CN107976459A - The analyzing detecting method of two-phase proportion in a kind of two phase stainless steel as-cast structure - Google Patents
The analyzing detecting method of two-phase proportion in a kind of two phase stainless steel as-cast structure Download PDFInfo
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Abstract
The present invention relates to a kind of analyzing detecting method of two-phase proportion in two phase stainless steel as-cast structure, belong to Analysis of Metallic Materials field, be applied particularly to the accurate measure of ferrite and austenite phase content in two phase stainless steel as-cast structure.The present invention electrobrightening 20s~30s destressing layers, voltage 10V~20V, electric current 1A~2A in the perchloric acid alcoholic solution that volume fraction is 10%~20%.The analysis sample to be detected prepared, and two distributed mutuallies are determined according to each mutually special Kikuchi style that EBSD analysis systems possess, it is no longer limited by being difficult to the artificial corrosion's dyeing held, it is not obvious so that being difficult to differentiate between enough avoids contrast between causing each phase because of corrosive effect difference;Quantitative analysis, and accuracy higher can be carried out to each phase content.
Description
Technical field
The present invention relates to a kind of analyzing detecting method of two-phase proportion in two phase stainless steel as-cast structure, belong to metal material
Analysis field, is applied particularly to the accurate measure of ferrite and austenite phase content in two phase stainless steel.
Background technology
Ferrite/austenitic duplex stainless steel has the higher-strength of ferritic stainless steel and resistance to chloride stress corrosion concurrently
The advantages that excellent in toughness and weldability of energy and austenitic stainless steel, it is widely used in oil, chemical industry, food, the energy, ship
The fields such as oceangoing ship, building materials, military project.The experimental results show that two-phase proportion is to its mechanical property, corrosion resistance in two phase stainless steel
There can be material impact with processing performance, therefore it is most important accurately to measure its two-phase proportion.
Existing analyzing detecting method mainly has chemical analysis-diagrammatical method, method of magnetic and metallographic method.Chemical analysis-diagrammatical method
Measurement accuracy is relatively low, and error is larger.Method of magnetic requires material surface height, relatively low plus accuracy of instrument, causes measurement result smart
True property is poor, and application limitation is larger.Metallographic method is more to be used cooperatively with related softwares such as graphical analyses, and is generally required pair
Sample carries out corrosion treatment, but since corrosive effect is difficult to hold, contrast is not enough substantially difficult between frequently resulting in each phase
Distinguish, be unfavorable for accurate quantitative analysis.
The content of the invention
It is an object of the invention to provide the essence of two-phase proportion in a kind of ferrite/austenitic duplex stainless steel as-cast structure
Quasi- analyzing detecting method, the external world may interfere with that factor is few, and analysis result is accurate, comparativity and favorable reproducibility.
Analyzing detecting method of the present invention includes cutting, grinding, mechanical polishing, electrobrightening, cleaning, analysis detection
Step, wherein, the electrobrightening step is:The electrobrightening in the perchloric acid alcoholic solution that volume fraction is 10%~20%
20s~30s is to remove stressor layers.
Specific cutting, grinding, mechanical polishing, electrobrightening, cleaning operation step are as follows:
(1) sample is intercepted from two-phase stainless steel casting centre by wire cutting, and it is 10mm × 5mm to be processed into specification
The thin slice of × 3mm;
(2) burr and wedge angle of sample are ground off on abrasive machine, and then successively 60Cw, 150Cw, 400Cw, 600Cw,
Sample viewing surface is roughly ground on the sand paper of 800Cw, 1000Cw, 1200Cw, 1500Cw and 2000Cw and fine grinding;
(3) sample viewing surface is mechanically polished using velvet (polishing cloth) and diamond (antiscuffing paste), until reaching
Mirror effect, it is ensured that visually observe without obvious cut;
(4) spot of sample viewing surface is rinsed using the plastic squeeze bottle for holding alcohol, and is dried up with hair-dryer from side direction,
Avoid leaving alcohol and air-dry trace;
(5) electrobrightening 20s~30s destressing layers in the perchloric acid alcoholic solution that volume fraction is 10%~20%,
Voltage 10V~20V, electric current 1A~2A.It is worth noting that, perchloric acid alcoholic solution concentration is too low can not to meet that electricity throws requirement,
Excessive concentration will cause the time to be difficult to hold, and easily cause electricity to be thrown excessive;Electric current can not effectively remove stressor layers, electric current when too low
It is excessive, cause sample viewing surface uneven;
(6) sample is gently swung back and forth in alcohol after clamping electrobrightening with tweezers rapidly, removes specimen surface residual
Thing;
(7) sample is placed in deionized water as early as possible and is cleaned by ultrasonic, more than time 30s, further removes sample table
Face residue;
(8) reuse and hold the plastic squeeze bottle of alcohol and rinse the spot of sample viewing surface, and with hair-dryer from side direction
Drying.
