CN105445185B - The method of the second distributed mutually of segregation uniformity in accurate determination of material - Google Patents

The method of the second distributed mutually of segregation uniformity in accurate determination of material Download PDF

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CN105445185B
CN105445185B CN201410428916.7A CN201410428916A CN105445185B CN 105445185 B CN105445185 B CN 105445185B CN 201410428916 A CN201410428916 A CN 201410428916A CN 105445185 B CN105445185 B CN 105445185B
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phase
segregation
uniformity
sample
distributed
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CN105445185A (en
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李阁平
张利峰
李明远
王练
彭胜
吴松全
高博
顾恒飞
庞丽侠
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Institute of Metal Research of CAS
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Abstract

The method of the second distributed mutually of segregation uniformity in accurate determination of material;Second phase is abstracted into mass concentration in the particle at center by it;The uniformity degree of second phase in the base is embodied followed by mathematical method is quantitative, numeralization;Then mathematical method is written as program, user only needs, in terminal input coordinate data, can directly obtain uniformity results;End user summarizes acquired results together, is organized into chart.The present invention overcomes the existing methods using sxemiquantitative to analyze metallographic and a large amount of statistical work, on the basis of random distribution the second phase statistical method, for with segregation or distribution there is the second phase of directionality to be evenly distributed in the base sex chromosome mosaicism, proposes a kind of the second phase of characterization segregation that new method can be quantitatively distributing homogeneity in the base.It is more objective, easy, accurate to have the characteristics that, and there is no limit to the numbers of particles of metallographic visual field.

Description

The method of the second distributed mutually of segregation uniformity in accurate determination of material
Technical field
The utility model belongs to technical field of metallographic detection, and in particular to the second phase of segregation point in a kind of accurate determination of material The method of cloth uniformity.
Background technology
The space distribution situation of second phase in the base can qualitatively be divided into be uniformly distributed, random distribution, segregation distribution three A type, wherein segregation distribution be segmented into aggregation it is agglomerating, be gathered into line and be gathered into the multiple types such as face (layered distribution), such as Shown in Fig. 1-4.
In practical structures and functional material, the second phase is distributed in the base to be less able to according to uniform sequential shown in Fig. 1 Distribution, and most of second phase is distributed in random or segregation state in matrix in the base.For example, at mild steel annealing After reason, the second phase is all to be randomly distributed in matrix;Fiber cross-sectional is distributed random distribution in matrix in fibre reinforced composites, As shown in Figure 2;After the heat treatment of (alpha+beta) biphase titanium alloy, the second phase is agglomerating around primary alpha phase boundary segregation;Titanium alloy, high temperature Alloy powder through hydrostatic profile and heat treatment after the second phase around initial boundary forming core, grow up, and segregation initial boundary week It encloses, as shown in Figure 3;To cold drawing wirework, processing streamline is distributed in the axial direction;α or (alpha+beta) titanium alloy are through monophase field Quenching and temper after, the second phase mainly in lath interface forming core, magnify, and on lath interface segregation be distributed, such as Fig. 3 institutes Show.
For the second phase of random distribution in material matrix, relevant work has been unfolded in many researchers, still The problem of for the second phase of segregation, there are no provide direct method to be counted and described.In conjunction with the experiment item of oneself Part, distributing homogeneity has carried out the description of system to affiliated the second phase of scientific research task group pair of inventor in the base.Previous《It measures The method of transgranular second phase distributing homogeneity in the base》In patent application document, the agglomerating phenomenon of segregation can be solved, but The phenomenon that segregation is agglomerated into line cannot be counted.
For previous deficiency, it is intended that obtaining other methods to describe the second phase with second of segregation phenomenon.
Invention content
The object of the present invention is to provide a kind of the second phases of quantitative determination segregation that technique effect is excellent to be distributed in the base The method of even property.
The method of the second distributed mutually of segregation uniformity in accurate determination of material of the present invention;It is characterized in that:Second phase is taken out As at particle;The quantitative uniformity degree materialization by the second phase in the base, numeralization are gone followed by mathematical method; Then mathematical method is written as program, user only needs, in terminal input data, can directly obtain desired result.Most Whole user summarizes the result that program obtains together, is organized into chart.It can intuitively reflect material using chart data In the second phase distributing homogeneity degree.
The requirement of the method for the second distributed mutually of segregation uniformity is in the accurate determination of material:Institute first in acquisition field of view There is the centre coordinate of the second phase of matrix, the second phase uniformity results in the base are then calculated according to coordinate information.
In the accurate determination of material in the method for the second distributed mutually of segregation uniformity, statistical indicator is to measure to regard in two dimension Each Second Phase Particle is closest, secondary closest or other require the spacing and each second phase of the second phase with its in Grain is closest, secondary closest or other require the slope of the second phase with its, then comprehensive analysis;Specific requirement is as follows successively:
First, metallographic sample and metallographic observation are prepared;Metallographic sample surface requirements:Contrast is clearly demarcated, and contour line is clearly uniform, Flatness, cleanliness factor, uniformity will be got well;
Then, each Second Phase Particle centre coordinate in visual field is obtained using Metallographic Analysis software or image analysis software (Xi Yi), and each coordinate value is saved in text file;
Finally, according to each Second Phase Particle centre coordinate (X in visual fieldi Yi), the second phase of measurement write using me Above-mentioned text file need to only be copied in the text file of requirement, is calculated in this visual field by the software of distributing homogeneity Average nearest, secondary nearest or other definition spacing of all second phase particles in two dimensional surfaceWith corresponding standard deviationt, together When provide the slope y ' of each Second Phase Particle closest, secondary closest second phase with its, and slope is converted into x-axis just The angle theta in direction;
By integrating the data under all visual fields, makeAnd σtWith the chart of sample position, the second phase of reflection is entire two The uniformity of dimension space distribution;Numbers of particles/the percentage composition in different angle theta sections is made with the change curve of angle theta, reflection Second phase, which whether there is, segregation phenomenon.
The requirement for preparing metallographic sample and metallographic observation is as follows:
1) sample is chosen:To enable measurement data really to reflect, truth value, same material really have generation at it The position of table selects 3-5 parallel sample, including at the end point of sample, center and at 1/2;It is uniform to alloy structure The larger alloy of gender gap should increase the number of sample or make special statistics and calculating to uneven position;There is side to tissue The material selection of tropism is hung down perpendicular and parallel in the oriented flour milling for organizing direction plane as metallographic specimen;
2) sample grinding and polishing:After being cut to sample wire cutting, 150#, 320#, 800#, 2000# abrasive paper for metallograph mill are used in surface successively Then light uses the silicon dioxide polishing solution that granularity is 50 μm to polish
3) sample corrodes:Etching pit method is specially one of the following or a combination thereof:Chemical corrosion method, electrochemistry are rotten Erosion method, decoration method.In order to improve the accuracy of measurement data, in etching pit, not only to show respectively organized in alloy it is thin Section and feature also want the contrast of each tissue display clearly demarcated, and contour line is clearly uniform, the flatness of entire sample, cleanliness factor, uniformly Property will be got well.
4) Storage of sample:After the completion of etching pit, sample surfaces are rinsed well with deionized water and absolute ethyl alcohol successively, Cool breeze dries up, and is then sealed.
5) metallographic observation:For the same metallographic specimen, all kinds of representative measurement field positions should be chosen, are specifically included Sample marginal position, center;And randomness and statistics should be had by measuring visual field, be ensured in visual field comprising more than 100 A second phase particles.Specifically metallographic observation method is:It is bright field illumination, oblique illumination, dark-ground illumination, polarised light, interference technique, glimmering Light microtechnic, ultraviolet light microtechnic.
In the accurate determination of material in the method for the second distributed mutually of segregation uniformity, under the second phase uniformity meets State requirement:
1) metallograph is converted into gray level, adjusts contrast difference between the second phase and matrix so that the profile of the second phase Line is apparent, and contrast is clearly demarcated;
2) each Second Phase Particle geometric center in visual field is obtained using Metallographic Analysis software or common image analysis software Coordinate (Xi Yi), and each coordinate value is saved in text file;
3) above-mentioned text file is copied to and is required in file, you can obtain the flat of all second phase particles in this visual field It is nearest, secondary recently or other specify SpacingWith corresponding standard deviationt
4) closest, secondary neighbouring under each visual field or other two desired particles slopes are calculated, and slope is converted into With the angle theta of positive direction of the x-axis;
5) data for combining other visual fields to obtain, all spacingAnd standard deviationtData are made a two dimension folding Line chart, the wherein numerical value of standard deviation can reflect the uniformity of the second phase local distribution in the base, and average headway is with visual field The variation of chosen position can reflect the uniformity that the second phase is distributed in entire material;
Be evenly distributed in the second phase matrix sex chromosome mosaicism for the second phase being distributed with segregation, can byAnd σtTwo On the basis of tieing up line chart, the numbers of particles/percentage composition in different angle theta sections is made with the change curve of angle theta, two groups of numbers According to be combineding with each other, the second phase with segregation phenomenon can be characterized;
For different angle theta sections numbers of particles/ratio with angle theta change curve, if the second phase is in material base Random distribution in body, then curve can be approximately horizontal line, show that the second distributed mutually is evenly distributed in different directions;If the second phase Segregation is distributed in material matrix, then several maximum occurs in curve, shows that the second phase has segregation in extreme value place direction Phenomenon, and segregation degree is characterized by the size of Curve Maximization, number;
The mathematical method used in the method for the second distributed mutually of segregation uniformity in the accurate determination of material is as follows:
The formula of Second Phase Particles spacing t:
Average arest neighbors Second Phase Particles spacingFormula:
The standard deviation of arest neighbors Second Phase Particles spacingtFormula:
The slope y ' of arest neighbors Second Phase Particles spacing:
Wherein (x1,y1) and (x2,y2) distribution be Second Phase Particles 1 and 2 position coordinates;t1:In visual field and the second phase matter The particle spacing of 1 arest neighbors of point, t2、t3、…tNSuch as t1;N:One shares N number of Second Phase Particles.
Advantages of the present invention:This method overcomes the existing method using sxemiquantitative to analyze metallographic and a large amount of statistics work Make, on the basis of random distribution the second phase statistical method, for segregation or distribution with the second phase of directionality in matrix In be evenly distributed sex chromosome mosaicism, propose a kind of the second phase of characterization segregation that new method can quantify distributing homogeneity in the base.Tool There have the characteristics that be more objective, easy, accurate, and there is no limit to the numbers of particles of metallographic visual field.
Description of the drawings
Below in conjunction with the accompanying drawings and embodiment the present invention is described in further detail:
Fig. 1 is the second phase equally distributed schematic diagram in the base;
Fig. 2 is the schematic diagram of the second phase random distribution in the base;
Fig. 3 is the second phase pockets of schematic diagram of segregation in the base;
Fig. 4 be the second phase in the base segregation at line schematic diagram;
Fig. 5 is the distribution map of the second phase of spherical graphite in spheroidal graphite cast-iron;
Fig. 6 is the average headway of the second phase of arest neighbors spherical graphite in spheroidal graphite cast-iron with the change curve of sample position;
Fig. 7 be spheroidal graphite cast-iron in cross arest neighbors the second phase of graphite straight line from the angle of X-axis positive direction in different angle theta areas Between percentage composition with angle theta change curve;
Fig. 8 is the second phase when being uniformly distributed, the percentage composition in different angle theta sections with angle theta change curve;
When Fig. 9 is that the second skew is polymerized to, the percentage composition in middle difference angle theta section with angle theta change curve Figure 10 When being polymerized to line for the second skew, the percentage composition in different angle theta sections with angle theta change curve;
Figure 11 is the linear distribution map of Zr-Nb alloys second phase after deformation and heat treatment;
Figure 12 is the average headway of the second phase of arest neighbors in Zr-Nb alloys with sample position change curve;
Figure 13 is shown in Figure 11 in the second phase, in different angle theta sections, the percentage composition of the second phase with angle theta variation Curve.
Specific implementation mode
Embodiment 1
The method of the second distributed mutually of segregation uniformity in the present embodiment accurate determination of material:The matter that second phase is abstracted into Point;The quantitative uniformity degree materialization by the second phase in the base, numeralization are gone followed by mathematical method.
The requirement of the method for the second distributed mutually of segregation uniformity is in the accurate determination of material:Institute first in acquisition field of view There is the centre coordinate of the second phase of matrix, the second phase uniformity results in the base are then calculated according to coordinate information.
In the accurate determination of material in the method for the second distributed mutually of segregation uniformity, statistical indicator is to measure to regard in two dimension Each Second Phase Particle is closest, secondary closest or other require the spacing and each second phase of the second phase with its in Grain is closest, secondary closest or other require the slope of the second phase with its, then comprehensive analysis;Specific requirement is as follows successively:
First, metallographic sample and metallographic observation are prepared;
Then, analysis obtains each Second Phase Particle centre coordinate (X in visual fieldi Yi), and each coordinate value is preserved;
Finally, according to each Second Phase Particle centre coordinate (X in visual fieldi Yi), it is calculated all in this visual field Average nearest, secondary nearest or other definition spacing of Secondary phase particle in two dimensional surfaceWith corresponding standard deviationt, provide simultaneously Each Second Phase Particle is closest, secondary closest or other require the slope y ' of the second phase with its, and slope is converted into and x The angle theta of axis positive direction;
By integrating the data under all visual fields, makeAnd σtWith the chart of sample position, the second phase of reflection is entire two The uniformity of dimension space distribution;Numbers of particles/the percentage composition in different angle theta sections is made with the change curve of angle theta, reflection Second phase, which whether there is, segregation phenomenon.
The requirement for preparing metallographic sample and metallographic observation is as follows:
1) sample is chosen:To enable measurement data really to reflect, truth value, same material really have generation at it The position of table selects 3-5 parallel sample, including at the end point of sample, center and at 1/2;It is uniform to alloy structure The larger alloy of gender gap should increase the number of sample or make special statistics and calculating to uneven position;Have to tissue The material of directionality selects the perpendicular and parallel flour milling in oriented tissue direction plane as metallographic specimen that hangs down;
2) sample grinding and polishing:After being cut to sample wire cutting, 150#, 320#, 800#, 2000# abrasive paper for metallograph mill are used in surface successively Then light uses the polishing fluid that granularity is 50 μm to polish;
3) sample corrodes:Etching pit method is specially one of the following or a combination thereof:Chemical corrosion method, electrochemistry are rotten Erosion method, decoration method;
4) Storage of sample:After the completion of etching pit, sample surfaces are rinsed well with deionized water and absolute ethyl alcohol successively, Cool breeze dries up, and is then sealed;
5) metallographic observation:For the same metallographic specimen, all kinds of representative measurement field positions should be chosen, are specifically included Sample marginal position, center;And randomness and statistics should be had by measuring visual field, be ensured in visual field comprising more than 100 A second phase particles.Specifically metallographic observation method is:It is bright field illumination, oblique illumination, dark-ground illumination, polarised light, interference technique, glimmering Light microtechnic, ultraviolet light microtechnic.
In the accurate determination of material in the method for the second distributed mutually of segregation uniformity, under the second phase uniformity meets State requirement:
1) metallograph is converted into gray level, adjusts contrast difference between the second phase and matrix so that the profile of the second phase Line is apparent, and contrast is clearly demarcated;
2) each Second Phase Particle geometric center in visual field is obtained using Metallographic Analysis software or common image analysis software Coordinate (Xi Yi), and each coordinate value is saved in text file;
3) above-mentioned text file is copied to and is required in file, you can obtain the flat of all second phase particles in this visual field It is nearest, secondary recently or other specify SpacingWith corresponding standard deviationt
4) closest, secondary neighbouring under each visual field or other two desired particles slopes are calculated, and slope is converted into With the angle theta of positive direction of the x-axis;
5) data for combining other visual fields to obtain, all spacingAnd standard deviationtData are made a two dimension folding Line chart, the wherein numerical value of standard deviation can reflect the uniformity of the second phase local distribution in the base, and average headway is with visual field The variation of chosen position can reflect the uniformity that the second phase is distributed in entire material;
Be evenly distributed in the second phase matrix sex chromosome mosaicism for the second phase being distributed with segregation, byAnd σtTwo dimension folding On the basis of line chart, the numbers of particles/percentage composition in different angle theta sections is made with the change curve of angle theta, two groups of data phases It mutually combines, the second phase with segregation phenomenon can be characterized;
For different angle theta sections numbers of particles/ratio with angle theta change curve, if the second phase is in material base Random distribution in body, then curve can be approximately horizontal line, show that the second distributed mutually is evenly distributed in different directions;If the second phase Segregation is distributed in material matrix, then several maximum occurs in curve, shows that the second phase has segregation in extreme value place direction Phenomenon, and segregation degree is characterized by the size of Curve Maximization, number;
The mathematical method used in the method for the second distributed mutually of segregation uniformity in the accurate determination of material is as follows:
The formula of Second Phase Particles spacing t:
Average arest neighbors Second Phase Particles spacingFormula:
The standard deviation of arest neighbors Second Phase Particles spacingtFormula:
The slope y ' of arest neighbors Second Phase Particles spacing:
Wherein (x1,y1) and (x2,y2) distribution be Second Phase Particles 1 and 2 position coordinates;t1:In visual field and the second phase matter The particle spacing of 1 arest neighbors of point, t2、t3、…tNSuch as t1;N:One shares N number of Second Phase Particles.
The advantages of the present embodiment:This method overcomes the existing method using sxemiquantitative to analyze metallographic and a large amount of statistics Work, on the basis of random distribution the second phase statistical method, for segregation or distribution with the second phase of directionality in base Be evenly distributed sex chromosome mosaicism in body, proposes a kind of the second phase of characterization segregation that new method can quantify distributing homogeneity in the base. It is more objective, easy, accurate to have the characteristics that, and there is no limit to the numbers of particles of metallographic visual field.
Embodiment 2
The present embodiment content is substantially the same manner as Example 1, the difference is that:
It is specifically in spheroidal graphite cast-iron the second phase of graphite be evenly distributed in the base sex chromosome mosaicism;Referring to attached drawing 5-10;Specifically Description is as follows:
The visual field for choosing 10 different locations in the sample, shoots metallograph.And metallograph is converted into gray scale Grade adjusts contrast difference between the second phase and matrix.Then it is obtained in visual field in each Second Phase Particle using image analysis software Heart coordinate (Xi Yi), and coordinate value is saved in the file of " coordinate file .txt " (with space or carriage return between coordinate X, Y Key separates).Finally operation program can be obtained average nearest, the secondary nearest spacing of all second phase particles in each visual field With corresponding standard deviationt, and the straight slope of two particles is corresponded to excessively, and slope is converted into the angle theta with positive direction of the x-axis. All visual fields are obtained、σtWith θ data summarizations to together, being organized into chart respectively such as Fig. 6 and Fig. 7.Wherein, Fig. 6 gives The change curve that graphite the second phase average arest neighbors spacing changes with standard deviation with sample position, and this partial content is special Profit《A method of accurately measuring transgranular second phase distributing homogeneity in the base》In be described later in detail;Fig. 7 gave The angle theta of the straight line and X-axis positive direction of the second phase of arest neighbors graphite, and percentage shared by the Second Phase Particle of different angle thetas section contain Measure the change curve with angle, θ.From figure 7 it can be seen that within the scope of different angle the content of the second phase between 4%~7%, This is also demonstrated when the second phase of graphite is distributed in the base from side close to uniform.
From above-mentioned analysis result it is found that when the second phase be distributed in the base close to it is uniform when, from arest neighbors the second phase spacing Angle and be consistent from the analysis result of the angle with X-axis positive direction angle.But when the second distributed mutually in Fig. 1, Fig. 3 and When shown in Fig. 4, if only cannot comprehensively, accurately analyze the second distributed mutually from the angle analysis of arest neighbors the second phase spacing Uniformity coefficient, this just needs further to analyze from the angle with X-axis positive direction angle.Fig. 8, Fig. 9 and Figure 10 are set forth (as shown in Figure 3) and segregation are different at (as shown in Figure 4) when line when (as shown in Figure 1), segregation are agglomerating when the second phase regular distribution Percentage composition shared by the Second Phase Particle of angle theta section with angle, θ change curve.From figure 8, it is seen that all arest neighbors For second phase on 0 ° and 90 ° of directions, this is corresponding with Fig. 1;From fig. 9, it can be seen that the distribution of the second phase of arest neighbors Direction regularity is not strong, is all distributed in all directions;From fig. 10 it can be seen that the second phase of all arest neighbors is at 30 ° Segregation on~90 ° of directions.
Embodiment 3
The present embodiment content is substantially the same manner as Example 1, the difference is that:
It is specifically the sex chromosome mosaicism that is evenly distributed that Zr-Nb alloys segregation after deformation and heat treatment analyzes the second phase;Referring to Attached drawing 11-13;It is as follows to illustrate content:
The visual field for choosing 5 different locations in the sample, shoots electron scanning micrograph.And photo is converted into Gray level adjusts contrast difference between the second phase and matrix.Then each second phase in visual field is obtained using image analysis software Grain centre coordinate (Xi Yi), and coordinate value is saved in the file of " coordinate file .txt " (between coordinate X, Y with space or Enter key separates).Finally operation program can be obtained all second phase particles in each visual field it is average it is nearest, secondary recently between Away fromWith corresponding standard deviationt, and excessively corresponding two particles straight slope, and slope data is converted into and positive direction of the x-axis Angle theta.All visual fields are obtainedσtWith θ data summarizations to together, being organized into chart respectively such as Figure 12 and Figure 13.Its In, Figure 12 gives the change curve that graphite the second phase average arest neighbors spacing changes with standard deviation with sample position, and The data analysing method is in patent《A method of accurately measuring transgranular second phase distributing homogeneity in the base》In have in detail Analytical mathematics.Figure 13 gives percentage composition shared by the Second Phase Particle of different angle theta sections with the change curve of angle, θ.From Figure 12 data can be seen that the second distributed mutually uniformity is preferable, and the second distributed mutually segregation is smaller on various sample position, but this and figure Second distributed mutually figure result is inconsistent in 11, therefore for there is the analysis of the second distributed mutually uniformity of linear segregation needs to borrow Change curve shown in Figure 13 is helped intuitively to show.As can be seen from Figure 13, the second phase is mainly inclined on direction between -20 °~20 ° It is poly-, and be distributed in the other direction less.It is linear segregation, segregation angle that this also demonstrates the second phase and be distributed in the base from side Degree is between ± 20 °.

Claims (3)

1. the method for the second distributed mutually of segregation uniformity in accurate determination of material;It is characterized in that:Second phase is abstracted into quality Concentrate on the particle at center;The uniformity degree of second phase in the base is embodied followed by mathematical method is quantitative, Numeralization;Then mathematical method is written as program, user only needs, in terminal input coordinate data, can directly obtain Even property result;End user summarizes acquired results together, is organized into chart;
The requirement of the method for the second distributed mutually of segregation uniformity is in the accurate determination of material:All bases first in acquisition field of view Then the uniformity results of the second phase in the base are calculated according to coordinate information in the centre coordinate of the second phase of body;
In the accurate determination of material in the method for the second distributed mutually of segregation uniformity, statistical indicator is measured in two-dimensional field of view Each Second Phase Particles is closest, secondary closest or other require the spacing and each second phase matter of Second Phase Particles with its Point is closest with it, secondary closest or other require the slopes of Second Phase Particles, then comprehensive analysis;Specific requirement is successively such as Under:
First, metallographic sample and metallographic observation are prepared;
Then, each Second Phase Particles centre coordinate (X in visual field is obtained using Metallographic Analysis software or image analysis softwarei Yi), and each coordinate value is stored in text file;
Finally, according to each Second Phase Particles centre coordinate (X in visual fieldi Yi), utilize the soft of the second distributed mutually uniformity of measurement Part need to only copy to the content in above-mentioned text file in the text file of requirement, and operation program is calculated this and regards Average nearest, secondary nearest or other requirements spacing of all Second Phase Particles in two dimensional surface inWith corresponding standard deviation Poor σt, while the slope y ' of each Second Phase Particles closest Second Phase Particles closest with it, secondary is provided, and slope is turned Change the angle theta with positive direction of the x-axis into;
By integrating the data under all visual fields, makeAnd σtWith the chart of sample position, the second phase of reflection is empty in entire two dimension Between the uniformity that is distributed;Particle number/the percentage composition in different angle theta sections is made with the change curve of angle theta, with intuitive Reflect the second phase with the presence or absence of there is segregation phenomenon.
2. according to the method for the second distributed mutually uniformity of segregation in accurate determination of material described in claim 1, it is characterised in that:System The requirement of standby metallographic sample and metallographic observation is as follows:
1) sample is chosen:To enable measurement data really to reflect, truth value, same material are really representative at it Position select 3-5 parallel sample, including at the end point of sample, center and at 1/2;According to the uniform of alloy structure Property increase sample number or special statistics and calculating are made to uneven position;Have directive material, selection to tissue Hang down the perpendicular and parallel flour milling in oriented tissue direction plane as metallographic specimen;
2) sample grinding and polishing:After sample wire cutting, surface uses 150#, 320#, 800#, 2000# abrasive paper for metallograph to polish successively, then The silicon dioxide polishing solution for being 50 μm with granularity polishes;
3) sample corrodes:Caustic solution is specially one of the following or a combination thereof:Chemical corrosion method, electrochemical erosion method, dye Color method;In order to improve the accuracy of measurement data, in etching pit, the details respectively organized in alloy and spy are not only shown Sign also wants the contrast of each tissue display clearly demarcated, and contour line is clearly uniform, and flatness, cleanliness factor, the uniformity of entire sample will It is good;
4) Storage of sample:After the completion of etching pit, sample surfaces are rinsed well with deionized water and absolute ethyl alcohol successively, cool breeze Drying, is then sealed;Metallographic surface oxidation or contaminated is prevented, metallography microscope sem observation is used in combination;
5) metallographic observation:For the same metallographic specimen, sample marginal position, center are chosen;And measuring visual field should have There are randomness and statistics, selects amplification factor to ensure in visual field comprising more than 100 second phase particles;In addition, in order to carry Contrast difference between high two-phase, specific metallographic observation method are:Bright field illumination, dark-ground illumination, polarised light, is done oblique illumination Relate to technology, fluorescence microscopy, ultraviolet light microtechnic.
3. according to the method for the second distributed mutually uniformity of segregation in accurate determination of material described in claims 1 or 2, feature exists In:In the accurate determination of material in the method for the second distributed mutually of segregation uniformity, the second phase uniformity meets following want It asks:
1) metallograph is converted into gray level, adjusts contrast difference between the second phase and matrix so that the contour line of the second phase is bright Aobvious, contrast is clearly demarcated;
2) each Second Phase Particles Geometric center coordinates in visual field are obtained using Metallographic Analysis software or common image analysis software (Xi Yi), and each coordinate value is saved in text file;
3) above-mentioned text file is copied to and is required in file, you can obtain all Second Phase Particles in this visual field it is average most Closely, secondary nearest or other requirements spacingWith corresponding standard deviationt
4) it calculates closest, secondary neighbouring under each visual field or other two desired particles slopes, and slope is converted into and x-axis The angle theta of positive direction;
5) data for combining other visual fields to obtain, all spacingAnd standard deviationtData are made a two-dimentional line chart, Wherein the numerical value of standard deviation can reflect that the uniformity of the second phase local distribution in the base, average headway choose position with visual field The variation set can reflect the uniformity that the second phase is distributed in entire material;
Be evenly distributed in the second phase matrix sex chromosome mosaicism for the second phase being distributed with segregation, byAnd σtTwo-dimentional line chart On the basis of, the particle number/percentage composition in different angle theta sections is made with the change curve of angle theta, and two groups of data are mutually tied It closes, the second phase with segregation phenomenon can be characterized;
For different angle theta sections particle number/ratio with angle theta change curve, if the second phase is in material matrix Random distribution, then curve approximation is horizontal line, shows that the second distributed mutually is evenly distributed in different directions;If the second phase is in material Segregation is distributed in matrix, then several maximum occurs in curve, shows that the second phase has segregation phenomenon in extreme value place direction, and And segregation degree is characterized by the size of Curve Maximization, number;
The mathematical method used in the method for the second distributed mutually of segregation uniformity in the accurate determination of material is as follows:
The formula of Second Phase Particles spacing t:
Average arest neighbors Second Phase Particles spacingFormula:
The standard deviation of arest neighbors Second Phase Particles spacingtFormula:
The slope y ' of arest neighbors Second Phase Particles spacing:
Cross the angle theta between the straight line and horizontal line of two Second Phase Particles of arest neighbors:θ=arctany,
Wherein (x1,y1) and (x2,y2) be respectively Second Phase Particles 1 and 2 position coordinates;t1:In visual field most with Second Phase Particles 1 The particle spacing of neighbour, t2、t3、…tNSuch as t1;N:One shares N number of Second Phase Particles.
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