CN112747992A - Metallographic structure display method of Mg-containing 440C corrosion-resistant stainless bearing steel based on three-step method - Google Patents
Metallographic structure display method of Mg-containing 440C corrosion-resistant stainless bearing steel based on three-step method Download PDFInfo
- Publication number
- CN112747992A CN112747992A CN202011630643.6A CN202011630643A CN112747992A CN 112747992 A CN112747992 A CN 112747992A CN 202011630643 A CN202011630643 A CN 202011630643A CN 112747992 A CN112747992 A CN 112747992A
- Authority
- CN
- China
- Prior art keywords
- sample
- corrosion
- polishing
- metallographic
- bearing steel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000005260 corrosion Methods 0.000 title claims abstract description 87
- 230000007797 corrosion Effects 0.000 title claims abstract description 87
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 37
- 239000010959 steel Substances 0.000 title claims abstract description 37
- 229910001213 440C Inorganic materials 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000005498 polishing Methods 0.000 claims abstract description 58
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 4
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 238000000227 grinding Methods 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 238000005530 etching Methods 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 22
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 20
- 229910017604 nitric acid Inorganic materials 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000003518 caustics Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 11
- 239000004744 fabric Substances 0.000 claims description 10
- 229940057950 sodium laureth sulfate Drugs 0.000 claims description 10
- SXHLENDCVBIJFO-UHFFFAOYSA-M sodium;2-[2-(2-dodecoxyethoxy)ethoxy]ethyl sulfate Chemical compound [Na+].CCCCCCCCCCCCOCCOCCOCCOS([O-])(=O)=O SXHLENDCVBIJFO-UHFFFAOYSA-M 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 9
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 8
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims description 8
- 229940045803 cuprous chloride Drugs 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000000861 blow drying Methods 0.000 claims description 5
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000006386 neutralization reaction Methods 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims description 2
- 229920001778 nylon Polymers 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229910003460 diamond Inorganic materials 0.000 claims 1
- 239000010432 diamond Substances 0.000 claims 1
- 238000003780 insertion Methods 0.000 claims 1
- 230000037431 insertion Effects 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 11
- 238000011156 evaluation Methods 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 description 16
- 238000010586 diagram Methods 0.000 description 10
- 239000013078 crystal Substances 0.000 description 8
- 239000000835 fiber Substances 0.000 description 4
- 230000009286 beneficial effect Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- SNIOPGDIGTZGOP-UHFFFAOYSA-N Nitroglycerin Chemical compound [O-][N+](=O)OCC(O[N+]([O-])=O)CO[N+]([O-])=O SNIOPGDIGTZGOP-UHFFFAOYSA-N 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 229910001105 martensitic stainless steel Inorganic materials 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229940073020 nitrol Drugs 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000003381 solubilizing effect Effects 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
Images
Classifications
-
- 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
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Investigating And Analyzing Materials By Characteristic Methods (AREA)
- Sampling And Sample Adjustment (AREA)
- ing And Chemical Polishing (AREA)
Abstract
The invention discloses a metallographic structure display method of Mg-containing 440C corrosion-resistant stainless bearing steel based on a three-step method, which comprises the steps of corroding a polished sample by using a self-made corrosive liquid, neutralizing by using a hot alkali solution, slightly polishing, corroding again, removing corrosion products on the surface of the sample, and gradually deepening grain boundary marks to obtain a clear metallographic structure of the Mg-containing 440C corrosion-resistant stainless bearing steel. The grain boundary of the metallographic specimen obtained by the method is clearly displayed, and the problem of grain size grade evaluation in the 440C corrosion-resistant stainless bearing steel containing Mg is solved.
Description
Technical Field
The invention belongs to the field of metallographic sample preparation, and relates to a metallographic structure display method of Mg-containing 440C corrosion-resistant stainless bearing steel.
Background
The 440C steel is martensite stainless steel, has the carbon content of 1.0 percent and the chromium content of 16 to 18 percent, has stronger anti-rust capability and is high-quality stainless steel. The method is mainly used for manufacturing bearing parts working in a corrosive environment and a non-lubricating strong oxidizing atmosphere. 440C has better high-temperature dimensional stability, so the steel can also be used as corrosion-resistant high-temperature bearing steel. In addition, the method can be used for manufacturing high-quality cutters such as medical scalpels, scissors and the like. And a certain amount of Mg element is added into the 440C corrosion-resistant stainless bearing steel to play a role in refining the structure and improving the comprehensive performance of the 440C corrosion-resistant stainless bearing steel.
Because the 440C corrosion-resistant stainless bearing steel has extremely high contents of chromium and carbon, the corrosion resistance of the steel is very strong, and a large amount of carbide is attached to the surface of a sample, the corrosion is carried out according to a conventional method, and the clear structure appearance displayed by a grain boundary is difficult to obtain. Since the grain boundaries cannot be clearly shown, it is difficult to evaluate the grain size grade of the sample, which poses a certain obstacle to the subsequent research on the 440C corrosion-resistant stainless bearing steel.
The existing metallographic display method for martensitic stainless steel is generally a nital reagent, but after the test, the metallographic surface of a sample is over-corroded locally after the nital reagent is corroded, most areas have no obvious change, and a grain boundary cannot be displayed.
