CN112747992B - 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
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- CN112747992B CN112747992B CN202011630643.6A CN202011630643A CN112747992B CN 112747992 B CN112747992 B CN 112747992B CN 202011630643 A CN202011630643 A CN 202011630643A CN 112747992 B CN112747992 B CN 112747992B
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- 238000005260 corrosion Methods 0.000 title claims abstract description 84
- 230000007797 corrosion Effects 0.000 title claims abstract description 84
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 39
- 239000010959 steel Substances 0.000 title claims abstract description 39
- 229910001213 440C Inorganic materials 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000005498 polishing Methods 0.000 claims abstract description 62
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 230000003472 neutralizing effect Effects 0.000 claims abstract 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 238000000227 grinding Methods 0.000 claims description 29
- 238000005530 etching Methods 0.000 claims description 23
- 238000005406 washing Methods 0.000 claims description 20
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 17
- 229910017604 nitric acid Inorganic materials 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 9
- 239000004744 fabric Substances 0.000 claims description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 9
- 229940057950 sodium laureth sulfate Drugs 0.000 claims description 9
- 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 9
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims description 8
- 239000003518 caustics Substances 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
- 239000000843 powder Substances 0.000 claims description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 7
- 238000006386 neutralization reaction Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 240000007817 Olea europaea Species 0.000 claims 1
- 238000005299 abrasion Methods 0.000 claims 1
- 229910003460 diamond Inorganic materials 0.000 claims 1
- 239000010432 diamond Substances 0.000 claims 1
- 239000007788 liquid Substances 0.000 abstract description 17
- 238000010586 diagram Methods 0.000 description 15
- 235000019441 ethanol Nutrition 0.000 description 14
- 229910002651 NO3 Inorganic materials 0.000 description 13
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 13
- 238000012360 testing method Methods 0.000 description 8
- 244000137852 Petrea volubilis Species 0.000 description 6
- 239000013078 crystal Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 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
- 230000009286 beneficial effect Effects 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
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- SFNALCNOMXIBKG-UHFFFAOYSA-N ethylene glycol monododecyl ether Chemical compound CCCCCCCCCCCCOCCO SFNALCNOMXIBKG-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 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
- 238000004519 manufacturing process Methods 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
- 229920001778 nylon Polymers 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
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
Abstract
The invention discloses a metallographic structure display method of 440C corrosion-resistant stainless bearing steel containing Mg based on a three-step method, which comprises the steps of corroding a polished sample by self-made corrosive liquid, neutralizing by hot alkali solution, lightly polishing, corroding again, removing corrosion products on the surface of the sample, and gradually deepening grain boundary traces to obtain a clear metallographic structure of the 440C corrosion-resistant stainless bearing steel containing Mg. The metallographic specimen obtained according to the invention has clear grain boundary display, and solves the problem of grain size grade assessment in the 440C corrosion-resistant stainless bearing steel containing Mg.
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 a martensite stainless steel, the carbon content is 1.0%, the chromium content is 16% -18%, the rust resistance is strong, and the stainless steel is high-quality stainless steel. The method is mainly used for manufacturing the bearing parts working in a corrosive environment and a lubrication-free strong oxidizing atmosphere. 440C has better high-temperature dimensional stability, so can also be used as corrosion-resistant high-temperature bearing steel. In addition, it can be used to make high quality cutters, such as medical scalpels, scissors, etc. And a certain amount of Mg element is added into 440C corrosion-resistant stainless bearing steel to refine the structure and improve the comprehensive performance of 440C corrosion-resistant stainless bearing steel.
Because 440C corrosion-resistant stainless bearing steel has extremely high chromium and carbon content, the steel has very strong corrosion resistance, and a large amount of carbide is adhered to the surface of a sample, the steel is corroded according to a conventional method, and the grain boundary is difficult to obtain and shows clear tissue morphology. Since grain boundaries are not clearly visible, it is difficult to evaluate grain size grades of the samples, which poses a certain impediment to subsequent studies of 440C corrosion resistant stainless bearing steels.
The existing metallographic display method for martensitic stainless steel is generally nitrate alcohol reagent, but after the test, the metallographic surface of the sample is corroded by the nitrate alcohol reagent, so that the local corrosion is excessive, most areas have no obvious change, and the grain boundary cannot be displayed.
