CN113063847A - Method for detecting defects of 35NCD16 alloy magnetic powder flaw detection - Google Patents
Method for detecting defects of 35NCD16 alloy magnetic powder flaw detection Download PDFInfo
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- 230000007547 defect Effects 0.000 title claims abstract description 175
- 238000000034 method Methods 0.000 title claims abstract description 28
- 239000006247 magnetic powder Substances 0.000 title claims abstract description 23
- 229910045601 alloy Inorganic materials 0.000 title claims abstract description 17
- 239000000956 alloy Substances 0.000 title claims abstract description 17
- 238000001514 detection method Methods 0.000 title claims abstract description 12
- 238000007689 inspection Methods 0.000 claims abstract description 25
- 230000003647 oxidation Effects 0.000 claims abstract description 20
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 20
- 230000007797 corrosion Effects 0.000 claims abstract description 12
- 238000005260 corrosion Methods 0.000 claims abstract description 12
- 239000006249 magnetic particle Substances 0.000 claims abstract description 8
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 150000001875 compounds Chemical class 0.000 claims description 25
- 239000002893 slag Substances 0.000 claims description 19
- 238000003723 Smelting Methods 0.000 claims description 18
- 230000002159 abnormal effect Effects 0.000 claims description 14
- 230000003287 optical effect Effects 0.000 claims description 10
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 7
- 238000009826 distribution Methods 0.000 claims description 6
- 238000005498 polishing Methods 0.000 claims description 6
- 238000010183 spectrum analysis Methods 0.000 claims description 6
- 229910001338 liquidmetal Inorganic materials 0.000 claims description 3
- 238000005242 forging Methods 0.000 abstract description 5
- 238000001228 spectrum Methods 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 description 14
- 229910052804 chromium Inorganic materials 0.000 description 9
- 229910052742 iron Inorganic materials 0.000 description 9
- 229910052759 nickel Inorganic materials 0.000 description 9
- 229910052782 aluminium Inorganic materials 0.000 description 5
- 229910052791 calcium Inorganic materials 0.000 description 5
- 229910052749 magnesium Inorganic materials 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 238000010891 electric arc Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 229910001182 Mo alloy Inorganic materials 0.000 description 1
- 241001085205 Prenanthella exigua Species 0.000 description 1
- 229910000746 Structural steel Inorganic materials 0.000 description 1
- 229910000797 Ultra-high-strength steel Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910001634 calcium fluoride Inorganic materials 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- OGSYQYXYGXIQFH-UHFFFAOYSA-N chromium molybdenum nickel Chemical compound [Cr].[Ni].[Mo] OGSYQYXYGXIQFH-UHFFFAOYSA-N 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000005496 tempering Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/72—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables
- G01N27/82—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables for investigating the presence of flaws
- G01N27/83—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables for investigating the presence of flaws by investigating stray magnetic fields
- G01N27/84—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating magnetic variables for investigating the presence of flaws by investigating stray magnetic fields by applying magnetic powder or magnetic ink
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/32—Polishing; Etching
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Abstract
The invention discloses a method for detecting defects of 35NCD16 alloy magnetic powder flaw detection, which is implemented according to the following steps: step 1, observing the shape and size of a defect under magnetic particle inspection, and recording the position of the defect; step 2, cutting a normal sample and a defect sample, carrying out microscopic structure analysis, judging the samples to be metallurgical defects, and carrying out step 3; step 3, carrying out oxidation phenomenon analysis on the corrosion state defect sample, judging non-oxidation loss, and carrying out step 4; and 4, analyzing the microstructure components of the corrosion state defect sample. According to the scheme, the properties and reasons of the defects of the 35NCD16 alloy forging are determined by methods such as magnetic powder inspection defect observation, high-low magnification tissue observation, scanning electron microscope tissue observation, energy spectrum component analysis and the like.
Description
Technical Field
The invention belongs to the technical field of metal quality inspection, and relates to a method for detecting defects of 35NCD16 alloy magnetic powder inspection.
Background
35NCD16 is a chromium-nickel-molybdenum alloy structural steel that can be used as both a wrought steel and an ultra-high strength steel. In a modulation processing state, the composite material has excellent combination of strength, toughness and plasticity; after quenching and low-temperature tempering, the steel has high strength. The smelting is generally carried out by adopting an electric arc furnace and vacuum consumable remelting or an electric arc furnace and electroslag remelting process. The composite material is widely used as parts such as important aviation shafts, bolts, aircraft landing gears and the like.
