CN108896339A - The preparation method of metallographic specimen - Google Patents
The preparation method of metallographic specimen Download PDFInfo
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- CN108896339A CN108896339A CN201810293538.4A CN201810293538A CN108896339A CN 108896339 A CN108896339 A CN 108896339A CN 201810293538 A CN201810293538 A CN 201810293538A CN 108896339 A CN108896339 A CN 108896339A
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- metallographic
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- metallographic specimen
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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
- G01N1/02—Devices for withdrawing samples
- G01N1/04—Devices for withdrawing samples in the solid state, e.g. by cutting
- G01N1/06—Devices for withdrawing samples in the solid state, e.g. by cutting providing a thin slice, e.g. microtome
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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
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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
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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
- G01N2001/364—Embedding or analogous mounting of samples using resins, epoxy
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of preparation methods of metallographic specimen, include the following steps：S1, sampling：Sample is cut respectively at the edge of sample and the center of sample；S2, it inlays：Colloid is slowly guided to inlay in mould by galvanized wire and is solidified；S3, polishing；S4, polishing；S5, corrosion：Metallographic detection faces are corroded with corrosive liquid.The present invention can effectively prevent metallographic specimen to generate bubble and shorten polishing time while improving polishing effect, convenient for improving the accuracy of detection to metallographic detection faces metallographic observation.
Description
Technical field
The invention belongs to measuring for materials fields, more particularly to a kind of preparation method of metallographic specimen.
Background technique
Metallographic Analysis is that people study metal and alloy microscopic structure size, form, distribution, number by metallographic microscope
Amount and property a kind of method, with this method come investigate as alloying element, composition transfer and its microscopic structure change pass
System, since research material is different, the preparation method of metallographic specimen be it is diversified, unsuitable operation is likely to form " pseudo- group
Knit " lead to error analysis.Textual details are shown for what can be removed, do not make sample surface layer that any tissue occur in sample making course
Variation, program are commonly divided into several main processes such as sampling, edge sample, polishing, and sample obtained is thrown by this method
It is longer between light time, and there is also metallic particles and polishing scratch for burnishing surface, influence detection faces smoothness, seriously affect the knot of metal lographic examination
Fruit.
A kind of metallographic specimen preparation method disclosed in 103759993 U of Chinese patent publication No. CN, concrete operations include：
Firstly, metallographic specimen samples；Secondly, metallographic specimen is inlayed；Again, metallographic specimen polishes；Again, the polished face of metallographic specimen
Acid etch, flushing：It treats after burnishing surface is put into nital etch and is rinsed with water；Finally, metallographic specimen polishes, although logical
It crosses and increases nital bedroom erosion process before polishing, dissolve the abrasive grain stayed on flour milling and metal filings particle,
Sample after polishing will not leave behind apparent polishing scratch, improve the smoothness on metallographic specimen surface, but sample is inlayed in mosaic process
It is easy to generate bubble, influences to observe clarity, after sample is inlayed, edge sample is difficult to be removed from the molds, and be easy to cause edge sample report
It is useless.
Summary of the invention
The invention mainly solves the technical problem of providing a kind of preparation methods of metallographic specimen, effectively prevent metallographic specimen
It generates bubble and shortens polishing time while improving polishing effect, convenient for observing metallographic detection faces, improve inspection
The accuracy of survey.
