutions in the embodiments of the present invention will be described in detail below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
Referring to fig. 1, a method for preparing a steel sample for high-temperature confocal microscope observation with a diameter of 6mm comprises the following steps:
1. a steel bar with the diameter of phi 6mm is taken, 1 original sample 1 is cut by a metallographic cutter, and the upper bottom surface and the lower bottom surface of the sample are observed to be unparallel and the thickness of the sample is about 3.5 mm.
2. And (3) inlaying and polishing the sample 1 obtained in the step (1) according to a conventional metallographic sample preparation method, taking the sample out of the inlaying block, and enabling the obtained sample 1 to have a flat and smooth bottom surface.
3. Testing the compression ratio of the embedding material, measuring the embedding material with the volume of 12mL, using an embedding cylinder with the diameter phi of 30mm of a hot-pressing embedding machine to embed the embedding material under a certain embedding condition to obtain an embedding block with the volume of 5mL, and calculating to obtain the compression ratio of the embedding material under the condition of 2.4.
4. The volume of the target sample was measured by the drainage method using a measuring cylinder having a minimum division value of 0.1 mL.
5. The maximum height of the measurement target sample is 3.7mm, therefore, the sample needs to be inlaid into an inlaid block 2 with the diameter of phi 30mm and the height of 3.7mm, the volume of the inlaid block is calculated to be 2.6mL, the volume occupied by the compressed inlaid material in the inlaid block is 2.5mL, and the volume of the inlaid material to be added is 6 mL.
Marking the smooth surface of the target sample as a surface 4 a, placing the smooth surface on a base of an embedding cylinder with the diameter of phi 30mm, adding an embedding material with the volume of 6mL, wherein the height of an embedded block 2 obtained after embedding is just 3.7mm of the maximum height of the target sample, embedding the sample by using the compressed embedding resin, and marking the surface, containing the surface a of the original sample, of the embedded block 2 obtained after embedding as a surface 4 a and the other surface opposite to the surface a as a surface 3 b.
And 7, downwards placing the b surface 3 of the mosaic block 2 obtained by mosaic in the step (6) in a mosaic cylinder with the diameter of phi 40mm, and mosaic again to obtain a mosaic block 5 with the diameter of phi 40mm and the height of 15mm, wherein in the obtained mosaic block 5, the bottom surface of the original mosaic block, namely the b surface 3, is still marked as the b surface 3.
And 8, downwards placing the b surface 3 of the mosaic block 5 prepared in the step (7) on an automatic polishing machine for polishing, continuously checking in the polishing process, observing that the exposure area of the target sample is larger and larger until the section of the whole target sample is completely exposed, and then performing subsequent polishing.
And 9, taking the target sample out of the mosaic block 5 ground in the step (8), properly grinding the side edges, and cleaning by using ultrasonic waves, wherein the upper bottom surface and the lower bottom surface of the obtained sample are parallel to meet the requirement of observation in a high-temperature confocal microscope.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The foregoing is merely a detailed description of the present application, and it should be noted that modifications and embellishments could be made by those skilled in the art without departing from the principle of the present application, and these should also be considered as the protection scope of the present application.
Claims (6)
1. A preparation method of a steel sample for high-temperature confocal microscope observation is characterized by comprising the following steps: the method comprises the following steps:
step (1): selecting a target sample, polishing the target sample after inlaying the target sample according to a conventional metallographic sample preparation method, and taking the sample out of the inlaying block;
step (2): marking the polished surface of the target sample in the step (1) as an a surface, downwards placing the marked a surface on a base of a first embedding cylinder, adding an embedding material to prepare a first embedding block, wherein the bottom surface of the a surface of the target sample is still marked as the a surface, and the other opposite bottom surface is marked as a b surface;
and (3): placing the first mosaic block b in the step (2) on a second mosaic cylinder base in a downward mode, adding a mosaic material to prepare a second mosaic block, wherein the bottom surface of the b surface of the original first mosaic block is marked as a b surface;
and (4): polishing the surface b of the second mosaic block in the step (3) until the section of the target sample is completely exposed, and automatically polishing;
and (5): and (4) taking out the target sample in the second mosaic block processed in the step (4), cleaning the target sample by an ultrasonic cleaning machine, and then placing the target sample under a high-temperature confocal microscope for experiment.
2. The method for preparing a steel sample for high temperature confocal microscope observation according to claim 1, wherein the method comprises the following steps: in the step (2), the first mosaic block is consistent with the height of the target sample.
3. The method for preparing a steel sample for high temperature confocal microscope observation according to claim 1, wherein the method comprises the following steps: in the step (2), the addition amount of the embedding material meets the following requirements:
Vx＝(V2-V1)×I
wherein: vxThe volume of the added quantity of the embedding material; v2Is the volume of the first mosaic, V1I is the volume of the target sample and I is the compression ratio of the insert.
4. The method for preparing a steel sample for high temperature confocal microscope observation according to claim 3, wherein the method comprises the following steps: selecting a volume of V3The embedding material is placed on a first embedding cylinder base, and under a certain embedding condition, the embedding material is embedded to obtain a V-shaped volume4The compression ratio of the mosaic material meets the following requirements:
5. the method for preparing a steel sample for high temperature confocal microscope observation according to claim 1, wherein the method comprises the following steps: the diameter of the second embedded cylinder base is larger than that of the first embedded cylinder base.
6. The method for preparing a steel sample for high temperature confocal microscope observation according to claim 1, wherein the method comprises the following steps: in the step (3): the height of the second mosaic block is more than 8 mm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110202128.6A CN112881397B (en) | 2021-02-23 | 2021-02-23 | Preparation method of steel sample for high-temperature confocal microscope observation |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118130191A (en) * | 2024-02-05 | 2024-06-04 | 南昌航空大学 | Preparation method and application of high-temperature laser scanning confocal microscope small-size in-situ observation sample |
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| CN107091830A (en) * | 2017-03-07 | 2017-08-25 | 江苏省沙钢钢铁研究院有限公司 | Method for observing BN precipitation behavior in boron-containing steel |
| CN110632075A (en) * | 2019-10-31 | 2019-12-31 | 安徽工业大学 | Observation assistive device for high-temperature laser confocal microscope sample and using method |
| CN210037366U (en) * | 2019-04-12 | 2020-02-07 | 广东韶钢松山股份有限公司 | High-temperature confocal microscope sample preparation device |
| CN110954382A (en) * | 2019-12-03 | 2020-04-03 | 镇江耐丝新型材料有限公司 | Preparation method of solid-liquid multiphase metallographic sample with superfine steel wire cross section |
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- 2021-02-23 CN CN202110202128.6A patent/CN112881397B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107091830A (en) * | 2017-03-07 | 2017-08-25 | 江苏省沙钢钢铁研究院有限公司 | Method for observing BN precipitation behavior in boron-containing steel |
| CN210037366U (en) * | 2019-04-12 | 2020-02-07 | 广东韶钢松山股份有限公司 | High-temperature confocal microscope sample preparation device |
| CN110632075A (en) * | 2019-10-31 | 2019-12-31 | 安徽工业大学 | Observation assistive device for high-temperature laser confocal microscope sample and using method |
| CN110954382A (en) * | 2019-12-03 | 2020-04-03 | 镇江耐丝新型材料有限公司 | Preparation method of solid-liquid multiphase metallographic sample with superfine steel wire cross section |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN118130191A (en) * | 2024-02-05 | 2024-06-04 | 南昌航空大学 | Preparation method and application of high-temperature laser scanning confocal microscope small-size in-situ observation sample |
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