CN102331391B - Method for measuring and calculating aggregation and coarsening degree of multi-phase grain in refractory steel - Google Patents
Method for measuring and calculating aggregation and coarsening degree of multi-phase grain in refractory steel Download PDFInfo
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Abstract
The invention discloses a method for measuring and calculating aggregation and coarsening degree of a multi-phase grain in refractory steel. The method comprises the following steps of: (1) finishing, polishing and etching an observation surface of a refractory steel sample to be tested; (2) photographing a plurality of pieces of back scattering electronic pictures of precipitated phases in the sample by using an electron probe or a scanning electron microscope; (3) blackening scales of the obtained back scattering electronic pictures so as to obtain pictures containing no scales; (4) counting pixels (N) included by areas (A) of different light and dark regions of one of the pictures containing no scales and scale normal length (L) by using software Image proplus; (5) calculating sizes ofgrain clusters of different precipitated phases by using A, L and N in the step (4); and (6) repeating the steps (4) and (5) to obtain the sizes of the grain clusters of the different precipitated phases in the series of pictures and taking the average value, namely the actual size of the grain clusters of the different precipitated phases. The measurement and calculation result of the invention is excellently matched with related reports, and is easy to operate and time-saving. The method can be used for important fields of design, breakage, failure analysis and the like of refractory steel.
Description
Technical field
The microstructure that the present invention relates to heat-resisting steel is measured, and specifically, relates to the method for each precipitated phase particle aggregation coarsening rate in the measuring and calculating heat-resisting steel.
Background technology
In order to satisfy the requirement of ultra supercritical thermal power generation unit to the material combination property, heat-resisting steel of new generation (like P92, Super304h etc.) has extensively been applied to the high-temperature component of such boiler.Research shows that the fracture of heat-resisting steel excessively is an intercrystalline fracture by transgranular fracture under hot conditions.This phenomenon shows as on microcosmic: because diffusion is carried out at the crystal boundary place easily; Heat-resisting steel under arms in the process precipitated phase particle of the small and dispersed of crystal boundary punishment cloth can assemble, alligatoring, chaining; Thereby weaken the toughness and tenacity at material crystal boundary place, and finally cause the fracture failure of material; The crystal boundary place that makes of diffusion simultaneously forms easily new precipitated phase, the original precipitated phase reciprocation of new precipitated phase that forms and gathering, alligatoring, chaining, thus influence the toughness and tenacity at material crystal boundary place.Therefore, the degree of precipitated phase particle aggregation alligatoring is all very important to design, exploitation, production, the assessment of ultra supercritical power plant boiler material in the evaluation heat-resisting steel that holds water.At present, the method for heterogeneous particle coarsening rate is not appeared in the newspapers as yet in the measuring and calculating heat-resisting steel; Have only when having unique precipitated phase in the steel, traditional metallographic method can be analyzed its phase particle coarsening rate.Use the metallographic method measuring and calculating to need sample is taken a large amount of metallographs, utilize precipitated phase particle in the related software comparison film painted and calculate the size on the coloured part different directions then, after get the average-size that its mean value is precipitated phase in the sample.The problem of using this method to exist is following: the enlargement factor of (1) metaloscope is lower; And its size of main precipitated phase in the heat-resisting steel generally between tens between the hundreds of nanometers; Therefore under traditional metaloscope, be difficult to observe these less phase particles clearly, more can't calculate its size; (2) when having multiple precipitated phase particle in the material, dissimilar precipitated phases often flock together, and metallograph can not be distinguished it, also can't observe its distribution situation.Therefore, when having multiple precipitated phase particle in the steel and assembling alligatoring, adopt traditional metallographic method can't calculate the coarsening rate of each phase.In order to overcome the above problems, this method is distinguished different precipitated phase particles in the steel through backscattered electron image, characterizes the situation of heterogeneous particle aggregation alligatoring in the steel according to the size of cluster of particle.How to make in the heat-resisting steel the quantitative measuring and calculating of heterogeneous cluster of particle size accomplish accurate, easy, to save time be a key of the present invention.
Summary of the invention
The object of the present invention is to provide each precipitated phase particle in a kind of heat-resisting steel to assemble the measuring method of coarsening rate mutually, this method results of measuring is accurate, easy and simple to handle, save time.