In order to solve the above technical problems, one technical scheme adopted by the invention is that：A kind of preparation of metallographic specimen is provided
Method includes the following steps：
S1, sampling：Cut sample respectively at the edge of sample and the center of sample, the direction of cutting will be parallel to examination
The metallographic detection faces of sample do following processing to sample according to the thickness of sample：
(1) when the thickness of sample is less than 30mm, directly using cut surface as metallographic detection faces；
(2) when the thickness of sample is between 30-50mm, it is 2 that the sample of acquirement is truncated at the 2/3 of thickness direction
Sample, and using truncation surface as metallographic detection faces；
(3) when the thickness of sample is greater than 50mm, by the sample of acquirement, 3 equal points of truncations are 3 samples in a thickness direction,
And using truncation surface as metallographic detection faces；
S2, it inlays：Acrylic powder and curing agent are pressed 1.4:1 volume ratio mixing, is made colloid after mixing evenly,
The surface of the sample taken coats one layer of colloid, is then placed in the metallographic detection of sample downwards and inlays in mould, colloid is led to
It crosses galvanized wire and is slowly directed into and inlay in mould, be put into 30-50 DEG C of baking oven, baking 5-8min is solidified so that metallographic examination is made
Sample；
S3, polishing：Whether detection metallographic specimen is fully cured before polishing, then takes out metallographic specimen from inlaying in mould,
Metallographic observation face is roughly ground and refined, sand paper is first installed to grinding and polishing disk, is then gently pressed to sample in grinding and polishing disk
Heart position polishes to metallographic detection faces, and side edging translates metallographic specimen outward, good simultaneously to metallographic specimen and sand paper contact
It when without bounce, can be ground with sample is forced, grinding dynamics is 1.5-2kgf, and every grinding 5-8s metallographic specimen rotates 90 °；
S4, polishing：Flocked fabric is soaked in 5-10min in water and is then mounted to grinding and polishing disk to moisten Flocked fabric completely
After rotate grinding and polishing disk, velocity of rotation 200-300r/min rotates 30s, to get rid of extra moisture content, by polishing agent from mill
It instils at the center dumped, then grinding and polishing disk rotating speed is adjusted to 600-800r/min, it is finally that the metallographic detection faces of metallographic specimen are light
The center of grinding and polishing disk is gently pressed to, side edging translates metallographic specimen outward, well has no to metallographic specimen and Flocked fabric contact
It when bounce, can be ground with sample is forced, grinding dynamics is 0.8-1.2kgf, and every grinding 5-8s metallographic specimen rotates 90 °；
S5, corrosion：Metallographic detection faces are corroded with corrosive liquid, is cleaned after corroding 3-5s with clear water, is then used
Alcohol is observed after being wiped with microscope, according to the suitable corrosive liquid of the material selection of sample, selects mode as follows：
The tissue of low-alloy steel is shown：Nitric acid alcohol；
The tissue of austenitic evanohm is shown：Wang aqueous solution；
Stainless steel, austenite high nickel steel, copper or copper alloy tissue show：Liquor ferri trichloridi；
Ferritic tissue display：Sodium hydroxide；
Thickness of coating, graphite grade, nonmetallic inclusionsin steel tissue show：Corroded without corrosive liquid, directly
It is observed with after alcohol wipe with microscope.
It further says, the mould of inlaying in the S2 step includes the identical mold of two structures and connection buckle, the mould
Tool includes side wall and bottom plate, and the side wall is located at the upper surface of the bottom plate and connect with the bottom plate, one in two molds
The two sides of a mold are respectively provided at least one connection buckle, one end of the connection buckle and mold it is side walls hinged and described
The other end of connection buckle is equipped with the button hole to match with the salient point of another mold so that two mold realizations are detachably connected.
It further says, the cross section of the sample cut in the S1 step is round or square.
It further says, the side length of the circular diameter and the square is all 15mm.
It further says, the curing agent includes the raw material of following parts by weight：Trimethylolpropane diacrylate rouge 30-40
Part and 20-25 parts of laruyl alcohol acrylate.
It further says, the mesh number of sand paper selected by the corase grinding is 400-600 mesh, sand paper selected by the fine grinding
Mesh number be 1000-1200 mesh.
It further says, in S3, the revolving speed of grinding and polishing disk is 200-300r/min when corase grinding, the revolving speed of grinding and polishing disk when fine grinding
For 400-500r/min.
It further says, the polishing agent is alumina powder polishing agent, magnesium oxide powder polishing agent, chromium oxide polishing powder end
Photo etching or diamond dust polishing agent, the granularity of powder is 5-10 mesh in the polishing agent.
It further says, polishing and polish selected polishing machine is MP-2B type polisher lapper.