Therefore, the present invention is directed to a metallographic structure display method suitable for 440C corrosion-resistant stainless bearing steel containing Mg.
Disclosure of Invention
The invention aims to provide a metallographic structure display method suitable for Mg-containing 440C corrosion-resistant stainless bearing steel, so that the grain boundary of the matrix structure of the Mg-containing 440C corrosion-resistant stainless bearing steel is comprehensively and clearly displayed, and the problem of grain size grade evaluation is solved.
In order to achieve the above object, the present invention provides a metallographic structure display method applicable to 440C corrosion-resistant stainless bearing steel containing Mg, the method comprising the steps of: a. sample inlaying: and (5) carrying out sample inlaying by using inlaying powder. b. Grinding a sample: polishing the sample by using water abrasive paper until the direction of the surface grinding mark of the sample is consistent; c. primary polishing: polishing the ground sample; d. primary corrosion: and putting the polished sample in a corrosive agent for etching for 30-90 seconds, after no obvious bubbles are generated on the surface of the sample, washing the sample with a large amount of clear water, then washing with absolute ethyl alcohol, and drying the surface by using a blower. At this time, the surface of the sample was observed under a metallographic microscope to develop blue color. e. And (3) neutralizing the sample by using 8% potassium hydroxide aqueous solution (50-60 ℃), wherein the treatment time is 1-5 min, and the treatment time is subject to that the sample surface shows light blue to nearly white when observed under a metallographic microscope. f. And (3) secondary polishing: and (3) lightly polishing the neutralized sample on polishing cloth by using water, so that the first corrosion product which is not completely neutralized is thoroughly polished, and the surface of the sample is white and has slight grain boundary traces when observed under a metallographic microscope. g. Secondary corrosion: and corroding the sample subjected to the secondary corrosion in the corrosive agent for 5-30 seconds, washing the sample with a large amount of clear water, then washing with absolute ethyl alcohol, and blow-drying the surface of the sample by using a blower to observe the sample.
According to a preferred embodiment of the present invention, the sample grinding step is to grind the samples sequentially from coarse to fine through 180, 240, 400, 600, 800, 1000, 1200, 1500 and 2000 mesh water grinding sandpaper after the samples are mounted by a sample mounting machine.
According to another preferred embodiment of the present invention, the metallographic display method of Mg-containing 440C corrosion-resistant stainless bearing steel according to claim 1, wherein polishing is performed using a nylon cloth and polishing pastes of particles W3.5, W2.5 and W1.5 in this order, and the sample is rotated by 90 ° for every 30 seconds of polishing until no significant wear marks are observed by naked eyes, and then lightly polished with water to remove the adhering polishing paste.
According to another preferable scheme of the invention, the corrosive agent comprises cuprous chloride, ferric trichloride, distilled water, absolute ethyl alcohol, hydrochloric acid, nitric acid and sodium laureth sulfate, and the mass percentages of the components are as follows: cuprous chloride: 0.5% -0.8%, ferric chloride: 2.0% -2.5%, nitric acid: 2.1% -2.3%, absolute ethyl alcohol: 24% -26%, hydrochloric acid: 36-38%, sodium laureth sulfate: 2 to 3 percent of water and the balance of distilled water. Wherein, the content of the nitric acid is strictly controlled between 2.1 percent and 2.3 percent, and the corrosion degree of the sample is accurately controlled. The amphoteric surfactant sodium laureth sulfate is particularly added into the corrosive disclosed by the invention, and the sodium laureth sulfate can be dissolved in water and ethanol, has a solubilizing property, is beneficial to dissolving a corrosion product in a corrosive liquid, reduces the corrosion product attached to the surface of a sample, and enables the reaction to be deeper. And the ferric trichloride and the copper chloride act together to accelerate the corrosion of the sample and change the color of the surface of the sample, thereby being beneficial to controlling the corrosion process.
The invention has the beneficial effects that: by adopting the corrosion liquid and the corrosion method, the grain boundary of the Mg-containing 440C corrosion-resistant stainless bearing steel can be comprehensively and clearly displayed, and the problem of grain size grade evaluation in the Mg-containing 440C corrosion-resistant stainless bearing steel is solved.
Drawings
FIG. 1 is a schematic view showing the etching of the test piece in example 1 for 10 seconds by using a nital etchant, from which it can be seen that individual etching points appear on the test piece and no crystal grains appear.
FIG. 2 is a schematic diagram of the sample etched with the nital etchant for 30s in example 1, from which it can be seen that individual etch spots appear on the sample, and no significant change or crystal grains appear from FIG. 1.
FIG. 3 is a schematic diagram of the sample etched by the nital etchant for 60s in example 1, from which it can be seen that individual etch spots appear on the sample, and no significant change or crystal grains appear from FIG. 2.
FIG. 4 is a schematic view showing the 180s etching of the sample in example 1 with a nital etchant, from which it can be seen that individual etch spots appear on the sample, and no significant change or crystal grains appear from FIG. 3.
FIG. 5 is a schematic view showing the etching of the test piece in example 1 for 300 seconds using a nital etchant, from which it can be seen that a small number of etching sites but no crystal grains were present in the test piece.