According to the scheme, the properties and reasons of the defects of the 35NCD16 alloy forging are determined by methods such as magnetic powder inspection defect observation, high-low magnification tissue observation, scanning electron microscope tissue observation, energy spectrum component analysis and the like.
Disclosure of Invention
The invention aims to provide a method for detecting defects of 35NCD16 alloy magnetic powder inspection, which solves the problem that the prior art lacks a method for detecting and analyzing defects of 35NCD16 alloy forgings in a system specification.
The invention adopts the technical scheme that a method for detecting the defects of 35NCD16 alloy magnetic powder flaw detection is implemented according to the following steps:
a defect detection method for 35NCD16 alloy magnetic powder inspection is implemented according to the following steps:
step 1, observing the shape and size of a defect under magnetic particle inspection, and recording the position of the defect;
step 2, cutting a normal sample and a defect sample, carrying out microscopic structure analysis, judging the samples to be metallurgical defects, and carrying out step 3;
step 3, carrying out oxidation phenomenon analysis on the corrosion state defect sample, judging non-oxidation loss, and carrying out step 4;
and 4, analyzing the microstructure components of the corrosion state defect sample.
The invention is also characterized in that:
the step 2 is implemented according to the following steps:
step 2.1, polishing the normal sample and the defect sample to obtain a polished normal sample and a polished defect sample;
step 2.2, observing the polished defect sample under a 100X optical microscope;
step 2.3, if other abnormal defects exist near the defect, the defect is caused by the abnormal defect;
step 2.4, if no other abnormal defects exist near the defects and the content of the non-metallic inclusions near the defects exceeds the standard requirement, the defects are cracks caused by the fact that the content of the non-metallic inclusions exceeds the standard;
and 2.5, if no other abnormal defects exist near the defects and the content and distribution of the non-metallic inclusions near the defects are basically uniform and consistent with those of the polished normal sample, determining the defects as metallurgical defects and analyzing the oxidation phenomenon.
Step 3 is specifically implemented according to the following steps:
step 3.1, grinding and polishing the normal sample and the defect sample, and corroding the normal sample and the defect sample by using a corrosive to obtain a corrosion state defect sample;
and 3.2, observing under a 100X optical microscope, wherein if an oxidation phenomenon occurs near the defect and the oxide film remains, the defect is formed when the oxide film is rolled into the liquid metal, and if no oxidation phenomenon exists, the step 4 is carried out.
The etchant of step 3.1 is a 4% nital solution.
Step 4 is specifically implemented according to the following steps:
step 4.1, performing energy spectrum analysis on the polished defect sample, and performing energy spectrum analysis on metal components of compounds around and inside the defect;
4.2, analyzing the main element composition of the metal components of the compounds around and inside the defect, and comparing the main element composition with the composition of the molten slag added in the smelting process;
and 4.3, if the components of the slag added in the smelting of the granular compounds are consistent, slag inclusion formed by incomplete smelting of the added slag in the smelting process is avoided, otherwise, the slag inclusion is not achieved.
The invention has the beneficial effects that: according to the scheme, the properties and reasons of the defects of the 35NCD16 alloy forging are determined by methods such as magnetic powder inspection defect observation, high-low magnification tissue observation, scanning electron microscope tissue observation, energy spectrum component analysis and the like.
Drawings
FIG. 1 is a view showing a defect inspection using magnetic powder according to example 1;
FIG. 2 is a polished high magnification texture map of example 1;
FIG. 3 is a high power corrosion microstructure of example 1;
FIG. 4 is a scanning electron micrograph of example 1;
FIG. 5 is a diagram showing the energy spectrum component analysis position in example 1.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
A defect detection method for 35NCD16 alloy magnetic powder inspection is implemented according to the following steps:
step 1, observing the shape and size of a defect under magnetic particle inspection, and recording the position of the defect;
step 2, cutting a normal sample and a defect sample, carrying out microscopic structure analysis, judging the samples to be metallurgical defects, and carrying out step 3;
step 3, carrying out oxidation phenomenon analysis on the corrosion state defect sample, judging non-oxidation loss, and carrying out step 4;
and 4, analyzing the microstructure components of the corrosion state defect sample.
The step 2 is implemented according to the following steps:
step 2.1, polishing the normal sample and the defect sample to obtain a polished normal sample and a polished defect sample;
step 2.2, observing the polished defect sample under a 100X optical microscope;
step 2.3, if other abnormal defects exist near the defect, the defect is caused by the abnormal defect;
step 2.4, if no other abnormal defects exist near the defects and the content of the non-metallic inclusions near the defects exceeds the standard requirement, the defects are cracks caused by the fact that the content of the non-metallic inclusions exceeds the standard;
and 2.5, if no other abnormal defects exist near the defects and the content and distribution of the non-metallic inclusions near the defects are basically uniform and consistent with those of the polished normal sample, determining the defects as metallurgical defects, and analyzing the oxidation phenomenon for determining the cause of the specific metallurgical defects.
Step 3 is specifically implemented according to the following steps:
step 3.1, grinding and polishing the normal sample and the defect sample, and corroding the normal sample and the defect sample by using a corrosive to obtain a corrosion state defect sample;
and 3.2, observing under a 100X optical microscope, wherein if an oxidation phenomenon occurs near the defect and the oxide film remains, the defect is formed when the oxide film is rolled into the liquid metal, and if no oxidation phenomenon exists, the step 4 is carried out.
The etchant of step 3.1 is a 4% nital solution.
Step 4 is specifically implemented according to the following steps:
step 4.1, performing energy spectrum analysis on the polished defect sample, and performing energy spectrum analysis on metal components of compounds around and inside the defect;
4.2, analyzing the metal component and main element composition of compounds around and inside the defect, and comparing the metal component and the main element composition with the components of the molten slag added in the smelting process;
and 4.3, if the components of the slag added in the smelting of the granular compounds are consistent, slag inclusion formed by incomplete smelting of the added slag in the smelting process is avoided, otherwise, the slag inclusion is not achieved.
The analytical results were as follows:
as shown in fig. 2a, 2 b. The high power samples at the magnetic powder inspection linear display position and the magnetic powder inspection normal position are observed under a 100X optical microscope after being ground and polished, and the transverse high power tissue of the polished state is shown in figure 2. The magnetic powder flaw detection linear display position surface has a defect. The defect was about 0.16mm long, about 0.03mm wide, about 0.13mm deep, and at an angle of about 60 ° to the surface. The defects appeared to be discontinuous in black under an optical microscope. Except the defects, other abnormal defects are not seen near the defects, and the content and distribution of the non-metallic inclusions near the defects are basically uniform with other parts. The defects are not caused by processing operation errors or external force damage.
As shown in fig. 3a, 3 b. The high power samples at the magnetic powder flaw detection linear display position and the flaw detection normal position are polished and corroded and then observed under a 100X optical microscope, and the corroded transverse high power tissue is shown in figure 3. The linear display position of the magnetic powder flaw detection has a black discontinuous defect which is basically consistent with the size, the shape and the distribution of a polished state, and the oxidation phenomenon is not seen near the defect. Except the defects, other abnormal defects are not seen near the defects, and the linear display position of the magnetic powder inspection is basically uniform with the tissues of other parts (the grain size is about 6.5 grades).
The polished state and corroded state structures of the defects are observed under a 1KX scanning electron microscope, the sizes, the shapes and the distribution of the defects in the polished state and the corroded state are basically consistent, the defects are discontinuous, the boundaries are not smooth, and a small number of point-like defects exist near the defects, as shown in figures 4a and 4 b. And (3) observing a defect structure under a 9KX scanning electron microscope, wherein the defect and the matrix are basically in the same plane and have no obvious pits, granular compounds are distributed in the defect, a small amount of point defects near the defect are also granular compounds, and the defect has no oxidation phenomenon, and is not caused by oxidation loss as shown in figures 4c and 4 d.
The results of step 4 are as follows: the energy spectrum components of the defect and the normal are analyzed in a comparative way, the analysis position is shown in figure 5, and the component analysis result is shown in table 1. The normal part elements (matrix elements) mainly comprise Cr, Fe and Ni; the main elements of the granular compounds in the defects are O, Mg, Al, Ca, Cr, Fe and Ni, the difference between the types and the contents of the main elements of the granular compounds in the defects and the matrix is relatively large, and the granular compounds in the defects also contain more elements such as O, Mg, Al, Ca and the like besides the matrix elements of Cr, Fe and Ni; the main elements of the compound-free positions in the defects contain matrix elements Cr, Fe and Ni which are relatively close to the matrix content, and a trace amount of Al element.
TABLE 1 analysis of spectral components
The defects displayed by magnetic powder inspection are surface defects. The defect was about 6mm axially long, about 0.13mm deep, about 0.03mm wide and at an angle of about 60 ° to the surface. The defect is displayed as a bright white defect under magnetic powder inspection; the defect is a black discontinuous defect under a 100X optical microscope; under a 1KX scanning electron microscope, the defect is discontinuous, the boundary is not smooth, and a small amount of granular defects exist nearby; under a 9KX scanning electron microscope, the defects and the matrix are basically in the same plane, obvious pits do not exist, granular compounds are distributed in the defects, and a small amount of nearby granular defects are also granular compounds. These characteristics indicate that the defect is a compound inclusion. The inclusions deform along with the deformation of the forging in the deformation process to form linear inclusion strips distributed along the axial direction, and the linear inclusion strips are characterized as defects along the axial direction under the magnetic powder inspection.