The objective of the invention is to realize like this: at first by conventional metallographic sample preparation method with the polishing of tested sample sightingpiston, polishing and etch; Select the backscattered electron imaging pattern down at electron probe (EPMA) or surface sweeping Electronic Speculum (SEM) then, under 2000 ~ 5000 times enlargement ratio, take the backscattered electron photo of precipitated phase in the sample, the captured number of pictures of each sample is no less than 5; Thereby the photo that the scale blacking of gained backscattered electron photo is not contained scale; Utilize image quantitation software Image pro plus to count the pixel light and shade distribution plan of one of above-mentioned gained photo (establish it and be numbered 1), this figure is divided into matrix region m and precipitated phase zone a, b ....Wherein, the crest number R in the pixel light and shade distribution plan is the precipitated phase number, and R is followed successively by 1 from right to left; 2 ... R, the corresponding crest 1 of a is with the zone on the right side; The corresponding crest 1 of b, the zone between 2 ..., the zone between the flex point A of corresponding crest R-1 of last precipitated phase and crest R right flank; The A point is the matrix region with a left side; Calculate the area A in each precipitated phase zone then
A1, A
B1..., unit is a pixel, wherein the captured photo of subscript 1 expression sample is numbered 1; In addition, measure the number of pixels N that the nominal length L of scale is comprised in photo; Area A according to each the precipitated phase zone that is obtained
A1, A
B1And formula
Calculate the equivalent size L of different precipitated phase cluster of particles in the steel
A1, L
B1, unit is a pixel, utilizes formula then
Converse the physical size D of precipitated phase cluster of particle
A1, D
B1, wherein,
K=a, bRepresent precipitated phases different in the sample; Other photos are repeated above-mentioned steps, thereby obtain the physical size D of different precipitated phase cluster of particles in the serial-gram
A2, D
B2, D
A3, D
B3, the numbering of the captured photo of subscript 2,3 expression samples; Calculate D then
A1, D
A2, D
A3, D
B1, D
B2, D
B3Mean value, gained is D as a result
a, D
bBe this sample a, b ... The average-size of precipitated phase cluster of particle.
The inventive method results of measuring is accurate, easy and simple to handle, save time.
Description of drawings
Fig. 1, Fig. 2 are respectively the pixel light and shade distribution plan of 625 ℃ of lasting sample backward scattering photos of P92 steel of certain factory's production;
Fig. 3 is the micro-organization chart of 625 ℃ of lasting samples of P92 steel of this factory's production;
Fig. 4 is the micro-organization chart of 700 ℃ of lasting samples of Super304h steel of certain factory's production;
Fig. 5 is M in the 625 ℃ of lasting samples of P92 steel that obtain with this method measuring and calculating
23C
6With Laves cluster of particle dimensional drawing mutually; Fig. 6 is M in 625 ℃ of lasting samples of P92 steel
23C
6With Laves phase content variation diagram;
Fig. 7 calculates M in the 700 ℃ of lasting samples of Super304h steel that obtain for this method
23C
6Phase cluster of particle dimensional drawing;
Fig. 8 is M in 700 ℃ of lasting samples of Super304h steel
23C
6The phase content variation diagram.
Embodiment
Method of the present invention may further comprise the steps:
1. by conventional metallographic sample preparation method with the polishing of tested sample sightingpiston, polishing, etch;
2. select the backscattered electron imaging pattern down at electron probe (EPMA) or surface sweeping Electronic Speculum (SEM); Under 2000 ~ 5000 times enlargement ratio, take the backscattered electron photo of precipitated phase in the sample; The captured backscattered electron photo of each sample is no less than 5 (in theory, take pictures number more its results accurate more);
Thereby the photo that 3. the scale blacking of gained backscattered electron photo is not contained scale;
4. utilize image quantitation software Image pro plus to count the 3. pixel light and shade distribution plan of one of middle gained photo (establish it and be numbered 1) of step, this figure is divided into matrix region m and precipitated phase zone a, b ...; Wherein, the crest number R in the pixel light and shade distribution plan is the precipitated phase number, and R is followed successively by 1 from right to left; 2 ... R, the corresponding crest 1 of a is with the zone on the right side; The corresponding crest 1 of b, the zone between 2 ..., the zone between the flex point A of corresponding crest R-1 of last precipitated phase and crest R right flank; The A point is the matrix region with a left side; Calculate the area A in each precipitated phase zone then
A1, A
B1..., unit is a pixel, wherein the captured photo of subscript 1 expression sample is numbered 1; In addition, measure the number of pixels N that the nominal length L of scale is comprised in photo;
5. through the regional area A of each precipitated phase in the 4. middle gained backscattered electron photo of step
A1, A
B1And formula
Calculate the equivalent size L of different precipitated phase cluster of particles in the steel
A1, L
B1, unit is a pixel, utilizes formula then
Converse the physical size D of precipitated phase cluster of particle
A1, D
B1, wherein,
K=a, bRepresent precipitated phases different in the sample;
4. and 5. 6. repeating step obtains the physical size D of different precipitated phase cluster of particles in the serial-gram
A2, D
B2, D
A3, D
B3Calculate D then
A1, D
A2, D
A3, D
B1, D
B2, D
B3Mean value, gained is D as a result
a, D
bBe this sample a, b ... The average-size of precipitated phase cluster of particle.