FIG. 6 is a schematic view showing the etching of the test piece in example 1 with a nital etchant for 600s, from which it can be seen that the test piece shows more etching points but no crystal grains.
FIG. 7 is a schematic view showing the case where the sample of example 1 was etched with a nital etchant for 1800s, from which it was seen that a large number of corrosion sites were present but no crystal grains were present.
FIG. 8 is a schematic view of the example 1 in which the sample was etched 3600s by using a nital etchant, and it can be seen that a large number of etch spots appear on the sample, and the change is not obvious and no crystal grains appear as compared with FIG. 7.
FIG. 9 is a schematic view showing the corrosion of the sample in example 2 by the self-made corrosive liquid of the present invention for 10s, from which it can be seen that the sample is slightly corroded.
FIG. 10 is a schematic view showing the etching of the sample in example 2 by the self-made etching solution of the present invention for 20 seconds, from which it can be seen that the etching of the sample is further advanced.
FIG. 11 is a schematic view showing the etching of the sample in example 2 for 30s using the self-made etching solution of the present invention, from which it can be seen that the etching of the sample continues to progress.
FIG. 12 is a schematic view of the corrosion of the sample in example 2 by the self-made corrosive liquid of the present invention for 40s, from which it can be seen that the degree of corrosion of the sample is further increased and the surface of the sample begins to appear blue.
FIG. 13 is a schematic diagram of the corrosion of the sample in example 2 by the self-made corrosive liquid of the present invention for 50s, from which it can be seen that the degree of corrosion of the sample continues to increase, the surface of the sample exhibits a deep blue color, and a portion of grain boundaries appear.
FIG. 14 is a schematic view of the sample of example 2 after being etched for 50s in the self-made etchant of the present invention, and the trace of the grain boundary is shallow as can be seen.
FIG. 15 is a schematic view of the sample of example 2 after being lightly polished and then etched in the home-made etchant of the present invention for 10 seconds, wherein the grain boundaries are clearly seen.
FIG. 16 is a schematic diagram showing the corrosion of the sample for 10s in example 3, after the nitric acid content of the self-made corrosion solution is changed, and it can be seen that the sample is slightly corroded.
FIG. 17 is a schematic diagram showing the corrosion of the sample for 20s in example 3, after the nitric acid content in the self-made etching solution was changed, and it can be seen that the degree of corrosion of the sample was increased.
FIG. 18 is a schematic diagram showing the corrosion of the sample for 30s in example 3, after the nitric acid content in the self-made etching solution was changed, and it can be seen that the degree of corrosion of the sample was further increased.
FIG. 19 is a schematic diagram of sample corrosion for 40s in example 3 after changing the content of nitric acid in the self-made corrosion solution, and it can be seen from the diagram that the degree of sample corrosion continues to increase, and the test surface appears blue overall, but no grain boundary trace exists.
FIG. 20 is a schematic diagram of sample corrosion for 50s in example 3 after changing the content of nitric acid in the self-made corrosion solution, and it can be seen from the diagram that the corrosion degree of the sample continuously increases, the test surface appears black overall, the corrosion is excessive, but no grain boundary trace appears.
Detailed Description
Hereinafter, the Mg-containing 440C corrosion-resistant stainless bearing steel metallographic structure display method of the present invention will be described with reference to the exemplary embodiments.
The method for displaying the metallographic structure of the 440C corrosion-resistant stainless bearing steel containing Mg according to the exemplary embodiment of the present invention comprises the steps of:
a. sample inlaying: and (5) carrying out sample inlaying by using inlaying powder.
b. Grinding a sample: before preparing a metallographic sample, the sample needs to be ground to reduce the surface roughness of the sample, so that preparation is made for subsequent polishing work. The 440C corrosion-resistant stainless bearing steel sample is directly ground, so that fingers are easily scratched. Therefore, the sample is inlaid by using the inlaying machine before the sample is polished, the working efficiency is improved, and the test safety is ensured. In the invention, samples are respectively ground by 180, 240, 400, 600, 800, 1000, 1200, 1500 and 2000-mesh water grinding sandpaper from coarse to fine in sequence, grinding scratches on the samples into one direction four times on each piece of sandpaper, and the grinding directions are separated by 90 degrees.
c. Primary polishing: a sample polished by 2000-mesh sandpaper is sequentially polished by polishing pastes of W3.5, W2.5 and W1.5. At the time of polishing, the sample was rotated 90 degrees in the polishing direction every 30 seconds, and the fine grinding marks and the surface deformation layer left on the sample surface by the fine grinding were removed, so that the surface was a mirror surface having no grinding marks. And washing the surface of the polished sample by using a large amount of clear water, removing the attached polishing paste and polishing cloth fibers, and drying the surface of the sample by using absolute ethyl alcohol and a blower.
d. Primary corrosion: preparing an etching solution before etching, then placing the polished sample in the etching agent for etching for 30-90 seconds, after no obvious bubbles are generated on the surface of the sample, washing the sample with a large amount of clear water, then washing with absolute ethyl alcohol, and drying the surface by using a blower. At this time, the surface of the sample was observed under a metallographic microscope to be blue, and the metallographic structure was not sufficiently apparent because the surface of the sample was covered with a large amount of corrosion products and carbides.