The normal part elements (matrix elements) are mainly Cr, Fe and Ni. The main elements of the compounds in the defects are O, Mg, Al, Ca, Cr, Fe and Ni, the types and the contents of the main elements of the compounds in the defects are greatly different from those of the matrix, and the compounds in the defects also contain more elements such as O, Mg, Al, Ca and the like besides the matrix elements of Cr, Fe and Ni. The main elements of the defect without compound sites contain trace Al elements besides matrix elements Cr, Fe and Ni which are relatively close to the matrix content, which is supposed to be because the compounds in the defect are peeled off in the sample grinding process, so that the defect is free of obvious compound particles and the element content of the defect is close to the matrix. The smelting process of the bar used by the forge piece is electric arc furnace and electroslag remelting process smelting, the common slag of the electroslag remelting process is based on CaF2 and is prepared by adding proper CaO, Al2O3, MgO, SiO2 and other oxides, and compounds in defects contain matrix elements of Cr, Fe and Ni, and more O, Mg, Al, Ca and other elements, and basically accord with the components of the slag added by smelting. Therefore, the compounds in the defects can be basically judged to be slag commonly used in the electroslag remelting process.
The defect of magnetic powder inspection is slag inclusion formed by incomplete smelting of slag added in the smelting process.
Claims (5)
1. A defect detection method for 35NCD16 alloy magnetic powder inspection is characterized by comprising the following steps:
step 1, observing the shape and size of a defect under magnetic particle inspection, and recording the position of the defect;
step 2, cutting a normal sample and a defect sample, carrying out microscopic structure analysis, judging the samples to be metallurgical defects, and carrying out step 3;
step 3, carrying out oxidation phenomenon analysis on the corrosion state defect sample, judging non-oxidation loss, and carrying out step 4;
and 4, analyzing the microstructure components of the corrosion state defect sample.
2. The method for detecting the 35NCD16 alloy magnetic particle inspection defect according to claim 1, wherein the step 2 is implemented by the following steps:
step 2.1, polishing the normal sample and the defect sample to obtain a polished normal sample and a polished defect sample;
step 2.2, observing the polished defect sample under a 100X optical microscope;
step 2.3, if other abnormal defects exist near the defects, the defects are caused by the abnormal defects, step 2.4, if other abnormal defects do not exist near the defects and the content of the non-metallic inclusions near the defects exceeds the standard requirement, the defects are cracks caused by the superscript content of the non-metallic inclusions,
and 2.5, if no other abnormal defects exist near the defect and the content and distribution of the non-metallic inclusions near the defect are basically uniform and consistent with those of the polished normal sample, determining that the defect belongs to a metallurgical defect, and then analyzing the oxidation phenomenon to determine that the defect belongs to the metallurgical defect type.
3. The method for detecting the 35NCD16 alloy magnetic particle inspection defect according to claim 2, wherein the step 3 is implemented by the following steps:
step 3.1, grinding and polishing the normal sample and the defect sample, and corroding the normal sample and the defect sample by using a corrosive to obtain a corrosion state defect sample;
and 3.2, observing under a 100X optical microscope, wherein if an oxidation phenomenon occurs near the defect and the oxide film remains, the defect is formed when the oxide film is rolled into the liquid metal, and if no oxidation phenomenon exists, the step 4 is carried out.
4. The method for 35NCD16 alloy magnetic particle inspection defect detection according to claim 3, wherein the etchant of step 3.1 is 4% nital.
5. The method for detecting the defects of the 35NCD16 alloy magnetic particle inspection according to claim 3, wherein the step 4 is implemented by the following steps:
step 4.1, performing energy spectrum analysis on the polished defect sample, and performing energy spectrum analysis on metal components of compounds around and inside the defect;
4.2, analyzing the metal component and main element composition of compounds around and inside the defect, and comparing the metal component and the main element composition with the components of the molten slag added in the smelting process;
and 4.3, if the components of the slag added in the smelting of the granular compounds are consistent, the defect is slag inclusion formed by incomplete smelting of the added slag in the smelting process, otherwise, the defect is not.
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CN114578015B (en) * | 2022-04-12 | 2024-02-13 | 安徽龙磁金属科技有限公司 | Intelligent quality detection method for soft magnetic ferrite |
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