The beneficial effects of the invention are as follows：
The present invention is handled sample by sampling, inlaying, polishing, polishing and corroding, through the invention distinctive edge
Embedding method effectively prevent metallographic specimen to generate bubble, is observed conducive to microscope, then by polishing and polishing, tries metallographic
The viewing surface of sample is polished, and while improving polishing effect, shortens polishing time, is finally detected with corrosive liquid to metallographic
Face is corroded, and the abrasive grain remained in metallographic detection faces and metal removal particle are dissolved, convenient for observation；
In sampling procedure of the invention, sample is cut respectively at the edge of sample and the center of sample, according to sample
The difference of thickness is handled, to guarantee the accuracy of Metallographic Analysis, it is worth mentioning at this point that, cutting is oriented parallel to try
The metallographic detection faces of sample carry out processing convenient for the later period, shorten milling time to guarantee the flatness of metallographic detection faces；
Of the invention inlays in step, coats one layer of colloid on the surface of the sample taken, in glue and sample contacts,
It effectively prevent specimen surface to generate bubble, influences observing effect, more preferably, colloid is slowly guided to edge by galvanized wire
In embedding mould, metallographic specimen is effectively prevent to generate bubble；
The center that sample of the invention gently presses to grinding and polishing disk polishes to metallographic detection faces, and side edging is put down outward
Move metallographic specimen prevents metallographic specimen from damaging to prevent metallographic specimen from slipping from hand, guarantees the safety of operator, often
It grinds 5-8s metallographic specimen and rotates 90 °, guarantee the flatness of metallographic viewing surface, increase the service life of sand paper or Flocked fabric, drop
Low grinding cost；
The present invention is polished by Flocked fabric, to improve the polishing effect of metallographic specimen, keeps its surface more smooth, benefit
In being observed under the microscope；
The present invention corrodes metallographic detection faces according to the suitable corrosive liquid of material selection of sample, dissolves and remains in
Abrasive grain and metal removal particle in metallographic detection faces improve detection accuracy convenient for observing metallographic detection faces；
It includes two molds being detachably connected that the present invention, which inlays the mould of inlaying in step, and two molds pass through connection buckle reality
It now connects, consequently facilitating metallographic specimen is taken out from inlaying in mould, prevents damage metallographic specimen.
Detailed description of the invention
Fig. 1 is structural schematic diagram of the invention；
The appended drawing reference of each section is as follows in figure：
Side wall 1, salient point 11, bottom plate 2, connection buckle 3 and button hole 31.
Specific embodiment
The preferred embodiments of the present invention will be described in detail below so that advantages and features of the invention can be easier to by
It will be appreciated by those skilled in the art that so as to make a clearer definition of the protection scope of the present invention.
Embodiment：A kind of preparation method of metallographic specimen, as shown in Figure 1, including the following steps：
S1, sampling：Cut sample respectively at the edge of sample and the center of sample, the direction of cutting will be parallel to examination
The metallographic detection faces of sample do following processing to sample according to the thickness of sample：
(1) when the thickness of sample is less than 30mm, directly using cut surface as metallographic detection faces；
(2) when the thickness of sample is between 30-50mm, it is 2 that the sample of acquirement is truncated at the 2/3 of thickness direction
Sample, and using truncation surface as metallographic detection faces；
(3) when the thickness of sample is greater than 50mm, by the sample of acquirement, 3 equal points of truncations are 3 samples in a thickness direction,
And using truncation surface as metallographic detection faces；
S2, it inlays：Acrylic powder and curing agent are pressed 1.4:1 volume ratio mixing, is made colloid after mixing evenly,
The surface of the sample taken coats one layer of colloid, is then placed in the metallographic detection of sample downwards and inlays in mould, colloid is led to
It crosses galvanized wire and is slowly directed into and inlay in mould, be put into 30-50 DEG C of baking oven, baking 5-8min is solidified so that metallographic examination is made
Sample；
S3, polishing：Whether detection metallographic specimen is fully cured before polishing, then takes out metallographic specimen from inlaying in mould,
Metallographic observation face is roughly ground and refined, sand paper is first installed to grinding and polishing disk, is then gently pressed to sample in grinding and polishing disk
Heart position polishes to metallographic detection faces, and side edging translates metallographic specimen outward, good simultaneously to metallographic specimen and sand paper contact
It when without bounce, can be ground with sample is forced, grinding dynamics is 1.5-2kgf, and every grinding 5-8s metallographic specimen rotates 90 °；
S4, polishing：Flocked fabric is soaked in 5-10min in water and is then mounted to grinding and polishing disk to moisten Flocked fabric completely
After rotate grinding and polishing disk, velocity of rotation 200-300r/min rotates 30s, to get rid of extra moisture content, by polishing agent from mill
It instils at the center dumped, then grinding and polishing disk rotating speed is adjusted to 600-800r/min, it is finally that the metallographic detection faces of metallographic specimen are light
The center of grinding and polishing disk is gently pressed to, side edging translates metallographic specimen outward, well has no to metallographic specimen and Flocked fabric contact
It when bounce, can be ground with sample is forced, grinding dynamics is 0.8-1.2kgf, and every grinding 5-8s metallographic specimen rotates 90 °；
S5, corrosion：Metallographic detection faces are corroded with corrosive liquid, is cleaned after corroding 3-5s with clear water, is then used
Alcohol is observed after being wiped with microscope, according to the suitable corrosive liquid of the material selection of sample, selects mode as follows：
The tissue of low-alloy steel is shown：Nitric acid alcohol；
The tissue of austenitic evanohm is shown：Wang aqueous solution；
Stainless steel, austenite high nickel steel, copper or copper alloy tissue show：Liquor ferri trichloridi；
Ferritic tissue display：Sodium hydroxide；
Thickness of coating, graphite grade, nonmetallic inclusionsin steel tissue show：Corroded without corrosive liquid, directly
It is observed with after alcohol wipe with microscope.