Present invention analysis detecting step is as follows:
(1) sample prepared is put on sample platform of scanning electronic microscope, keeps sample viewing surface horizontal by 70 ° of folders
Angle, accelerating potential 20kV, randomly chooses preferable observation visual field, obtains clearly to be analyzed under being 150 times in amplification factor
The image in region;
(2) selection needs the ferritic phase (body-centered cubic demarcated in EBSD analysis systems:) and austenite phase (face bcc
The heart cube:Fcc the Kikuchi style corresponding to), sets the relevant parameters such as scanning step (5~10 μm), gathers initial data, output
Phase statistics (including each phase area percentage, crystallite dimension, crystal boundary length and grain boundary orientation) and EBSD images (including
Distributed mutually figure, inverse pole figure and crystal boundary distribution map etc.), different thing phases is distinguished by color;
(3) phase point identified according to EBSD is calculated the area percentage composition of ferrite and austenite by software:wαAnd wγ,
And it is w to calculate two-phase proportionα/wγ。
Beneficial effects of the present invention:Compared with prior art, has the following advantages:
1. different colours are presented in ferritic phase and austenite phase in EBSD images, sharpness of border is readily identified;
2. relatively simple electrobrightening technology is used, and each mutually special Kikuchi flower possessed according to EBSD analysis systems
Sample determines two distributed mutuallies, is no longer limited by being difficult to the artificial corrosion's dyeing held, to avoid cause because of corrosive effect difference
Contrast is not obvious so that being difficult to differentiate between enough between each phase;
3. quantitative analysis can be carried out to each phase content, and accuracy higher.
Brief description of the drawings
The two-phase distribution map that Fig. 1 is gathered for the scanned Electronic Speculum of No. 1 sample and EBSD analysis systems in the present invention;(white
Region is austenite, and gray area is ferrite)
The two-phase distribution map that Fig. 2 is gathered for the scanned Electronic Speculum of No. 2 samples and EBSD analysis systems in the present invention.(white
Region is austenite, and gray area is ferrite)
The two-phase distribution map that Fig. 3 is gathered for the scanned Electronic Speculum of No. 3 samples and EBSD analysis systems in the present invention.(white
Region is austenite, and gray area is ferrite, black region None- identified)
Embodiment
Embodiment 1
The analyzing detecting method of two-phase proportion includes in present invention measure ferrite/austenitic duplex stainless steel as-cast structure
Following steps:
Step is 1.:Two-phase stainless steel curved beam is cut successively, is roughly ground, fine grinding and mechanical polishing.It is described to be cut into:Can
Sample is processed using Wire EDM, sample specification is the thin slice of 10mm × 5mm × 3mm;The corase grinding is:Sample
Viewing surface polishes on the sand paper of 60Cw, 150Cw, 400Cw and 600Cw successively, and lubricant is done with water;The fine grinding is:Will be thick
Grind the sample wet-milling on the sand paper of 800Cw, 1000Cw, 1200Cw, 1500Cw and 2000Cw successively;The mechanical polishing is:Will
The good sample of fine grinding is thrown 3~5 minutes on velvet polishing cloth with 2.5 μm of diamond polishing cream is wet, until reach mirror effect,
Ensure to visually observe without obvious cut.
Step is 2.:Electrobrightening is carried out to sample after step 1. middle mechanical polishing, removes stressor layers.The electrobrightening
For:Using the perchloric acid alcoholic solution that volume fraction is 15% as electrolytic polishing liquid, voltage 15V, electric current 1.5A, electricity are thrown
Sample is clamped with tweezers in alcohol gently to swing back and forth, remove specimen surface residue, be subsequently placed at deionization rapidly after 25s
It is cleaned by ultrasonic more than 30s in water, further removes specimen surface residue, finally with alcohol rinse sample viewing surface, and with blowing
Wind turbine is dried up from side direction.
Step is 3.:Sample after step 2. middle electricity throwing is placed on objective table, by scanning electron microscope and EBSD analysis systems, if
Relevant parameter is put, gathers image and data, the output phase statistics and EBSD images.The scanning electron microscopic observation is:Keep examination
For sample viewing surface horizontal by 70 ° of angles, accelerating potential 20kV, preferable see is randomly choosed under being 150 times in amplification factor
Visual field is examined, obtains the image in clearly region to be analyzed;The EBSD is analyzed:Selection needs the ferritic phase (body-centered demarcated
Cube:) and austenite phase (face-centered cubic bcc:Fcc the Kikuchi style corresponding to), sets the ginseng such as scanning step (5~10 μm)
Number, collection initial data, the output phase statistics (including each phase area percentage, crystallite dimension, crystal boundary length and crystal boundary take
To difference) and EBSD images (including distributed mutually figure, inverse pole figure and crystal boundary distribution map etc.), different thing phases is distinguished by color.
Step is 4.:The area percentage of ferrite and austenite is calculated by software according to the step phase point that 3. middle EBSD is identified
Content:wαAnd wγ, and it is w to calculate two-phase proportionα/wγ.It is the scanned Electronic Speculum of No. 1 sample and EBSD in the present invention shown in Fig. 1
The two-phase distribution map that analysis system is gathered, the wherein area percentage shared by ferrite and austenite are respectively:wα=
42.7%, wγ=57.3%, then wα/wγ=0.745.It is that the scanned Electronic Speculum of No. 2 samples and EBSD divide in the present invention shown in Fig. 2
The two-phase distribution map that analysis system is gathered, the wherein area percentage shared by ferrite and austenite are respectively:wα=55.2%,
wγ=44.8%, then wα/wγ=1.232.
Embodiment 2
Consistent, scanning electron microscope and EBSD after electricity is thrown in sample cutting, corase grinding, fine grinding and mechanical polishing process and embodiment 1
It is consistent in analytic process and embodiment 1.Difference is, electrolysis throwing is carried out to sample using the voltage of 10V and the electric current of 1A
Light.It has been observed that specimen surface smoother compared with embodiment 1, the influence unobvious of residual stress layer, still may be used at this time
To carry out effective EBSD analyses, final result is not influenced.
Embodiment 3
Consistent, scanning electron microscope and EBSD after electricity is thrown in sample cutting, corase grinding, fine grinding and mechanical polishing process and embodiment 1
It is consistent in analytic process and embodiment 1.Difference is, electrolysis throwing is carried out to sample using the voltage of 20V and the electric current of 2A
Light.It has been observed that specimen surface is uneven compared with embodiment 1, but still suitable EBSD analyzed areas can be found, no
Influence final result.
Comparative example 1
Consistent, scanning electron microscope and EBSD after electricity is thrown in sample cutting, corase grinding, fine grinding and mechanical polishing process and embodiment 1
It is consistent in analytic process and embodiment 1.Difference is, electrobrightening is carried out to sample using the electric current of 0.5A.Observation hair
It is existing, specimen surface still smoother, the no significant difference compared with after mechanical polishing, but compared with after electricity in embodiment 1 is thrown, it is poor
Away from notable, illustrate to be unable to reach electricity in the electric current short time of 0.5A and skim the effect of de-stress layer, and EBSD analyses are by stress
Layer influences substantially, and as a result accuracy is poor.
Comparative example 2
Consistent, scanning electron microscope and EBSD after electricity is thrown in sample cutting, corase grinding, fine grinding and mechanical polishing process and embodiment 1
It is consistent in analytic process and embodiment 1.Difference is, electrobrightening is carried out to sample using the electric current of 3A.With embodiment 1
Middle electricity is compared after throwing, and specimen surface is uneven to be become apparent from, and substantial amounts of pit-hole occurs, finds suitable EBSD analyzed areas
Difficulty increases, and the black region (as shown in Figure 3) of some None- identifieds occurs in figure, seriously affects the essence of EBSD analysis results
Degree.
Claims (3)
1. the analyzing detecting method of two-phase proportion in a kind of two phase stainless steel as-cast structure, two phase stainless steel as-cast structure is iron element
Body phase and austenite phase, it is characterised in that:Including cutting, grinding, mechanically polishing, electrobrightening, cleaning, analysis detecting step,
Wherein, the electrobrightening step is:Volume fraction be 10%~20% perchloric acid alcoholic solution in electrobrightening 20s~
30s is to remove stressor layers.