e. And (3) neutralization treatment: and (2) neutralizing the sample by using 8% potassium hydroxide aqueous solution (50-60 ℃), wherein the treatment time is 1-5 min, the treatment time is subject to the condition that the sample is observed under a metallographic microscope, the surface of the sample shows light blue to nearly white, only part of corrosion products or primary corrosion liquid is neutralized, and the neutralization reaction is not stopped when the sample is observed to show white, so that the following secondary corrosion is influenced because the sample is easy to generate alkali corrosion locally.
f. And (3) secondary polishing: the neutralized sample was lightly polished on a polishing cloth using water as a lubricant without using a polishing paste. The pressure applied during polishing is as small as possible, and the polishing cloth is slightly rubbed. When the discoloration caused by the corrosion on the surface of the sample disappears through frequent observation, the first corrosion product is completely removed, and the surface of the sample is white and has slight grain boundary traces through observation under a metallographic microscope. The purpose of the secondary polishing is to remove the corrosion products covering the surface of the sample, exposing the masked internal tissue.
g. Secondary corrosion: since the corrosion product prevents the reaction from proceeding during the first etching, part of the grain boundary is not corroded, or the corrosion mark is shallow, the second etching is needed after the second polishing. And corroding the sample subjected to secondary polishing in a corrosive agent for 5-30 seconds, washing the sample with a large amount of clear water, then washing with absolute ethyl alcohol, and blow-drying the surface by using a blower to observe the sample.
And (4) observing the metallographic structure of the sample under a metallographic microscope after the steps are finished.
In order to make the technical solutions of the present invention better understood and implemented by those skilled in the art, the present invention is further described below with reference to specific examples 1, 2 and 3, which are not intended to limit the present invention. Specific target compositions of the Mg-containing 440C corrosion resistant stainless bearing steel in this experiment are shown in table 1.
Table 1 experimental steel composition/wt. -%)
Example 1
The selected test sample is a Mg-containing 440C corrosion-resistant stainless bearing steel tempered test sample
The display of the metallographic structure is carried out according to the following steps:
a. and (3) embedding the metallographic sample by using embedding powder at 140 ℃.
b. The samples are respectively ground by 180, 240, 400, 600, 800, 1000, 1200, 1500 and 2000-mesh water grinding sandpaper from coarse to fine, grinding the grinding marks on the samples into one direction four times on each piece of sandpaper, and the grinding directions are separated by 90 degrees.
c. A sample polished by 2000-mesh sandpaper is sequentially polished by polishing pastes of W3.5, W2.5 and W1.5. At the time of polishing, the sample was rotated 90 degrees in the polishing direction every 30 seconds, and the fine grinding marks and the surface deformation layer left on the sample surface by the fine grinding were removed, so that the surface was a mirror surface having no grinding marks. And washing the surface of the polished sample by using a large amount of clear water, removing the attached polishing paste and polishing cloth fibers, and drying the surface of the sample by using absolute ethyl alcohol and a blower.
d. Preparing 4% nitric acid alcohol corrosive liquid, putting the polished sample in 4% nitric acid alcohol to etch for 10s, 30s, 60s, 180s, 300s, 600s, 1800s and 3600s respectively, washing the sample with a large amount of clear water after reaching a preset time, then washing with absolute alcohol, and drying the surface by using a blower. And observing the surfaces of the samples with different corrosion times under a metallographic microscope.
Example 2
The selected test sample is a Mg-containing 440C corrosion-resistant stainless bearing steel tempered test sample
The display of the metallographic structure is carried out according to the following steps:
a. and (3) embedding the metallographic sample by using embedding powder at 140 ℃.
b. Grinding samples by using 180, 240, 400, 600, 800, 1000, 1200, 1500 and 2000-mesh water-grinding abrasive paper in sequence from coarse to fine, grinding marks on the samples into one direction four times on each piece of abrasive paper, and spacing the grinding directions at 90 DEG each time
c. A sample polished by 2000-mesh sandpaper is sequentially polished by polishing pastes of W3.5, W2.5 and W1.5. At the time of polishing, the sample was rotated 90 degrees in the polishing direction every 30 seconds, and the fine grinding marks and the surface deformation layer left on the sample surface by the fine grinding were removed, so that the surface was a mirror surface having no grinding marks. And washing the surface of the polished sample by using a large amount of clear water, removing the attached polishing paste and polishing cloth fibers, and drying the surface of the sample by using absolute ethyl alcohol and a blower.
d. Preparing a self-made corrosive agent which comprises cuprous chloride, ferric trichloride, distilled water, absolute ethyl alcohol, hydrochloric acid, nitric acid and sodium laureth sulfate, wherein the mass percentages of the components are as follows: cuprous chloride: 0.6%, ferric chloride: 2.2%, nitric acid: 2.2%, absolute ethyl alcohol: 25% and hydrochloric acid: 37%, sodium laureth sulfate: 2.5 percent and the balance of distilled water. And corroding the sample subjected to secondary polishing in a self-made corrosive agent for 5-30 seconds, washing the sample with a large amount of clear water, then washing with absolute ethyl alcohol, and blow-drying the surface of the sample by using a blower to observe the sample.
