CN113092505A - Method for detecting non-metallic inclusions in steel - Google Patents
Method for detecting non-metallic inclusions in steel Download PDFInfo
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- CN113092505A CN113092505A CN202110245493.5A CN202110245493A CN113092505A CN 113092505 A CN113092505 A CN 113092505A CN 202110245493 A CN202110245493 A CN 202110245493A CN 113092505 A CN113092505 A CN 113092505A
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- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 29
- 239000010959 steel Substances 0.000 title claims abstract description 29
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000012528 membrane Substances 0.000 claims abstract description 55
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000003792 electrolyte Substances 0.000 claims abstract description 26
- 239000000243 solution Substances 0.000 claims abstract description 26
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000012535 impurity Substances 0.000 claims abstract description 22
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims abstract description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 16
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000007885 magnetic separation Methods 0.000 claims abstract description 13
- 238000000605 extraction Methods 0.000 claims abstract description 11
- 238000005728 strengthening Methods 0.000 claims abstract description 11
- OKIZCWYLBDKLSU-UHFFFAOYSA-M N,N,N-Trimethylmethanaminium chloride Chemical compound [Cl-].C[N+](C)(C)C OKIZCWYLBDKLSU-UHFFFAOYSA-M 0.000 claims abstract description 9
- 239000000853 adhesive Substances 0.000 claims abstract description 9
- 230000001070 adhesive effect Effects 0.000 claims abstract description 9
- 229910052751 metal Inorganic materials 0.000 claims abstract description 9
- 239000002184 metal Substances 0.000 claims abstract description 9
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 9
- 239000010935 stainless steel Substances 0.000 claims abstract description 9
- 239000006104 solid solution Substances 0.000 claims abstract description 8
- 238000005507 spraying Methods 0.000 claims abstract description 8
- 238000002955 isolation Methods 0.000 claims abstract description 4
- 229920002301 cellulose acetate Polymers 0.000 claims description 10
- 238000005868 electrolysis reaction Methods 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 description 12
- -1 polypropylene Polymers 0.000 description 12
- 229920001155 polypropylene Polymers 0.000 description 12
- 238000004140 cleaning Methods 0.000 description 8
- 238000009826 distribution Methods 0.000 description 7
- 238000000967 suction filtration Methods 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- 229910000639 Spring steel Inorganic materials 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
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Abstract
The invention discloses a method for detecting nonmetallic inclusion in steel, which adopts the following processes: preparing a rod-shaped sample after the sample to be detected is subjected to solid solution strengthening; using a stainless steel sleeve as a cathode and a rod-shaped sample as an anode, and adopting a semipermeable membrane for isolation to perform electrolytic extraction; the electrolyte comprises the following components in percentage by weight: 0.01-0.1 g/ml of tetramethylammonium chloride, 0.1-0.25 ml/ml of acetylacetone and the balance of methanol solution with the mass fraction of 95-99 percent; dissolving the electrolyzed electrolyte in absolute ethyl alcohol, and filtering by using a filter membrane; dissolving the impurities on the filter membrane in the absolute ethyl alcohol solution again, and obtaining clean impurities after magnetic separation and filtration; inlaying clean inclusions on a metal plane with conductive adhesive, and spraying platinum to prepare an ASPEX observation sample; and detecting the ASPEX observation sample by using an ASPEX automatic scanning electron microscope to obtain the detection information of all the extracted inclusions. The method can be used for detecting the nonmetallic inclusion in the steel in a nondestructive, complete and rapid manner, and greatly reduces the manual workload and the errors caused by manual work.
Description
Technical Field
The invention belongs to the field of electrochemical and physical detection, and particularly relates to a method for detecting nonmetallic inclusions in steel.
Background
Numerous studies have shown that the type, size, distribution, amount of non-metallic inclusions in steel have a great influence on the quality of the steel. The non-metallic inclusion destroys the continuity of steel matrix structure, can reduce the mechanical property and fatigue property of steel, and deteriorates the cold and hot workability and certain physical and chemical indexes of steel. Accurately and completely representing the nonmetallic inclusion in the steel is very important for improving the cleanliness of the steel.