Mould of inlaying in the S2 step includes the identical mold of two structures and connection buckle 3, and the mold includes side wall 1
With bottom plate 2, the side wall 1 is located at the upper surface of the bottom plate 2 and connect with the bottom plate 2, described in one in two molds
The two sides of mold are respectively provided at least one connection buckle 3, and one end of the connection buckle 3 and the side wall 1 of mold are hinged, and the connection
The other end of button 3 is equipped with the button hole 31 to match with the salient point 11 of another mold so that two mold realizations detachably connect
It connects.
The cross section of the sample cut in the S1 step is round or square.
The side length of the circular diameter and the square is all 15mm.
The curing agent includes the raw material of following parts by weight：30-40 parts of trimethylolpropane diacrylate rouge and laruyl alcohol
20-25 parts of acrylate.
The mesh number of sand paper selected by the corase grinding is 400-600 mesh, and the mesh number of sand paper selected by the fine grinding is
1000-1200 mesh.
In S3, the revolving speed of grinding and polishing disk is 200-300r/min when corase grinding, and the revolving speed of grinding and polishing disk is 400-500r/ when fine grinding
min。
The polishing agent is alumina powder polishing agent, magnesium oxide powder polishing agent, chromium oxide polishing powder end photo etching or Buddha's warrior attendant
Stone powder polishing agent, the granularity of powder is 5-10 mesh in the polishing agent.
Polishing machine selected by polishing and polishing is MP-2B type polisher lapper.
Working principle of the present invention is as follows：The present invention pass through by sample, inlay, polish, polish and corrode to sample into
Row processing, distinctive method for embedding, effectively prevent metallographic specimen to generate bubble, is observed conducive to microscope through the invention,
Again by polishing and polishing, the viewing surface of metallographic specimen is polished, while improving polishing effect, when shortening polishing
Between, finally metallographic detection faces are corroded with corrosive liquid, dissolve the abrasive grain and metal remained in metallographic detection faces
It is ground particle, convenient for observation, improves detection accuracy.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure transformation made by bright specification is applied directly or indirectly in other relevant technical fields, and is similarly included in
In scope of patent protection of the invention.