Technical process of the present invention and characteristics thereof:
1. prepare sample
The present invention by conventional metallographic method method of preparing sample to tested sample polish, polishing and etch.
2. microstructure is observed and is taken pictures
Under the backscattered electron imaging pattern of electron probe (EPMA) or ESEM (SEM), the precipitated phase in the sample is observed and taken pictures.Selecting the enlargement ratio of taking pictures for use is 2000 ~ 5000, and each sample is taken a picture to count and is no less than 5.
3. photo is handled
Thereby the photo that the scale blacking of gained backscattered electron photo is not contained scale.
4. distinguish different precipitated phases in the sample
Utilize image quantitation software Image pro plus to count the 3. pixel light and shade distribution plan of one of middle gained photo (establish it and be numbered 1) of step, this figure is divided into matrix region m and precipitated phase zone a, b ...; Wherein, the crest number R in the pixel light and shade distribution plan is the precipitated phase number, and R is followed successively by 1 from right to left; 2 ... R, the corresponding crest 1 of a is with the zone on the right side; The corresponding crest 1 of b, the zone between 2 ..., the zone between the flex point A of corresponding crest R-1 of last precipitated phase and crest R right flank; The A point is the matrix region with a left side; Calculate the area A in each precipitated phase zone then
A1, A
B1..., unit is a pixel, wherein the captured photo of subscript 1 expression sample is numbered 1; In addition, measure the number of pixels N that the nominal length L of scale is comprised in photo.Realize easily the size of its cluster of particle is distinguished and calculated to precipitated phases dissimilar in the heat-resisting steel by method of the present invention, thereby objectively respond the authenticity of each precipitated phase particle aggregation coarsening rate in the steel, this is core of the present invention place.
The present invention proposes, and utilizes image quantitation software Image pro plus to count the pixel light and shade distribution plan of backscattered electron photo, thereby distinguishes dissimilar precipitated phase in the heat-resisting steel.Concrete differentiating method is following:
Because the element of institute's enrichment difference in the different precipitated phases in the steel; Therefore each precipitated phase particle bright-dark degree in the backscattered electron photo is distinguished to some extent: when the element relative atomic mass of institute's enrichment was big in the precipitated phase, its brightness that in the backscattered electron photo, is shown was big more; Otherwise it is then more little.In addition, compare with precipitated phase, the contained heavy metal element of matrix relative scale is minimum, so brightness is the darkest.
Like Fig. 1, shown in 2, in the pixel light and shade distribution plan of sample backward scattering photo, the zones of different in the different precipitated phase corresponding diagram, its separation is flex point A and the crest 2 of precipitated phase of crest 1 right flank of matrix region.Except that matrix m, also have a in the steel, b two precipitated phases, a alpha region are the part that a separates out 1 right side, peak mutually; The b alpha region is the part between crest 1 and the A point; Matrix m is that the A point is with left half.
In like manner, when having more precipitated phases in the steel, the position that can in the pixel light and shade distribution plan of sample backward scattering photo, belong to according to the crest of homophase precipitated phase not and each precipitated phase of position judgment that A is ordered.
5. precipitated phase cluster of particle size calculation
Area A through each precipitated phase zone in the 4. middle gained backscattered electron photo of step
A1, A
B1And formula
Calculate the equivalent size L of different precipitated phase cluster of particles in the steel
A1, L
B1, unit is a pixel, utilizes formula then
Converse the physical size D of precipitated phase cluster of particle
A1, D
B1, wherein,
K=a, bRepresent precipitated phases different in the sample.
6. calculate the mean value of precipitated phase cluster of particle size
4. and 5. repeating step obtains the physical size D of different precipitated phase cluster of particles in the serial-gram
A2, D
B2, D
A3, D
B3Calculate D then respectively
A1, D
A2, D
A3, D
B1, D
B2, D
B3Mean value, gained is D as a result
a, D
bBe this sample a, b ... The average-size of precipitated phase cluster of particle.
Instance:
Instance is 1.: use 625 ℃ of lasting samples of P92 steel to be example with ultra-supercritical boiler.