The main defects of the traditional detection method for nonmetallic inclusions by combining electrochemical extraction and a field emission scanning electron microscope are as follows: 1. the electrolyte adopts acidic or alkaline solution, and in the electrolytic process, partial oxide impurities can be dissolved in the electrolyte; 2. the electrolytic sample which is not subjected to the solution treatment is difficult to remove carbides; 3. the field emission scanning electron microscope is used for detecting the inclusions, the analysis speed is low, the manual working measuring tool is large, no inclusions exist in 99 percent of the field of view, the inclusions need to be manually distinguished, and the field emission scanning electron microscope is 100mm2The scanning time of the detection area is about 10 hours; 4. the analysis result is unreliable, the field emission electron microscope belongs to static scanning, and the picture collected by analysis is not an actual sample and can not effectively distinguish inclusions and pollutants.
Disclosure of Invention
The invention aims to provide a method for quickly and accurately detecting nonmetallic inclusions in steel.
In order to solve the technical problem, the invention adopts the following process: (1) sample preparation: preparing a rod-shaped sample after the sample to be detected is subjected to solid solution strengthening;
(2) electrolysis: using a stainless steel sleeve as a cathode and a rod-shaped sample as an anode, and adopting a semipermeable membrane for isolation to perform electrolytic extraction; the electrolyte comprises the following components in percentage by weight: 0.01-0.1 g/ml of tetramethylammonium chloride, 0.1-0.25 ml/ml of acetylacetone and the balance of methanol solution with the mass fraction of 95-99 percent;
(3) collecting impurities: dissolving the electrolyzed electrolyte in absolute ethyl alcohol, and filtering by using a filter membrane; dissolving the impurities on the filter membrane in the absolute ethyl alcohol solution again, and obtaining clean impurities after magnetic separation and filtration;
(4) inlaying inclusions: inlaying clean inclusions on a metal plane with conductive adhesive, and spraying platinum to prepare an ASPEX observation sample;
(5) ASPEX auto-scan: and detecting the ASPEX observation sample by using an ASPEX automatic scanning electron microscope to obtain the detection information of all the extracted inclusions.
In the step (1), the sample to be detected is subjected to solid solution strengthening at 1000-1200 ℃.
In the step (2) of the present invention, the semipermeable membrane is a cellulose acetate membrane.
In the step (2) of the present invention, the electrolytic current is 0.05A/cm2～0.10A/cm2。
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in: the inclusion extracted by the invention is detected by adopting ASPEX automatic scanning, and has the following advantages: 1. the detection speed is high, the detection of the inclusions is synchronous with the chemical analysis, and the detection speed is 100mm2The steel sample with the size of 5000 inclusions only needs 1 hour for detection, and the information of images, the number, the types, the sizes, the distribution and the like of the inclusions is automatically stored; 2. the ASPEX adopts real-time dynamic analysis and calculation and an automatic inclusion locking technology, so that the error is greatly reduced, and the inclusion particle detection passes the certification of the American national standards and technology institute; 3. unmanned operation can be realized, and the inclusion information is automatically scanned and stored through system setting, so that the manual workload is greatly reduced. The method combining non-aqueous solution electrolytic extraction and ASPEX automatic scanning is adopted, so that the non-metallic inclusions in the steel can be detected nondestructively, completely and quickly, and the manual workload and errors caused by manual work are greatly reduced.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a schematic view of the construction of an electrolysis apparatus;
FIG. 2 shows Al in example 12O3A morphology map of inclusions;
FIG. 3 is a graph showing the morphology of TiN inclusions in example 1;
FIG. 4 is a morphology of MnS-TiS inclusion in example 1;
FIG. 5 shows MnS-Al in example 12O3-a topographic map of CaO inclusions;
FIG. 6 is a morphology of MnS inclusion in example 1;
FIG. 7 is a morphology of MnS-CaS inclusions in example 1;
FIG. 8 shows CaO-Al in example 12O3A morphology map of inclusions;
FIG. 9 shows MnS-Al in example 12O3A morphology map of inclusions;
FIG. 10 is a graph showing the morphology of CaO inclusion in example 1;
FIG. 11 is a graph showing the size, number and distribution of inclusions in the ASEPX automatic scan of example 1;
FIG. 12 is an ASEPX autoscan electrolyte inclusion distribution plot from example 2;
FIG. 13 is an ASEPX autoscan electrolyte inclusion distribution plot from example 3;
FIG. 14 is an ASEPX autoscan electrolyte inclusion distribution plot from example 4;
FIG. 15 is an ASEPX auto-scan distribution diagram of electrolytic inclusions in example 5.
In the figure: 1 is an isolation cover; 2 is electrolyte; 3 is a cathode; 4 is a semipermeable membrane; 5 is a cathode frame; 6 is an anode.