Example 3
The selected test sample is a Mg-containing 440C corrosion-resistant stainless bearing steel tempered test sample
The display of the metallographic structure is carried out according to the following steps:
a. and (3) embedding the metallographic sample by using embedding powder at 140 ℃.
b. The samples are respectively ground by 180, 240, 400, 600, 800, 1000, 1200, 1500 and 2000-mesh water grinding sandpaper from coarse to fine, grinding the grinding marks on the samples into one direction four times on each piece of sandpaper, and the grinding directions are separated by 90 degrees.
c. A sample polished by 2000-mesh sandpaper is sequentially polished by polishing pastes of W3.5, W2.5 and W1.5. At the time of polishing, the sample was rotated 90 degrees in the polishing direction every 30 seconds, and the fine grinding marks and the surface deformation layer left on the sample surface by the fine grinding were removed, so that the surface was a mirror surface having no grinding marks. And washing the surface of the polished sample by using a large amount of clear water, removing the attached polishing paste and polishing cloth fibers, and drying the surface of the sample by using absolute ethyl alcohol and a blower.
d. Preparing a self-made corrosive agent which comprises cuprous chloride, ferric trichloride, distilled water, absolute ethyl alcohol, hydrochloric acid, nitric acid and sodium laureth sulfate, wherein in the example, the content of nitric acid in the corrosive liquid is changed, the content of nitric acid is increased to 2.5%, and the mass percentages of the components are as follows: cuprous chloride: 0.6%, ferric chloride: 2.2%, nitric acid: 2.5%, absolute ethyl alcohol: 25% and hydrochloric acid: 37%, sodium laureth sulfate: 2.5 percent and the balance of distilled water. And corroding the sample subjected to secondary polishing in a self-made corrosive agent for 5-30 seconds, washing the sample with a large amount of clear water, then washing with absolute ethyl alcohol, and blow-drying the surface of the sample by using a blower to observe the sample.
FIGS. 1-8 are metallographic photographs of samples in a tempered condition obtained according to example one of the present invention. As can be seen from FIGS. 1 to 8, the conventional nitrol etching solution cannot show the metallographic structure of the Mg-containing 440C corrosion-resistant stainless bearing steel.
FIGS. 9-15 are metallographic photographs of samples in a tempered condition obtained according to example two of the present invention. As can be seen from FIGS. 9 to 15, the self-prepared corrosive liquid can corrode a clear metallographic structure of the Mg-containing 440C corrosion-resistant stainless bearing steel by matching with the corrosion method of the invention.
FIGS. 16 to 20 are metallographic photographs of samples in a tempered state obtained according to the third embodiment of the present invention, and it can be seen from FIGS. 16 to 20 that the metallographic structure of the Mg-containing 440C corrosion-resistant stainless bearing steel cannot be corroded when nitric acid in the self-made corrosive liquid exceeds a specified range.
In conclusion, the metallographic specimen grain boundary obtained by the method for displaying the metallographic structure of the Mg-containing 440C corrosion-resistant stainless bearing steel has clear display, the method is simple and easy to implement, and the metallographic structure has high definition.
While the present invention has been described above in connection with exemplary embodiments, it will be apparent to those of ordinary skill in the art that various modifications may be made to the above-described embodiments without departing from the spirit and scope of the claims.
Claims (8)
1. A metallographic display method of 440C corrosion-resistant stainless bearing steel containing Mg is characterized by adopting a three-step metallographic display method of 'primary polishing, primary corrosion + alkali solution neutralization treatment + secondary polishing and secondary corrosion', and the method comprises the following steps:
a. sample inlaying: inlaying samples by using inlaying powder;
b. grinding a sample: polishing the sample by using water abrasive paper until the scratch direction of the surface of the sample is consistent;
c. primary polishing: polishing the ground sample;
d. primary corrosion: and (3) putting the polished sample in a self-made corrosive agent for etching for 30-90 seconds, after no obvious bubbles are generated on the surface of the sample, washing the sample with a large amount of clear water, then washing with absolute ethyl alcohol, and drying the surface by using a blower. At this time, the surface of the sample was observed under a metallographic microscope to develop blue color.
e. And (3) neutralizing the sample by using 8% potassium hydroxide aqueous solution (50-60 ℃), wherein the treatment time is 1-5 min, and the treatment time is subject to that the sample surface shows light blue to nearly white when observed under a metallographic microscope.
f. And (3) secondary polishing: and (3) lightly polishing the primary corrosion sample on polishing cloth by using water to remove the primary corrosion product, wherein the surface of the sample is white and has slight grain boundary traces when observed under a metallographic microscope.
g. Secondary corrosion: and corroding the sample subjected to secondary polishing in a self-made corrosive agent for 5-30 seconds, washing the sample with a large amount of clear water, then washing with absolute alcohol, and blow-drying the surface by using a blower to observe the sample.
2. The metallographic display method for 440C corrosion-resistant stainless bearing steel containing Mg according to claim 1, wherein the corrosive agent in the invention comprises cuprous chloride, ferric trichloride, distilled water, absolute ethyl alcohol, hydrochloric acid, nitric acid, sodium laureth sulfate, and comprises the following components in percentage by mass:
cuprous chloride: 0.5 to 0.8 percent;
ferric chloride: 2.1% -2.3%;
nitric acid: 2.1% -2.3%;
anhydrous ethanol: 24% -26%;
hydrochloric acid: 36 to 38 percent;
sodium laureth sulfate: 2% -3%;
the balance of distilled water.