Claims (9)
1. a kind of preparation method of metallographic specimen, it is characterised in that：Include the following steps：
S1, sampling：Cut sample respectively at the edge of sample and the center of sample, the direction of cutting will be parallel to sample
Metallographic detection faces do following processing to sample according to the thickness of sample：
(1) when the thickness of sample is less than 30mm, directly using cut surface as metallographic detection faces；
(2) when the thickness of sample is between 30-50mm, the sample of acquirement is truncated at the 2/3 of thickness direction for 2 examinations
Sample, and using truncation surface as metallographic detection faces；
(3) when the thickness of sample is greater than 50mm, by the sample of acquirement, 3 equal points of truncations are 3 samples in a thickness direction, and will
Truncation surface is as metallographic detection faces；
S2, it inlays：Acrylic powder and curing agent are pressed 1.4:1 volume ratio mixing, colloid is made after mixing evenly, is taking
The surface of sample coat one layer of colloid, the detection of the metallographic of sample is placed in downwards then and is inlayed in mould, colloid is passed through into plating
Zinc-iron silk, which is slowly directed into, to be inlayed in mould, and 30-50 DEG C of baking oven is put into, and baking 5-8min is solidified so that metallographic specimen is made；
S3, polishing：Whether detection metallographic specimen is fully cured before polishing, then takes out metallographic specimen from inlaying in mould, to gold
Phase viewing surface is roughly ground and is refined, and sand paper is first installed to grinding and polishing disk, then sample is gently pressed to the centre bit of grinding and polishing disk
It sets and polishes metallographic detection faces, side edging translates metallographic specimen outward, well has no jump to metallographic specimen and sand paper contact
It when dynamic, can be ground with sample is forced, grinding dynamics is 1.5-2kgf, and every grinding 5-8s metallographic specimen rotates 90 °；
S4, polishing：Flocked fabric is soaked in 5-10min in water to be made after being then mounted to grinding and polishing disk with moistening Flocked fabric completely
The rotation of grinding and polishing disk, velocity of rotation 200-300r/min rotate 30s, to get rid of extra moisture content, by polishing agent from grinding and polishing disk
Center at instil, then grinding and polishing disk rotating speed is adjusted to 600-800r/min, finally gently presses the metallographic detection faces of metallographic specimen
To the center of grinding and polishing disk, side edging translates metallographic specimen outward, well has no bounce to metallographic specimen and Flocked fabric contact
When, it can be ground with sample is forced, grinding dynamics is 0.8-1.2kgf, and every grinding 5-8s metallographic specimen rotates 90 °；
S5, corrosion：Metallographic detection faces are corroded with corrosive liquid, is cleaned after corroding 3-5s with clear water, then uses alcohol
It is observed after being wiped with microscope, according to the suitable corrosive liquid of the material selection of sample, selects mode as follows：
The tissue of low-alloy steel is shown：Nitric acid alcohol；
The tissue of austenitic evanohm is shown：Wang aqueous solution；
Stainless steel, austenite high nickel steel, copper or copper alloy tissue show：Liquor ferri trichloridi；
Ferritic tissue display：Sodium hydroxide；
Thickness of coating, graphite grade, nonmetallic inclusionsin steel tissue show：Corroded without corrosive liquid, directly uses wine
It is observed after essence wiping with microscope.
2. the preparation method of metallographic specimen according to claim 1, it is characterised in that：Mould packet is inlayed in the S2 step
The identical mold of two structures and connection buckle are included, the mold includes side wall (1) and bottom plate (2), and the side wall is located at the bottom
It the upper surface of plate and is connect with the bottom plate, the two sides of a mold in two molds are respectively provided at least one connection buckle
(3), one end of the connection buckle and mold is side walls hinged, and the other end of the connection buckle is equipped with the salient point with another mold
(11) button hole (31) to match is so that two mold realizations are detachably connected.
3. the preparation method of metallographic specimen according to claim 1, it is characterised in that：The sample cut in the S1 step
Cross section be round or square.
4. the preparation method of metallographic specimen according to claim 3, it is characterised in that：The circular diameter and it is described just
Rectangular side length is all 15mm.
5. the preparation method of metallographic specimen according to claim 1, it is characterised in that：The curing agent includes following weight
The raw material of part：30-40 parts and 20-25 parts of laruyl alcohol acrylate of trimethylolpropane diacrylate rouge.
6. the preparation method of metallographic specimen according to claim 1, it is characterised in that：Sand paper selected by the corase grinding
Mesh number is 400-600 mesh, and the mesh number of sand paper selected by the fine grinding is 1000-1200 mesh.
7. the preparation method of metallographic specimen according to claim 1, it is characterised in that：In S3, grinding and polishing disk when corase grinding
Revolving speed is 200-300r/min, and the revolving speed of grinding and polishing disk is 400-500r/min when fine grinding.
8. the preparation method of metallographic specimen according to claim 1, it is characterised in that：The polishing agent is alumina powder
Polishing agent, magnesium oxide powder polishing agent, chromium oxide polishing powder end photo etching or diamond dust polishing agent, powder in the polishing agent
Granularity is 5-10 mesh.
9. the preparation method of metallographic specimen according to claim 1, it is characterised in that：Polishing selected by polishing and polishing
Machine is MP-2B type polisher lapper.
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