Detailed Description
The method for detecting the non-metallic inclusions in the steel adopts the following process steps: (1) preparing nonaqueous solution for electrolysis: electrolyte proportion of nonaqueous solution electrolysis: 0.01-0.1 g of tetramethylammonium chloride, 0.1-0.25 ml of acetylacetone and the balance of 95-99 wt% of methanol solution are added into each ml of electrolyte.
(2) Sample preparation: the steel to be detected is subjected to solid solution strengthening at 1000-1200 ℃, carbide is well solid-dissolved in the process, and inclusions cannot be solid-dissolved; then lathing into a rod-shaped sample with the diameter of 5mm and the length of 40mm, lathing off the surface iron oxide scale, ultrasonically cleaning the surface of the sample, and drying.
(3) Preparing an electrolytic semipermeable membrane: the adding ratio of the cellulose acetate to the acetone is 45g to 500ml, namely 90g of the cellulose acetate is added into 1000ml of the acetone; fully and uniformly mixing, and preparing the cellulose acetate semipermeable membrane by using the glass capsule cup and the capsule ring as membranes.
(4) Electrolysis: using stainless steel sleeve as cathode, rod-like sample as anode, adopting semipermeable membrane to separate, connecting electrolysis device as shown in figure 1 at 0.05A/cm2～0.1A/cm2The electrolytic extraction is performed at a constant current density.
(5) Collecting electrolytic sludge: after the rod-shaped sample is completely electrolyzed, dissolving the electrolyte and the electrolyte product on the semipermeable membrane in absolute ethyl alcohol, performing suction filtration by using a filter membrane, and filtering all impurities on the filter membrane; the precision of the filter membrane is determined according to the size of the inclusions to be observed, and a polypropylene microporous filter membrane is adopted.
(6) Magnetic separation, filtration and cleaning: dissolving the impurities on the filter membrane in an absolute ethyl alcohol solution, and carrying out graded magnetic separation in a magnetic separation device to remove magnetic components in the solution, wherein the magnetic separation strength is respectively 500Gs, 1000GS, 1500GS, 2000GS, 2500GS, 3000GS and 3500 GS; filtering the solution subjected to magnetic separation by using a filter membrane which is the same as the filter membrane obtained in the step 5, repeatedly cleaning the filter membrane for 3-4 times by using absolute ethyl alcohol, and finally, completely concentrating clean impurities on the filter membrane; the precision of the filter membrane is determined according to the size of the inclusions to be observed, and a polypropylene microporous filter membrane is adopted.
(7) Inlaying inclusions: uniformly embedding clean inclusions on a clean and flat metal plane by using conductive adhesive; platinum was sprayed on the inclusions to prepare an ASPEX observation sample.
(8) ASPEX auto-scan: and (3) detecting the ASPEX observation sample by using an ASPEX automatic scanning electron microscope to obtain a plurality of information such as three-dimensional morphology, size, quantity, type and the like of all the extracted inclusions.
Example 1: the method for detecting nonmetallic inclusions in the present steel is specifically as follows.
(1) Carrying out solution strengthening on a sample to be detected of GCr15 bearing steel at 1000 ℃ to prepare a rod-shaped sample; using stainless steel sleeve as cathode, rod-like sample as anode, and isolating with cellulose acetate semipermeable membrane at 0.05A/cm2Carrying out electrolytic extraction under constant current; the electrolyte comprises the following components in percentage by weight: 0.01g/ml of tetramethylammonium chloride, 0.1ml/ml of acetylacetone, and the balance of 99wt% methanol solution.
(2) Dissolving the electrolyzed electrolyte in absolute ethyl alcohol, and filtering by using a polypropylene microporous filter membrane of 1 um; and dissolving the impurities on the filter membrane into the absolute ethyl alcohol solution again, carrying out magnetic separation by 500Gs, 1000GS, 1500GS, 2000GS, 2500GS, 3000GS and 3500GS, carrying out suction filtration by using a polypropylene microporous filter membrane with the diameter of 1um, and cleaning for 3 times by using absolute ethyl alcohol, thus collecting all clean impurities on the filter membrane.
(3) Inlaying clean inclusions on a metal plane with conductive adhesive, and spraying platinum to prepare an ASPEX observation sample; the ASPEX observation sample is detected by an ASPEX automatic scanning electron microscope to obtain a plurality of information of three-dimensional morphology, size, quantity, type and the like of all the extracted inclusions, as shown in table 1, figures 2-10 and figure 11.