Wherein the content of the nitric acid is strictly controlled between 2.1 percent and 2.3 percent.
3. The method of claim 1, wherein the sample setting machine is a tripod XQ-2B sample setting machine, the sample setting temperature is 140 ℃, the input voltage is 220V and the input power is 800W.
4. The method of claim 1, wherein the mosaic powder is black metallurgical mosaic powder up to the HD-010 gauge.
5. The method for metallographic representation of Mg-containing 440C corrosion resistant stainless bearing steel according to claim 1, wherein said sandpaper is rhinocery brand water resistant sandpaper.
6. The method of claim 1, wherein the polishing paste is ZZSM KDN diamond grinding paste.
7. The method for displaying the metallographic phase of 440C corrosion-resistant stainless bearing steel containing Mg according to claim 1, wherein said grinding step comprises the steps of inserting the sample into a sample insertion machine, and grinding the sample with 180, 240, 400, 600, 800, 1000, 1200, 1500, 2000 mesh water abrasive paper in the order from coarse to fine.
8. The method for displaying the metallographic phase of 440C corrosion-resistant stainless bearing steel containing Mg according to claim 1, wherein polishing is performed using a nylon cloth, and polishing pastes of particles W3.5, W2.5, and W1.5 in this order, and the sample is rotated by 90 ° every 30 seconds during polishing, and after polishing is continued until no significant scratches are observed by the naked eye, the sample is lightly polished with water to remove the attached polishing paste.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011630643.6A CN112747992B (en) | 2020-12-31 | 2020-12-31 | Metallographic structure display method of Mg-containing 440C corrosion-resistant stainless bearing steel based on three-step method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011630643.6A CN112747992B (en) | 2020-12-31 | 2020-12-31 | Metallographic structure display method of Mg-containing 440C corrosion-resistant stainless bearing steel based on three-step method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112747992A true CN112747992A (en) | 2021-05-04 |
| CN112747992B CN112747992B (en) | 2024-03-15 |
Family
ID=75650766
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011630643.6A Active CN112747992B (en) | 2020-12-31 | 2020-12-31 | Metallographic structure display method of Mg-containing 440C corrosion-resistant stainless bearing steel based on three-step method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112747992B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113670691A (en) * | 2021-08-18 | 2021-11-19 | 广东韶钢松山股份有限公司 | Ultra-low carbon cold heading steel ferrite grain boundary display method |
| CN113758783A (en) * | 2021-08-11 | 2021-12-07 | 重庆材料研究院有限公司 | Method for displaying metallographic structure of platinum |
| CN116577170A (en) * | 2023-05-18 | 2023-08-11 | 陕西长羽航空装备股份有限公司 | Metallographic structure corrosion method of MoNiCr alloy for aeroengine part test and application thereof |
| CN117890187A (en) * | 2024-03-14 | 2024-04-16 | 东北大学 | Step-by-step corrosion method for cast structure of vanadium-containing bearing steel |
Citations (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003050196A (en) * | 2001-08-06 | 2003-02-21 | Mitsubishi Heavy Ind Ltd | Method for evaluating grain boundary corrosion sensitivity |
| US20040214159A1 (en) * | 2003-04-23 | 2004-10-28 | Tadamasa Fujimura | Carrier of a diamond fine particle for immobilizing virus |
| JP2005283252A (en) * | 2004-03-29 | 2005-10-13 | Nippon Steel & Sumikin Stainless Steel Corp | Method for simply analyzing component of metal material, and composition for simply analyzing component of metallic material |
| US20070298992A1 (en) * | 2006-06-21 | 2007-12-27 | Hida Hasinovic | Wheel and tire cleaner composition |
| CN101588715A (en) * | 2006-10-12 | 2009-11-25 | Nm技术纳米材料微型装置技术有限公司 | The material, article and the product that comprise composition with anti-microbial properties |
| US20100285573A1 (en) * | 2006-11-24 | 2010-11-11 | Kwong Joo Leck | Apparatus for processing a sample in a liquid droplet and method of using the same |
| JP2015178656A (en) * | 2014-03-19 | 2015-10-08 | 株式会社フジクラ | Copper etchant and method of producing circuit wiring board using the same |
| CN105823671A (en) * | 2016-06-12 | 2016-08-03 | 东北大学 | Display method of austenitic grain boundary of medium-manganese steel for automobile |
| JP2016216816A (en) * | 2015-05-22 | 2016-12-22 | 株式会社神戸製鋼所 | Two-phase stainless steel material, two-phase stainless steel pipe and surface treatment method for two-phase stainless steel material |
| JP2017004659A (en) * | 2015-06-05 | 2017-01-05 | Jnc株式会社 | Surface observation structure, surface evaluation method, base material manufacturing method, manufacturing method for electronic element, and manufacturing method for touch panel |