Accordingly, the present invention is directed to a metallographic structure display method suitable for Mg-containing 440C corrosion resistant stainless bearing steel.
Disclosure of Invention
The invention aims to provide a metallographic structure display method applicable to Mg-containing 440C corrosion-resistant stainless bearing steel, so as to comprehensively and clearly display crystal boundaries of a matrix structure of the Mg-containing 440C corrosion-resistant stainless bearing steel and solve the problem of grain size grade assessment.
In order to achieve the above object, the present invention provides a metallographic structure display method applicable to Mg-containing 440C corrosion-resistant stainless bearing steel, the method comprising the steps of: a. and (3) mounting: and (5) embedding the patterns by using embedding powder. b. Grinding: polishing the sample by using water-based abrasive paper until the direction of the polishing mark on the surface of the sample is consistent; c. primary polishing: polishing the polished sample; d. and (3) primary corrosion: and placing the polished sample in a corrosive agent to etch for 30-90 seconds, washing the sample with a large amount of clean water after no obvious bubbles are generated on the surface of the sample, washing the sample 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. e. And (3) carrying out neutralization treatment on the sample by adopting 8% potassium hydroxide aqueous solution (50-60 ℃) for 1-5 min, wherein the treatment time is based on the condition that the surface of the sample is light blue to nearly white when the sample is observed under a metallographic microscope. f. Secondary polishing: the neutralized sample is lightly polished by water on polishing cloth, 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 trace when observed under a metallographic microscope. g. And (3) secondary corrosion: and (3) corroding the sample subjected to secondary corrosion in a corrosive agent for 5-30 seconds, washing the sample with a large amount of clean water, washing the sample with absolute ethyl alcohol, drying the surface by a blower, and observing the sample.
According to a preferred embodiment of the present invention, the sample grinding step is to grind the sample from coarse to fine through 180, 240, 400, 600, 800, 1000, 1200, 1500, 2000 mesh water abrasive paper after the sample is inlaid by a inlaid machine.
According to another preferred embodiment of the present invention, the metallographic display method for Mg-containing 440C corrosion-resistant stainless bearing steel according to claim 1 is characterized in that polishing pastes of particles W3.5, W2.5, W1.5 are sequentially polished using a nylon cloth, and each polishing time 30s during polishing, the sample is rotated by 90 ° and polishing is continued until no significant wear marks are observed with the naked eye, and then light polishing is performed with water to remove the attached polishing pastes.
According to still another preferred scheme of the invention, the corrosive agent consists of 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 to 0.8 percent of ferric trichloride: 2.0 to 2.5 percent of nitric acid: 2.1 to 2.3 percent of absolute ethyl alcohol: 24% -26%, hydrochloric acid: 36% -38%, sodium laureth sulfate: 2% -3% of distilled 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 precisely controlled. The amphoteric surfactant sodium laureth sulfate is particularly added in the corrosive, so that the sodium laureth sulfate can be dissolved in water and ethanol, has solubilization performance, is favorable for dissolving corrosion products in corrosive liquid, reduces corrosion products attached to the surface of a sample, and enables the reaction to be carried out more deeply. And the ferric trichloride and the cupric 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 beneficial effects of the invention are as follows: the corrosion liquid and the corrosion method can fully and clearly display the grain boundary of the 440C corrosion-resistant stainless bearing steel containing Mg, and solve the problem of grain size grade assessment in the 440C corrosion-resistant stainless bearing steel containing Mg.
Drawings
FIG. 1 is a schematic diagram of the sample of example 1 being etched for 10 seconds with a nitrate alcohol etching solution, from which it can be seen that the sample has individual etching points and no grains are present.
FIG. 2 is a schematic diagram of the sample of example 1 being etched for 30 seconds with a nitrate alcohol etching solution, from which it can be seen that the sample has individual etching points, which are not significantly changed from FIG. 1, nor are grains present.
FIG. 3 is a schematic diagram of the sample of example 1 being etched for 60 seconds with a nitrate alcohol etching solution, from which it can be seen that the sample has individual etching points, which are not significantly changed from FIG. 2, nor are grains present.
FIG. 4 is a schematic diagram of the sample of example 1 being etched 180s with a nitrate alcohol etching solution, from which it can be seen that the sample has individual etching points, which are not significantly changed from FIG. 3, nor are grains present.
FIG. 5 is a schematic diagram of the sample of example 1 being etched for 300 seconds with a nitrate alcohol etching solution, from which it can be seen that the sample has few etching points but no grains.
FIG. 6 is a schematic diagram of the sample of example 1 being etched for 600 seconds with a nitrate alcohol etching solution, from which it can be seen that the sample has more etching points, but no grains.
FIG. 7 is a schematic diagram of the sample of example 1 being etched for 1800 seconds with a nitrate alcohol etching solution, from which it can be seen that a large number of etching spots appear in the sample, but no crystal grains appear.
Fig. 8 is a schematic diagram of the sample of example 1 being etched with a nitrate alcohol etching solution for 3600s, from which it can be seen that a large number of etching points appear on the sample, the change is insignificant compared with fig. 7, and no crystal grains appear.
FIG. 9 is a schematic diagram of the sample of example 2 being corroded for 10 seconds by the self-made corrosive liquid of the present invention, from which it can be seen that the sample is slightly corroded.
FIG. 10 is a schematic diagram of the sample in example 2 being corroded for 20s by the self-made corrosive liquid in the invention, and the sample corrosion can be seen to be further deepened.
FIG. 11 is a schematic diagram of the sample of example 2 being etched for 30s with the self-made etching solution of the present invention, from which it can be seen that the sample etching continued to be further advanced.
FIG. 12 is a schematic view of the sample in example 2 corroded by the self-made corrosive liquid in the invention for 40s, from which it can be seen that the corrosion degree of the sample is further increased, and the surface of the sample starts to appear blue.
FIG. 13 is a schematic view of the sample of example 2 corroded by the self-made corrosive liquid of the present invention for 50s, from which it can be seen that the corrosion degree of the sample is further increased, the surface of the sample exhibits a deeper blue color, and a part of grain boundary appears.
FIG. 14 is a schematic view of the sample of example 2 after being subjected to a light polishing after being corroded by the self-made corrosive for 50 seconds, and a shallower grain boundary trace can be seen from the figure.
FIG. 15 is a schematic view of the sample of example 2 after being lightly polished and then corroded for 10 seconds by the self-made corrosive of the invention, and clear grain boundaries can be seen from the figure.
FIG. 16 is a schematic diagram showing the sample corrosion for 10s after changing the nitric acid content of the self-made corrosive liquid in example 3, from which it can be seen that the sample is slightly corroded.
FIG. 17 is a schematic diagram showing the sample corrosion for 20s after the nitric acid content of the self-made corrosive liquid is changed in example 3, and the corrosion degree of the sample can be seen to be increased from the diagram.
FIG. 18 is a schematic diagram showing the sample corrosion for 30s after the nitric acid content of the self-made corrosive liquid is changed in example 3, and the corrosion degree of the sample can be further enhanced.
FIG. 19 is a schematic view showing that the sample is corroded for 40s after the nitric acid content of the self-made corrosive liquid is changed in example 3, and the corrosion degree of the sample is further deepened, so that the test surface is blue in overall, but no grain boundary trace exists.
FIG. 20 is a schematic view showing the corrosion of the sample for 50s after the nitric acid content of the self-made corrosive liquid is changed in example 3, and the corrosion degree of the sample is continuously deepened, the test surface is completely black, and the corrosion is excessive but no grain boundary trace is displayed.
Detailed Description
Hereinafter, the Mg-containing 440C corrosion resistant stainless bearing steel metallographic structure displaying method of the present invention will be described in connection with exemplary embodiments.
The metallographic structure display method of the 440C corrosion-resistant stainless bearing steel containing Mg according to the exemplary embodiment of the invention comprises the following steps:
a. and (3) mounting: and (5) embedding the patterns by using embedding powder.
b. Grinding: before preparing a metallographic sample, the sample needs to be subjected to sample grinding treatment, so that the surface roughness of the sample is reduced, and preparation is carried out for subsequent polishing work. Since 440C corrosion resistant stainless bearing steel samples are directly ground, the fingers are easily scratched. Therefore, the sample is inlaid by a sampler before polishing, so that the working efficiency is improved, and the test safety is ensured. In the invention, the samples are sequentially ground from thick to thin by using water grinding sand paper of 180, 240, 400, 600, 800, 1000, 1200, 1500 and 2000 meshes, grinding marks on the samples are ground into one direction on each sand paper four times, and the grinding directions are separated by 90 degrees.
c. Primary polishing: the sample polished with 2000 mesh sand paper was polished with polishing pastes of W3.5, W2.5, and W1.5 in this order. During polishing, the polishing surface was rotated 90 ° every 30s, and the fine grinding marks and the surface deformation layer left by fine grinding on the sample surface were removed, so that the surface became a mirror surface without grinding marks. And (3) washing the surface of the polished sample with a large amount of clean 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. And (3) primary corrosion: preparing etching liquid before etching, then placing the polished sample in an etchant to etch for 30-90 seconds, washing the sample with a large amount of clean water after no obvious bubbles are generated on the surface of the sample, then washing the sample with absolute alcohol, and drying the surface by using a blower. At this time, the surface of the sample is blue when observed under a metallographic microscope, and the observed metallographic structure is not obvious enough because the surface of the sample is covered with a large amount of corrosion products and carbides at this time.
e. And (3) neutralization treatment: the sample is neutralized by 8% aqueous potassium hydroxide solution (50-60 ℃) for 1-5 min, the treatment time is based on the observation of the sample under a metallographic microscope, the surface of the sample is light blue to nearly white, only partial corrosion products or primary corrosion liquid are neutralized, and the neutralization reaction is not stopped when the sample is observed to be white, because alkali corrosion is easy to occur locally on the sample at the moment to affect secondary corrosion.
f. 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. The trace of the primary corrosion is completely removed by applying excessive pressure, while the trace of the secondary corrosion is completely removed by applying smaller pressure, and when the discoloration generated by the corrosion of the surface of the sample is eliminated by frequently observing, the primary corrosion product is completely removed at this time, and the surface of the sample is white and has slight grain boundary trace when observed under a metallographic microscope. The purpose of the secondary polishing is to remove corrosion products coated on the surface of the specimen, exposing the masked internal tissue.
g. And (3) secondary corrosion: since the corrosion product can block the reaction from proceeding during the primary corrosion, part of the grain boundary is not corroded, or the corrosion trace is shallow, the secondary corrosion is required after the secondary polishing. After the sample after the secondary polishing is corroded in a corrosive agent for 5-30 seconds, a large amount of clean water is used for washing the sample, then absolute ethyl alcohol is used for washing, and the surface is dried by a blower to observe the sample.
The sample after the steps is completed can observe metallographic structure under a metallographic microscope.
In order to enable those skilled in the art to better understand the technical solutions of the present invention, the present invention will be further described with reference to specific examples 1, 2 and 3, but the present invention is not limited to the examples. 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 grade composition/wt.%
Example 1
The selected sample is a sample of Mg-containing 440C corrosion-resistant stainless bearing steel in a tempered state
The metallographic structure is displayed according to the following steps:
a. the metallographic phase is inlaid with inlaid powder at 140 ℃.
b. The test specimens were sequentially ground from coarse to fine by means of 180, 240, 400, 600, 800, 1000, 1200, 1500, 2000 mesh sandpaper, and the grinding marks on the test specimens were ground four times on each sandpaper in one direction, each grinding direction being spaced 90 ° apart.
c. The sample polished with 2000 mesh sand paper was polished with polishing pastes of W3.5, W2.5, and W1.5 in this order. During polishing, the polishing surface was rotated 90 ° every 30s, and the fine grinding marks and the surface deformation layer left by fine grinding on the sample surface were removed, so that the surface became a mirror surface without grinding marks. And (3) washing the surface of the polished sample with a large amount of clean 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% nitrate alcohol corrosive liquid, then placing the polished sample in 4% nitrate alcohol to respectively etch 10s, 30s, 60s, 180s, 300s, 600s, 1800s and 3600s, flushing the sample with a large amount of clear water after reaching a preset time, then flushing the sample with absolute alcohol, and drying the surface by a blower. The sample surfaces were observed under a metallographic microscope for different corrosion times.
Example 2
The selected sample is a sample of Mg-containing 440C corrosion-resistant stainless bearing steel in a tempered state
The metallographic structure is displayed according to the following steps:
a. the metallographic phase is inlaid with inlaid powder at 140 ℃.
b. Grinding the sample from coarse to fine by 180, 240, 400, 600, 800, 1000, 1200, 1500, 2000 mesh water abrasive paper, grinding the grinding mark on the sample into one direction on each abrasive paper four times, each grinding direction being spaced by 90 DEG
c. The sample polished with 2000 mesh sand paper was polished with polishing pastes of W3.5, W2.5, and W1.5 in this order. During polishing, the polishing surface was rotated 90 ° every 30s, and the fine grinding marks and the surface deformation layer left by fine grinding on the sample surface were removed, so that the surface became a mirror surface without grinding marks. And (3) washing the surface of the polished sample with a large amount of clean 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. The self-made corrosive agent is prepared from cuprous chloride, ferric trichloride, distilled water, absolute ethyl alcohol, hydrochloric acid, nitric acid and sodium laureth sulfate, and comprises the following components in percentage by mass: cuprous chloride: 0.6 percent of ferric trichloride: 2.2%, nitric acid: 2.2 percent of absolute ethyl alcohol: 25%, hydrochloric acid: 37% sodium laureth sulfate: 2.5% and the rest is distilled water. And (3) corroding the sample subjected to secondary polishing in a self-made corrosive for 5-30 seconds, washing the sample with a large amount of clean water, washing the sample with absolute ethyl alcohol, drying the surface by using a blower, and observing the sample.
Example 3
The selected sample is a sample of Mg-containing 440C corrosion-resistant stainless bearing steel in a tempered state
The metallographic structure is displayed according to the following steps:
a. the metallographic phase is inlaid with inlaid powder at 140 ℃.
b. The test specimens were sequentially ground from coarse to fine by means of 180, 240, 400, 600, 800, 1000, 1200, 1500, 2000 mesh sandpaper, and the grinding marks on the test specimens were ground four times on each sandpaper in one direction, each grinding direction being spaced 90 ° apart.
c. The sample polished with 2000 mesh sand paper was polished with polishing pastes of W3.5, W2.5, and W1.5 in this order. During polishing, the polishing surface was rotated 90 ° every 30s, and the fine grinding marks and the surface deformation layer left by fine grinding on the sample surface were removed, so that the surface became a mirror surface without grinding marks. And (3) washing the surface of the polished sample with a large amount of clean 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. The self-made corrosive agent is prepared, and consists of cuprous chloride, ferric trichloride, distilled water, absolute ethyl alcohol, hydrochloric acid, nitric acid and laureth sodium sulfate, wherein the nitric acid content of the corrosive liquid is changed in this example, and the nitric acid content is improved to 2.5%, and the mass percentages of the components are as follows: cuprous chloride: 0.6 percent of ferric trichloride: 2.2%, nitric acid: 2.5 percent of absolute ethyl alcohol: 25%, hydrochloric acid: 37% sodium laureth sulfate: 2.5% and the rest is distilled water. And (3) corroding the sample subjected to secondary polishing in a self-made corrosive for 5-30 seconds, washing the sample with a large amount of clean water, washing the sample with absolute ethyl alcohol, drying the surface by using a blower, and observing the sample.
FIGS. 1 to 8 are metallographic photographs of tempered samples obtained according to example one of the present invention. As can be seen from FIGS. 1 to 8, the conventional nitrate alcohol etching solution cannot show the metallographic structure of the Mg-containing 440C corrosion-resistant stainless bearing steel.
FIGS. 9-15 are metallographic photographs of tempered samples obtained according to example II of the present invention. As can be seen from FIGS. 9-15, the self-made corrosive liquid of the invention can corrode a clear metallographic structure of the 440C corrosion-resistant stainless bearing steel containing Mg by matching with the corrosion method of the invention.
FIGS. 16 to 20 are metallographic photographs of tempered samples obtained according to example III of the present invention, and it is understood from FIGS. 16 to 20 that when nitric acid in a self-made etching solution exceeds a specified range, a metallographic structure of Mg-containing 440C corrosion-resistant stainless bearing steel cannot be etched.
In conclusion, the metallographic specimen obtained by the metallographic structure display method of the Mg-containing 440C corrosion-resistant stainless bearing steel is clear in crystal boundary display, simple and feasible in method and high in metallographic structure definition.
Although the 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 can be made to the above-described embodiments without departing from the spirit and scope of the claims.
Claims (7)
1. A metallographic display method of a 440C corrosion-resistant stainless bearing steel containing Mg is characterized by adopting a three-step method metallographic display of primary polishing, primary corrosion, alkali solution neutralization treatment, secondary polishing and secondary corrosion, and the method comprises the following steps:
a. and (3) mounting: embedding with embedding powder;
b. grinding: polishing the sample by using water-based abrasive paper until the scratch directions on the surface of the sample are consistent;
c. primary polishing: polishing the polished sample;
d. and (3) primary corrosion: placing the polished sample in a self-made corrosive agent to etch for 30-90 seconds, washing the sample with a large amount of clean water after no obvious bubbles are generated on the surface of the sample, then washing the sample with absolute ethyl alcohol, drying the surface by a blower, and observing under a metallographic microscope at the moment, wherein the surface of the sample is blue;
e. neutralizing the sample by using 8% potassium hydroxide aqueous solution (50-60 ℃) for 1-5 min, wherein the treatment time is based on the condition that the surface of the sample is light blue to nearly white when the sample is observed under a metallographic microscope;
f. secondary polishing: the sample corroded at the first time is lightly polished by water on polishing cloth, so that the product corroded at the first time is polished, and at the moment, the sample is observed under a metallographic microscope, and the surface of the sample is white and has slight grain boundary trace;
g. and (3) secondary corrosion: etching the sample subjected to secondary polishing in a self-made corrosive for 5-30 seconds, washing the sample with a large amount of clean water, washing the sample with absolute alcohol, drying the surface by using a blower, and observing the sample;
the corrosive agent consists of 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 trichloride: 2.1% -2.3%;
nitric acid: 2.1% -2.3%;
absolute ethyl alcohol: 24% -26%;
hydrochloric acid: 36% -38%;
sodium laureth sulfate: 2% -3%;
the balance of distilled water.
2. The metallographic display method for the 440C corrosion resistant stainless bearing steel containing Mg according to claim 1, wherein the sample inserting machine is a tripod measuring XQ-2B sample inserting machine, the sample inserting temperature is 140 ℃, the input voltage is 220V when the sample is inserted, and the input power is 800W.
3. The metallographic display method of the 440C corrosion resistant stainless bearing steel containing Mg according to claim 1, wherein the mosaic powder is black-colored mosaic powder of model HD-010 of a Hengda instrument.
4. A metallographic display method for Mg-containing 440C corrosion-resistant stainless bearing steel according to claim 1, wherein the abrasion-resistant sandpaper is a Olive brand water-resistant sandpaper.
5. The method of metallographic display of Mg-containing 440C corrosion resistant stainless bearing steel according to claim 1, wherein the polishing paste is ZZSM model KDN diamond paste.
6. The method for displaying metallographic phase of 440C corrosion resistant stainless bearing steel containing Mg according to claim 1, wherein the step of grinding is to grind the sample from coarse to fine mesh water abrasive paper respectively by 180, 240, 400, 600, 800, 1000, 1200, 1500, 2000 mesh water abrasive paper after the sample is sample-inlaid by a sample inlaid machine.
7. The method for displaying metallographic phase of 440C corrosion resistant stainless bearing steel containing Mg according to claim 1, wherein polishing pastes of particles W3.5, W2.5, W1.5 are sequentially polished using a ni flannel, and each polishing step is performed for 30 seconds to rotate the sample by 90 ° during polishing, and after polishing is continued until no significant scratches are observed with naked eyes, the polishing pastes are removed by light polishing with water.
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