Table 1: example 1 results of detection of inclusions in samples
Example 2: the method for detecting nonmetallic inclusions in the present steel is specifically as follows.
(1) Carrying out solution strengthening on a sample to be detected made of 60Si2Mn spring steel at 1000 ℃ to prepare a rod-shaped sample; using stainless steel sleeve as cathode, rod-like sample as anode, and isolating with cellulose acetate semipermeable membrane at 0.05A/cm2Carrying out electrolytic extraction under constant current; the electrolyte comprises the following components in percentage by weight: 0.01g/ml of tetramethylammonium chloride, 0.1ml/ml of acetylacetone and the balance of 99wt%Methanol solution.
(2) Dissolving the electrolyzed electrolyte in absolute ethyl alcohol, and filtering by using a polypropylene microporous filter membrane of 1 um; and dissolving the impurities on the filter membrane into the absolute ethyl alcohol solution again, carrying out magnetic separation by 500Gs, 1000GS, 1500GS, 2000GS, 2500GS, 3000GS and 3500GS, carrying out suction filtration by using a polypropylene microporous filter membrane with the diameter of 1um, and cleaning for 3 times by using absolute ethyl alcohol, thus collecting all clean impurities on the filter membrane.
(3) Inlaying clean inclusions on a metal plane with conductive adhesive, and spraying platinum to prepare an ASPEX observation sample; the ASPEX observation sample is detected by an ASPEX automatic scanning electron microscope to obtain a plurality of information such as three-dimensional morphology, size, number, type and the like of all the extracted inclusions, as shown in table 2 and fig. 12.
Table 2: example 2 detection results of inclusions in samples
Example 3: the method for detecting nonmetallic inclusions in the present steel is specifically as follows.
(1) The method comprises the following steps of (1) carrying out solid solution strengthening on a sample to be detected of GCr15 bearing steel at 1100 ℃ to prepare a rod-shaped sample; using stainless steel sleeve as cathode, rod-like sample as anode, and isolating with cellulose acetate semipermeable membrane at 0.1A/cm2Carrying out electrolytic extraction under constant current; the electrolyte comprises the following components in percentage by weight: 0.05g/ml of tetramethylammonium chloride, 0.25ml/ml of acetylacetone, and the balance of a 95wt% methanol solution.
(2) Dissolving the electrolyzed electrolyte in absolute ethyl alcohol, and filtering by using a polypropylene microporous filter membrane of 1 um; and dissolving the impurities on the filter membrane into the absolute ethyl alcohol solution again, carrying out magnetic separation by 500Gs, 1000GS, 1500GS, 2000GS, 2500GS, 3000GS and 3500GS, carrying out suction filtration by using a polypropylene microporous filter membrane with the diameter of 1um, and cleaning for 4 times by using absolute ethyl alcohol, thus collecting all clean impurities on the filter membrane.
(3) Inlaying clean inclusions on a metal plane with conductive adhesive, and spraying platinum to prepare an ASPEX observation sample; the ASPEX observation sample was examined using an ASPEX automatic scanning electron microscope to obtain a variety of information on the three-dimensional morphology, size, number, type, etc. of all the extracted inclusions, as shown in table 3 and fig. 13.
Table 3: example 3 detection results of inclusions in samples
Example 4: the method for detecting nonmetallic inclusions in the present steel is specifically as follows.
(1) Preparing a rod-shaped sample from 60Si2Mn spring steel to-be-detected sample after solution strengthening at 1200 ℃; using stainless steel sleeve as cathode, rod-like sample as anode, and isolating with cellulose acetate semipermeable membrane at 0.08A/cm2Carrying out electrolytic extraction under constant current; the electrolyte comprises the following components in percentage by weight: 0.03g/ml of tetramethylammonium chloride, 0.15ml/ml of acetylacetone, and the balance of a 98wt% methanol solution.
(2) Dissolving the electrolyzed electrolyte in absolute ethyl alcohol, and filtering by using a polypropylene microporous filter membrane of 1 um; and dissolving the impurities on the filter membrane into the absolute ethyl alcohol solution again, carrying out magnetic separation by 500Gs, 1000GS, 1500GS, 2000GS, 2500GS, 3000GS and 3500GS, carrying out suction filtration by using a polypropylene microporous filter membrane with the diameter of 1um, and cleaning for 3 times by using absolute ethyl alcohol, thus collecting all clean impurities on the filter membrane.
(3) Inlaying clean inclusions on a metal plane with conductive adhesive, and spraying platinum to prepare an ASPEX observation sample; the ASPEX observation sample was examined using an ASPEX automatic scanning electron microscope to obtain a variety of information on the three-dimensional morphology, size, number, type, etc. of all the extracted inclusions, as shown in table 4 and fig. 14.
Table 4: example 4 detection results of inclusions in samples
Example 5: the method for detecting nonmetallic inclusions in the present steel is specifically as follows.
(1) The method comprises the following steps of (1) carrying out solid solution strengthening on a sample to be detected of GCr15 bearing steel at 1100 ℃ to prepare a rod-shaped sample; using stainless steel sleeve as cathode, rod-like sample as anode, and isolating with cellulose acetate semipermeable membrane at 0.07A/cm2Carrying out electrolytic extraction under constant current; the electrolyte comprises the following components in percentage by weight: 0.1g/ml of tetramethylammonium chloride, 0.2ml/ml of acetylacetone, and the balance of a 98wt% methanol solution.
(2) Dissolving the electrolyzed electrolyte in absolute ethyl alcohol, and filtering by using a polypropylene microporous filter membrane of 1 um; and dissolving the impurities on the filter membrane into the absolute ethyl alcohol solution again, carrying out magnetic separation by 500Gs, 1000GS, 1500GS, 2000GS, 2500GS, 3000GS and 3500GS, carrying out suction filtration by using a polypropylene microporous filter membrane with the diameter of 1um, and cleaning for 4 times by using absolute ethyl alcohol, thus collecting all clean impurities on the filter membrane.
(3) Inlaying clean inclusions on a metal plane with conductive adhesive, and spraying platinum to prepare an ASPEX observation sample; the ASPEX observation sample was examined using an ASPEX automatic scanning electron microscope to obtain a variety of information on the three-dimensional morphology, size, number, type, etc. of all the extracted inclusions, as shown in table 5 and fig. 15.
Table 5: example 5 detection results of inclusions in samples
Claims (4)
1. A method for detecting non-metallic inclusions in steel is characterized by comprising the following steps: (1) sample preparation: preparing a rod-shaped sample after the sample to be detected is subjected to solid solution strengthening;
(2) electrolysis: using a stainless steel sleeve as a cathode and a rod-shaped sample as an anode, and adopting a semipermeable membrane for isolation to perform electrolytic extraction; the electrolyte comprises the following components in percentage by weight: 0.01-0.1 g/ml of tetramethylammonium chloride, 0.1-0.25 ml/ml of acetylacetone and the balance of methanol solution with the mass fraction of 95-99 percent;
(3) collecting impurities: dissolving the electrolyzed electrolyte in absolute ethyl alcohol, and filtering by using a filter membrane; dissolving the impurities on the filter membrane in the absolute ethyl alcohol solution again, and obtaining clean impurities after magnetic separation and filtration;
(4) inlaying inclusions: inlaying clean inclusions on a metal plane with conductive adhesive, and spraying platinum to prepare an ASPEX observation sample;
(5) ASPEX auto-scan: and detecting the ASPEX observation sample by using an ASPEX automatic scanning electron microscope to obtain the detection information of all the extracted inclusions.
2. The method for detecting nonmetallic inclusions in steel as set forth in claim 1, wherein: in the step (1), the sample to be detected is subjected to solid solution strengthening at 1000-1200 ℃.
3. The method for detecting nonmetallic inclusions in steel as set forth in claim 1, wherein: in the step (2), the semipermeable membrane is a cellulose acetate membrane.
4. The method for detecting nonmetallic inclusions in steel as set forth in claim 1, 2, or 3, wherein: in the step (2), the electrolytic current is 0.05A/cm2～0.10A/cm2。
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113447509A (en) * | 2021-07-30 | 2021-09-28 | 钢铁研究总院 | Sample preparation method of scanning electron microscope sample for inclusions in rare earth weathering steel |
| CN114323873A (en) * | 2022-01-14 | 2022-04-12 | 慈兴集团有限公司 | Method for detecting particle components on surface of bearing |
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| JP2004198144A (en) * | 2002-12-16 | 2004-07-15 | Kobe Steel Ltd | Method for analyzing composition and/or particle size of nonmetallic inclusion in metal sample |
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