| CN106596217A (en) * | 2016-11-16 | 2017-04-26 | 河钢股份有限公司 | Metallographic corrosive agent of high nitrogen stainless steel and metallographic structure display method |
| CN106596235A (en) * | 2016-12-07 | 2017-04-26 | 东北大学 | Dendritic crystal corroding agent for high nitrogen austenitic stainless steel and preparation method thereof |
| US20170190921A1 (en) * | 2016-01-06 | 2017-07-06 | King Fahd University Of Petroleum And Minerals | Corrosion resistant coating composition of ni and a phosphate corrosion inhibitor and an electrodeposition method for the manufacture thereof |
| CN107502126A (en) * | 2017-08-30 | 2017-12-22 | 安徽省含山县潮林铸管厂（普通合伙） | A kind of surface treatment method of sewage water inspection well lid |
| CN108707959A (en) * | 2018-04-08 | 2018-10-26 | 湖北大学 | A kind of neutral environmentally friendly electrochemistry rust remover and technique for applying |
| CN108760419A (en) * | 2018-04-09 | 2018-11-06 | 东北大学 | A kind of cold acid corrosion reagent and its preparation and application of high nitrogen Retaining Ring Steel |
| CN108774597A (en) * | 2018-07-31 | 2018-11-09 | 广东利尔化学有限公司 | A kind of wiring board acidic cleaner and preparation method thereof |
| CN108896339A (en) * | 2018-04-04 | 2018-11-27 | 江苏科泰检测技术服务有限公司 | The preparation method of metallographic specimen |
| CN108893772A (en) * | 2018-05-14 | 2018-11-27 | 西安理工大学 | It is a kind of for showing the corrosive agent and caustic solution of almag metallographic structure |
| CN109055937A (en) * | 2018-07-03 | 2018-12-21 | 杭州电子科技大学 | A kind of chemical etching method obtaining high-transmission rate aluminium alloy |
| CN110553891A (en) * | 2018-05-30 | 2019-12-10 | 大族激光科技产业集团股份有限公司 | Macroscopic metallographic corrosive liquid and metallographic corrosive method for stainless steel aluminum alloy connecting layer |
| CN110819999A (en) * | 2019-11-15 | 2020-02-21 | 河北工业大学 | Alkaline cleaning solution for removing particles on surface of copper wafer to inhibit galvanic corrosion |
-
2020
- 2020-12-31 CN CN202011630643.6A patent/CN112747992B/en active Active
Patent Citations (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003050196A (en) * | 2001-08-06 | 2003-02-21 | Mitsubishi Heavy Ind Ltd | Method for evaluating grain boundary corrosion sensitivity |
| US20040214159A1 (en) * | 2003-04-23 | 2004-10-28 | Tadamasa Fujimura | Carrier of a diamond fine particle for immobilizing virus |
| JP2005283252A (en) * | 2004-03-29 | 2005-10-13 | Nippon Steel & Sumikin Stainless Steel Corp | Method for simply analyzing component of metal material, and composition for simply analyzing component of metallic material |
| US20070298992A1 (en) * | 2006-06-21 | 2007-12-27 | Hida Hasinovic | Wheel and tire cleaner composition |
| CN101588715A (en) * | 2006-10-12 | 2009-11-25 | Nm技术纳米材料微型装置技术有限公司 | The material, article and the product that comprise composition with anti-microbial properties |
| US20100285573A1 (en) * | 2006-11-24 | 2010-11-11 | Kwong Joo Leck | Apparatus for processing a sample in a liquid droplet and method of using the same |
| JP2015178656A (en) * | 2014-03-19 | 2015-10-08 | 株式会社フジクラ | Copper etchant and method of producing circuit wiring board using the same |
| JP2016216816A (en) * | 2015-05-22 | 2016-12-22 | 株式会社神戸製鋼所 | Two-phase stainless steel material, two-phase stainless steel pipe and surface treatment method for two-phase stainless steel material |
| JP2017004659A (en) * | 2015-06-05 | 2017-01-05 | Jnc株式会社 | Surface observation structure, surface evaluation method, base material manufacturing method, manufacturing method for electronic element, and manufacturing method for touch panel |
| US20170190921A1 (en) * | 2016-01-06 | 2017-07-06 | King Fahd University Of Petroleum And Minerals | Corrosion resistant coating composition of ni and a phosphate corrosion inhibitor and an electrodeposition method for the manufacture thereof |
| CN105823671A (en) * | 2016-06-12 | 2016-08-03 | 东北大学 | Display method of austenitic grain boundary of medium-manganese steel for automobile |
| CN106596217A (en) * | 2016-11-16 | 2017-04-26 | 河钢股份有限公司 | Metallographic corrosive agent of high nitrogen stainless steel and metallographic structure display method |
| CN106596235A (en) * | 2016-12-07 | 2017-04-26 | 东北大学 | Dendritic crystal corroding agent for high nitrogen austenitic stainless steel and preparation method thereof |
| CN107502126A (en) * | 2017-08-30 | 2017-12-22 | 安徽省含山县潮林铸管厂（普通合伙） | A kind of surface treatment method of sewage water inspection well lid |
| CN108896339A (en) * | 2018-04-04 | 2018-11-27 | 江苏科泰检测技术服务有限公司 | The preparation method of metallographic specimen |
| CN108707959A (en) * | 2018-04-08 | 2018-10-26 | 湖北大学 | A kind of neutral environmentally friendly electrochemistry rust remover and technique for applying |
| CN108760419A (en) * | 2018-04-09 | 2018-11-06 | 东北大学 | A kind of cold acid corrosion reagent and its preparation and application of high nitrogen Retaining Ring Steel |
| CN108893772A (en) * | 2018-05-14 | 2018-11-27 | 西安理工大学 | It is a kind of for showing the corrosive agent and caustic solution of almag metallographic structure |