2. the analyzing detecting method of two-phase proportion, its feature exist in two phase stainless steel as-cast structure according to claim 1
In:Specific cutting, grinding, mechanical polishing, electrobrightening, cleaning operation step are as follows:
(1) by wire cutting from two-phase stainless steel casting centre intercept sample, and be processed into specification for 10mm × 5mm ×
The thin slice of 3mm;
(2) burr and wedge angle of sample are ground off on abrasive machine, and then successively 60Cw, 150Cw, 400Cw, 600Cw,
Sample viewing surface is roughly ground on the sand paper of 800Cw, 1000Cw, 1200Cw, 1500Cw and 2000Cw and fine grinding;
(3) sample viewing surface is mechanically polished using velvet polishing cloth and diamond polishing cream, until reach mirror effect,
Ensure to visually observe without obvious cut;
(4) spot of sample viewing surface is rinsed using the plastic squeeze bottle for holding alcohol, and is dried up with hair-dryer from side direction, is avoided
Leave alcohol and air-dry trace;
(5) electrobrightening 20s~30s destressing layers, voltage in the perchloric acid alcoholic solution that volume fraction is 10%~20%
10V~20V, electric current 1A~2A;
(6) sample is gently swung back and forth in alcohol after clamping electrobrightening with tweezers rapidly, removes specimen surface residue;
(7) sample is placed in deionized water as early as possible and is cleaned by ultrasonic, more than time 30s, it is residual further to remove specimen surface
Stay thing;
(8) spot for the plastic squeeze bottle flushing sample viewing surface for holding alcohol is reused, and is dried up with hair-dryer from side direction.
3. the analyzing detecting method of two-phase proportion, its feature exist in two phase stainless steel as-cast structure according to claim 1
Include in the analysis detecting step:
1) sample prepared is put on sample platform of scanning electronic microscope, keeps sample viewing surface to accelerate horizontal by 70 ° of angles
Voltage is 20kV, and preferable observation visual field is randomly choosed under 150 times of amplification factor, obtains the figure in clearly region to be analyzed
Picture;
2) the Kikuchi style corresponding to ferritic phase and austenite phase that selection needs are demarcated in EBSD analysis systems, setting are swept
Step-length is retouched as 5~10 μm, gathered data simultaneously exports each phase area percentage, crystallite dimension, crystal boundary length and grain boundary orientation, with
And corresponding distributed mutually figure, inverse pole figure and crystal boundary distribution map;
3) phase point identified according to EBSD is calculated the area percentage composition of ferrite and austenite by software:wαAnd wγ, and calculate
It is w to go out two-phase proportionα/wγ。
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Cited By (8)
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CN108796597A (en) * | 2018-06-06 | 2018-11-13 | 重庆大学 | A kind of Al/Ti cold rolling composite plates electrolytic polishing method |
CN109406238A (en) * | 2018-12-07 | 2019-03-01 | 郑州机械研究所有限公司 | A kind of Multifunctional clamp and metallographic specimen preparation method for metallographic specimen preparation |
CN109900727A (en) * | 2019-03-18 | 2019-06-18 | 中国科学院金属研究所 | A kind of ultralow temperature light current flow control metal material EBSD sample preparation methods |
CN111910244A (en) * | 2020-07-07 | 2020-11-10 | 甘肃酒钢集团宏兴钢铁股份有限公司 | Method for preparing duplex stainless steel EBSD sample by pulse wave electrolytic polishing |
CN112229860A (en) * | 2020-08-26 | 2021-01-15 | 东莞材料基因高等理工研究院 | Austenitic stainless steel electrolytic polishing method for EBSD test |
CN112730171A (en) * | 2020-12-30 | 2021-04-30 | 成都市海瑞产品质量技术检测有限公司 | Grain size detection method for low-carbon high-alloy material |
CN112906641A (en) * | 2021-03-19 | 2021-06-04 | 北京科技大学 | EBSD metallographic image grain identification method and device |
CN114354321A (en) * | 2021-12-23 | 2022-04-15 | 包头钢铁(集团)有限责任公司 | Method for displaying grain size of high-manganese austenitic steel |
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