Fig. 3 is a backscattered electron photo of 625 ℃ of lasting samples of P92 steel.As shown in the figure, the microstructure of sample is the M that distributes on lath martensite matrix and the original austenite crystal prevention
23C
6With Laves particle mutually.Wherein, Laves presents white light tone, M because being rich in heavy element such as W, Mo in mutually
23C
6In be rich in Cr, relatively W, Mo quality are low weight, so gray, matrix is then the darkest.For this method: at first; 1. ~ 3. obtain totally 5 in the backscattered electron photo of tested sample by the practical implementation step, after 4. count the pixel light and shade distribution plan of one of above-mentioned steps gained photo (establish it and be numbered 1) and this figure be divided into M set by step according to distribution plan medium wave peak position with image quantitation software Image pro plus
23C
6, three zones of Laves and matrix m are (respectively to M in should steel
23C
6, two precipitated phases of Laves and matrix), and then calculate M
23C
6Area A with the Laves zone
(M23C6) 1, A
(Laves) 1Simultaneously, measure the number of pixels N that the nominal length L of scale is comprised in photo; Then with M in the 4. middle gained backscattered electron photo of step
23C
6Area A with the Laves zone
(M23C6) 1, A
(Laves) 1Pass through formula
Be scaled the equivalent size L of different precipitated phase cluster of particles in the heat-resisting steel
(M23C6) 1, L
(Laves) 1(unit is a pixel, Pix), utilizes formula again
(
kRepresent precipitated phases different in the steel, in this example
K=(M 23 C 6 ), (Laves))
Calculate the physical size D of precipitated phase cluster of particle
(M23C6) 1, D
(Laves) 1
4. and 5. last repeating step obtains the physical size D of different precipitated phase cluster of particles in other 4 photos
(M23C6) 2, D
(Laves) 2D
(M23C6) 3, D
(Laves) 3D
(M23C6) 4, D
(Laves) 4D
(M23C6) 5, D
(Laves) 5, calculate D respectively
(M23C6) 1, D
(M23C6) 2, D
(M23C6) 3, D
(M23C6) 4, D
(M23C6) 5And D
(Laves) 1, D
(Laves) 2, D
(Laves) 3, D
(Laves) 4, D
(Laves) 5Mean value, gained is D as a result
(M23C6), D
(Laves)Be this sample M
23C
6, the size of Laves precipitated phase cluster of particle.
This method results of measuring is as shown in table 1, and the result shows the results of measuring (shown in Figure 5) and this sample M of this method
23C
6With Laves phase content result of variations (shown in Figure 6) good consistance is arranged.
Table 1 the inventive method is surveyed 625 ℃ of lasting sample M of P92 steel
23C
6With Laves cluster of particle size mutually
| Loading stress/rupture time (MPa/h) | M 23C 6Cluster of particle size (nm) | Laves cluster of particle size (nm) |
| 180 / 30 | 266 | - |
| 160 / 170 | 298 | - |
| 160 / 243 | 334 | - |
| 150 / 454 | 318 | 262 |
| 140 / 2881 | 331 | 299 |
| 130 / 4018 | 336 | 304 |
| 120 / 7077 | 353 | 351 |
| 110 / 10122 | 371 | 385 |
Instance is 2.: use 700 ℃ of lasting samples of Super304H steel to be example with ultra-supercritical boiler.
Fig. 4 is a backscattered electron photo of 700 ℃ of lasting samples of Super304H steel.As shown in the figure, the microstructure of sample is mainly the M that distributes on austenitic matrix and the original austenite crystal prevention
23C
6Particle.For matrix, M
23C
6Therefore rich Cr is canescence in photo, matrix is then darker.For this method: at first; 1. ~ 3. obtain totally 5 in the backscattered electron photo of tested sample by the practical implementation step, after 4. count the pixel light and shade distribution plan of one of above-mentioned steps gained photo (establish it and be numbered 1) and this figure be divided into M set by step according to distribution plan medium wave peak position with image quantitation software Image pro plus
23C
6And two zones of matrix (Matrix) are (respectively to M in should steel
23C
6Precipitated phase and matrix), and then calculate M
23C
6The area A in zone
(M23C6) 1Simultaneously, measure the number of pixels N that the nominal length L of scale is comprised in photo; Then with M in the 4. middle gained backscattered electron photo of step
23C
6The area A in zone
(M23C6) 1Pass through formula:
Be scaled the equivalent size L of different precipitated phase cluster of particles in the heat-resisting steel
(M23C6) 1(unit is a pixel, Pix), utilizes formula again
(
kRepresent precipitated phases different in the steel, in this example
K=(M 23 C 6 ))
Calculate the physical size D of precipitated phase cluster of particle
(M23C6) 1
4. and 5. last repeating step obtains the physical size D of different precipitated phase cluster of particles in other 4 photos
(M23C6) 2D
(M23C6) 3D
(M23C6) 4D
(M23C6) 5, calculate D then
(M23C6) 1, D
(M23C6) 2, D
(M23C6) 3, D
(M23C6) 4, D
(M23C6) 5Mean value, gained is D as a result
(M23C6)Be this sample M
23C
6The size of precipitated phase cluster of particle.
This method results of measuring is as shown in table 2, and the result shows the results of measuring (shown in Figure 7) and this sample M of this method
23C
6Phase content result of variations (shown in Figure 8) has good consistance.
625 ℃ of lasting sample M of table 2 Super304h that the inventive method is surveyed
23C
6Phase cluster of particle size
| Loading stress/rupture time (MPa/h) | M 23C 6Cluster of particle size (nm) |
| 180 / 523 | 252 |
| 170 / 1080 | 255 |
| 160 / 1588 | 259 |
| 150 / 2024 | 272 |
| 130 / 4109 | 286 |
| 120 / 8688 | 333 |
The present invention has the following advantages and good effect:
1. to not measuring heterogeneous this present situation of particle aggregation coarsening rate method in the heat-resisting steel at present, proposed with the heterogeneous particle aggregation coarsening rate of cluster of particle characterization of size;
2. when only having monophased particles in the steel, compare, can measure the size that under metaloscope, can't measure between tens phase particle and cluster of particle sizes to the hundreds of nanometers scope with conventional metallographic method;
3. this method measuring and calculating process simple, fast, the result accurately, reliable;
4. this method also can be used for the size measuring and calculating of the precipitated phase particle and the cluster of particle of other steel grade and alloy except can be used for all kinds of heat-resisting steel, has broad application prospect.
Claims (1)
1. a method of calculating heterogeneous particle aggregation coarsening rate in the heat-resisting steel is characterized in that, may further comprise the steps: 1. by conventional metallographic sample preparation method with the polishing of tested sample sightingpiston, polishing and etch; 2. under electron probe or ESEM, select the backscattered electron imaging pattern, under 2000 ~ 5000 times enlargement ratio, take the backscattered electron photo of precipitated phase in the sample, the captured number of pictures of each sample is no less than 5; Thereby the photo that 3. the scale blacking of gained backscattered electron photo is not contained scale; 4. utilize image quantitation software Image pro plus to count 3. one of middle gained photo of step, establish it and be numbered 1 pixel light and shade distribution plan, this figure is divided into matrix region m and precipitated phase zone a, b ...; Wherein, the crest number R in the pixel light and shade distribution plan is the precipitated phase number, and R is followed successively by 1 from right to left; 2 ... R, the corresponding crest 1 of a is with the zone on the right side; The corresponding crest 1 of b, the zone between 2 ..., the zone between the flex point A of corresponding crest R-1 of last precipitated phase and crest R right flank; The A point is the matrix region with a left side; Calculate the area A in each precipitated phase zone then
A1, A
B1..., unit is a pixel, wherein the captured photo of subscript 1 expression sample is numbered 1; In addition, measure the number of pixels N that the nominal length L of scale is comprised in photo; 5. through the regional area A of each precipitated phase in the 4. middle gained backscattered electron photo of step
A1, A
B1And formula
Calculate the equivalent size L of different precipitated phase cluster of particles in the steel
A1, L
B1, unit is a pixel, utilizes formula then
Converse the physical size D of precipitated phase cluster of particle
A1, D
B1, wherein,
K=a, bRepresent precipitated phases different in the sample; 6. 4. and 5., to other photo repeating steps thus obtain the physical size D of different precipitated phase cluster of particles in the serial-gram
A2, D
B2, D
A3, D
B3, the numbering of the captured photo of subscript 2,3 expression samples; Calculate D then
A1, D
A2, D
A3, D
B1, D
B2, D
B3Mean value, gained is D as a result
a, D
bBe this sample a, b ... The average-size of precipitated phase cluster of particle.
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| CN103207179B (en) * | 2013-03-12 | 2016-04-20 | 宁波汉博贵金属合金有限公司 | A kind of evaluation method of silver based contact material metallographic structure |
| CN103674664A (en) * | 2013-10-21 | 2014-03-26 | 广东电网公司电力科学研究院 | Quantitative metallographic analysis method for phase M23C6 of Super 304H steel |
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