| CN110553891A (en) * | 2018-05-30 | 2019-12-10 | 大族激光科技产业集团股份有限公司 | Macroscopic metallographic corrosive liquid and metallographic corrosive method for stainless steel aluminum alloy connecting layer |
| CN109055937A (en) * | 2018-07-03 | 2018-12-21 | 杭州电子科技大学 | A kind of chemical etching method obtaining high-transmission rate aluminium alloy |
| CN108774597A (en) * | 2018-07-31 | 2018-11-09 | 广东利尔化学有限公司 | A kind of wiring board acidic cleaner and preparation method thereof |
| CN110819999A (en) * | 2019-11-15 | 2020-02-21 | 河北工业大学 | Alkaline cleaning solution for removing particles on surface of copper wafer to inhibit galvanic corrosion |
Non-Patent Citations (2)
| Title |
|---|
| 李国平: "2205双相不锈钢TIG焊接头组织及力学性能", 《材料研究学报》, vol. 30, no. 12, pages 897 - 902 * |
| 王琦: "加压条件下镁对轴承钢440C组织及耐蚀性影响研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》, no. 05, 15 May 2022 (2022-05-15), pages 96 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113758783A (en) * | 2021-08-11 | 2021-12-07 | 重庆材料研究院有限公司 | Method for displaying metallographic structure of platinum |
| CN113670691A (en) * | 2021-08-18 | 2021-11-19 | 广东韶钢松山股份有限公司 | Ultra-low carbon cold heading steel ferrite grain boundary display method |
| CN113670691B (en) * | 2021-08-18 | 2024-09-03 | 广东韶钢松山股份有限公司 | Ultralow-carbon cold forging steel ferrite grain boundary display method |
| CN116577170A (en) * | 2023-05-18 | 2023-08-11 | 陕西长羽航空装备股份有限公司 | Metallographic structure corrosion method of MoNiCr alloy for aeroengine part test and application thereof |
| CN116577170B (en) * | 2023-05-18 | 2024-03-01 | 陕西长羽航空装备股份有限公司 | Metallographic structure corrosion method of MoNiCr alloy for aeroengine part test and application thereof |
| CN117890187A (en) * | 2024-03-14 | 2024-04-16 | 东北大学 | Step-by-step corrosion method for cast structure of vanadium-containing bearing steel |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112747992B (en) | 2024-03-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112747992A (en) | Metallographic structure display method of Mg-containing 440C corrosion-resistant stainless bearing steel based on three-step method | |
| CN105092437B (en) | Ultra supercritical martensite heat resisting cast steel original austenite grains degree display methods | |
| CN107014661A (en) | A kind of caustic solution for showing high nitrogen martensitic stain less steel original austenite crystal boundary | |
| CN104805440B (en) | The corrosive agent and display methods of superstrength alloy structural steel original austenite crystal boundary | |
| CN104458511A (en) | Method for testing autstenitic grain size of steel bainite structure for nuclear pressure vessel | |
| CN103792128A (en) | Method for displaying two-phase grain boundary of duplex stainless steel | |
| CN112857950A (en) | Metallographic corrosive agent for biphase medium manganese steel and metallographic structure display method | |
| JP2012529043A (en) | Center segregation evaluation method for continuously cast slabs. | |
| CN109238813A (en) | The detection display methods of spring steel austenite grain | |
| WO2021135226A1 (en) | Method for displaying austenite grains of spring steel | |
| CN110823667B (en) | Metallographic corrosive agent for high-strength titanium alloy and preparation method of metallographic sample of high-strength titanium alloy | |
| CN103411814A (en) | Method for fast displaying original austenite grains of maraging steel containing Cr | |
| CN102419275A (en) | Method for observing metallographic structure of molybdenum-niobium alloy | |
| CN111811912A (en) | Metallographic corrosion method for high-carbon martensitic stainless steel grain boundary | |
| CN110389129A (en) | Corrosive agent for displaying 690 nickel-based alloy deposited metal grain boundary and etching method thereof | |
| CN110926912A (en) | Preparation and erosion method of etchant for displaying grain boundary of low-carbon super martensitic stainless steel | |
| JP6082625B2 (en) | Stainless steel strip manufacturing method | |
| CN110749718A (en) | Dendritic crystal corrosive agent and corrosion method for maraging stainless steel | |
| CN106840821B (en) | Etching liquid for identifying bearing ring forge piece and identification method | |
| CN111424279A (en) | Corrosive and corrosion method for displaying metallographic structure of cobalt-chromium-molybdenum alloy | |
| CN109518186A (en) | A kind of α, β two-phase brass metallographic etching agent and its display methods of metallographic structure | |
| CN105699137B (en) | The structure display methods of crome metal | |
| CN106568634A (en) | Acid etching testing method of macrostructure and defect of steels | |
| CN107976443B (en) | Method for observing pure magnesium metallographic structure | |
| JP2004325190A (en) | Method of making austenitic grain boundary of steel emerged |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |