CN101382494A - Method for displaying and quantitatively determining retained austenite or island martensite- austenite in TRIP steel - Google Patents
Method for displaying and quantitatively determining retained austenite or island martensite- austenite in TRIP steel Download PDFInfo
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- CN101382494A CN101382494A CNA2008100489737A CN200810048973A CN101382494A CN 101382494 A CN101382494 A CN 101382494A CN A2008100489737 A CNA2008100489737 A CN A2008100489737A CN 200810048973 A CN200810048973 A CN 200810048973A CN 101382494 A CN101382494 A CN 101382494A
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Abstract
The invention relates to a display and quantitative detection method of residual austenite or island martensite-austenite (MA island for short) in TRIP steel. The method comprises the steps: (1) a TRIP tapping sample is prepared into a metallographic specimen; (2) after grinding and polishing, the metallographic specimen is light etched for 5 to 8 seconds in Nital of 1 to 3 percent by weight, and water is sprinkled on a flannel polishing disk for 1 to 2 seconds; sodium pyrosulfite water solution of 1 to 3 percent by weight and picral of 2 to 6 percent by weight are mixed by volume ratio of 1:1 to prepare corrosive liquid, then the metallographic specimen is put into the corrosive liquid for etching of 55 to 65 seconds; (3) the structure of the TRIP steel is observed under a metallurgical microscopy: the delta ferrite is minus blue, the residual austenite or MA island is white, and bainite is brownish-black; and (4) each phase in the structure is carried out quantitative analysis. The method presents different colors, each phase of structure has distinct layers which are easy to distinguish; and a quantitative image analysis method is utilized to fix amount of the feature object structure, which is objective and accurate and has good repeatability.
Description
Technical field
The present invention relates to retained austenite or island martensite body-austenitic demonstration and quantitative detecting method in a kind of retained austenite or island martensite body-austenitic demonstration and the quantitative detecting method, particularly TRIP steel.
Background technology
In recent years, the application of TRIP steel in auto industry with high-intensity high-tenacity increased year by year, and market outlook are good.Factors such as the content of retained austenite in the TRIP steel (being martensite-austenite sometimes, because of it is island, so claim the MA island again), volume, pattern, size, existence play a part crucial to its tissue and Effect on Performance.The difficult point of employing quantitative metallography Technique on T RIP structure of steel analysis is identification and the extraction to the characteristic body tissue.With traditional caustic solution, the gray level image that can only obtain organizing, each mutually between because contrast obviously is difficult to differentiation inadequately, even the part details covered, and is unfavorable for the quantitative test of characteristic body.
Japanese patent application (2007-05-10) JP2007111765 discloses Nippon Steel Manufacturing Corp's " milling method of the deformation induced plasticity high-strength steel sheet of retained austenite " (" residual オ-ス テ Na イ ト metamorphosis has lured plasticity The The ゐ high-strength steel sheet Block レ ス manufacturing process "), company of to the effect that Japanese Nippon Steel provides a kind of intensity to reach more than the 590MPa, have excellent deep drawing quality, the metal lographic examination result reaches more than 80% or the manufacturing process of the controlled rolling TRIP steel plate below 70% for the retained austenite volume fraction.
Japanese patent application (2001-05-08) JP2000309842 discloses " retained austenite type high-strength steel sheet " (" residual オ-ス テ Na イ ト type high-tensile steel "), and a kind of of Mitsubishi motor corporation invention to the effect that has excellent extensibility and pore-creating character and contain the manufacture method of the automobile exterior panel of suitable retained austenite volume fraction with high-tensile steel.
More than two Jap.P. introductions be to contain the Automobile Plate of certain retained austenite or the manufacture method of TRIP steel, to the demonstration of retained austenite in the TRIP steel and not explanation of detection by quantitative.
Chinese patent application (2006-07-05) 200510097088 discloses " ultrahigh-strength thin steel sheet of hydrogen embrittlement resistance and excellent in workability ", main contents are reaching more than 1% through metallographic detection retained austenite that Kobe Steel of Co., Ltd. provides, and pulling strengrth is the above a kind of hydrogen embrittlement resistance of 1180MPa and the ultrahigh-strength thin steel sheet of excellent in workability.
Chinese patent application (2007-02-07) 200580002384 discloses " hot dip galvanized high strength steel sheet of plating adhesion and hole expansibility excellence and manufacture method thereof ", and main contents are that to have ferrite, bainite, area percentage be that 0.5～10% tempered martensite and percent by volume are 5% or the plating adhesion of above retained austenite and the hot dip galvanized high strength steel sheet and the manufacture method thereof of hole expansibility excellence to the metal structure of Nippon Steel Manufacturing Corp invention.
Chinese patent application (2003-03-22) 03107449 discloses " high tensile hot rolled steel sheet that ductility and stretch flangeability are outstanding and manufacture method thereof ", main contents for Japanese Jfe Steel Corp provide a kind of yield strength be more than 780 MPas or more than 980 MPas, contain high tensile hot rolled steel sheet and the manufacture method thereof of 2～7% retained austenites.
Above patent introduction be the manufacture method of the Automobile Plate, TRIP steel or the steel plate that contain certain retained austenite, demonstration and the detection by quantitative of retained austenite in the TRIP steel all do not had explanation.
Summary of the invention
For overcoming the deficiency of above-mentioned technology, provide a kind of and can obviously distinguish contrast, be convenient to the retained austenite of characteristic body quantitative test or the demonstration and the quantitative detecting method on MA island.
Above-mentioned purpose of the present invention reaches by the following technical programs:
The demonstration and the quantitative detecting method on retained austenite or MA island in a kind of TRIP steel, its step is as follows:
(1) by the sampling standard with TRIP steel sample to be checked intercepting after, inlay with phenolics edge material heat and to be prepared into metallographic specimen;
(2) described metallographic specimen is after grinding, polishing, the first light etch of nital with 1%～3% (wt.), the etch time is 5～8 seconds, gently polishing again, promptly a water is light on the flannelette polishing disk threw 1～2 second, utilize 1%～3% (wt.) Sodium Metabisulfite (Sodium Metabisulfite, molecular formula Na then
2S
2O
5) aqueous solution and 2%～6% (wt.) picral evenly is mixed and made into corrosive liquid for 1:1 by volume, and described metallographic specimen is put into described corrosive liquid etch 55～65 seconds;
(3) tissue of observation TRIP steel under leica DM6000 M metaloscope: ferrite is blue yellow, and austenite or MA island are white in color, and bainite is brownish black;
(4) to each carries out quantitative test mutually in the tissue.
Beneficial effect:
The present invention both overcome with gained tissue behind traditional nitric acid alcohol etch sample each mutually between contrast obviously be difficult to inadequately distinguish even the concealed deficiency of part details, help the extraction of characteristic body again, improved the accuracy of retained austenite or the quantitative test of MA island, also can carry out quantitative test mutually simultaneously ferrite, bainite etc.
Utilize Sodium Metabisulfite and have weak acid mixed liquor that uniform and stable corrosion renders a service as metallographic etchant, make the tissue in the TRIP steel present different colors, each phase constitution is well arranged, be easy to identification, utilize image quantitative analysis method that its characteristic body tissue is carried out quantitatively, objective and accurate, favorable reproducibility.
Compare the present invention with conventional art:
(1) make each phase constitution in the TRIP steel present different colors, clear-cut, well arranged, be easy to identification;
(2) can effectively carry out qualitative and quantitative analysis to each phase constitution, and quantitative result accuracy height, in production testing and fundamental research, vital role is arranged.
The present invention is described further below by the drawings and specific embodiments, but and do not mean that limiting the scope of the invention.
Description of drawings
Fig. 1 is the metallographic structure photo of TRIP steel after the etch of the traditional etch method of employing;
Fig. 2 is the metallographic structure photo of TRIP steel after the etch of employing etch method of the present invention;
When Fig. 3 is quantitative test of the present invention to the pseudo-colours identification figure on retained austenite in the TRIP steel or MA island;
Fig. 4 is the maximum slide calliper rule diameter statistical distribution histogram on retained austenite or MA island.
Embodiment
Comparative Examples 1
The demonstration and the quantitative detecting method on retained austenite or MA island in a kind of TRIP steel, its step is as follows:
(1) by the sampling standard with TRIP steel sample to be checked intercepting after, inlay with phenolics edge material heat and to be prepared into metallographic specimen;
(2) described metallographic specimen is put into 3% nital etch 60 seconds with described metallographic specimen after grinding, polishing;
(3) tissue of observation TRIP steel under leica DM6000 M metaloscope obtains metallographic structure photo as shown in Figure 1.
Can only see ferrite on the black and white picture as shown in Figure 1, and retained austenite or MA island profile and not obvious on picture, microscopic structure can not show at all.
Embodiment 1
The demonstration and the quantitative detecting method on retained austenite or MA island in a kind of TRIP steel, its step is as follows:
(1) by the sampling standard with TRIP steel sample to be checked intercepting after, inlay with phenolics edge material heat and to be prepared into metallographic specimen;
(2) described metallographic specimen is after grinding, polishing, and with the light etch of nital of 1% (wt.), the etch time is about 8 seconds earlier, gently polishing again, promptly a water is light on the flannelette polishing disk threw 2 seconds, utilized 1% (wt.) Sodium Metabisulfite (Sodium Metabisulfite, molecular formula Na then
2S
2O
5) aqueous solution and 6% (wt.) picral evenly is mixed and made into corrosive liquid for 1:1 by volume, and described metallographic specimen is put into described corrosive liquid etch 55 seconds;
(3) tissue of observation TRIP steel under leica DM6000 M metaloscope obtains metallograph as shown in Figure 2.Wherein, colored display effect can clearly be observed the bainite of the retained austenite of blue yellow ferrite, white or MA island, brownish black;
(4) utilize Analy SIS quantitative analysis software to each carries out quantitative test mutually in the tissue: after image was handled, recording ferritic mean intercept was 7.36 μ m, and corresponding grain size progression is 10.88 grades.
Extract characteristic body, to the pseudo-colours identification figure on retained austenite in the TRIP steel or MA island, recording the shared area percentage in retained austenite or MA island was 4.89% when Fig. 3 was quantitative test of the present invention.
Table 1 and table 2 for after the quantitative test to the statistic analysis result on retained austenite or MA island.
Fig. 4 is the maximum slide calliper rule diameter of a retained austenite or MA island statistical distribution histogram.Wherein horizontal ordinate is corresponding to " stepping mark " in the table 2, and ordinate is corresponding to " frequency " in the table 2.
The measurement statistics on table 1 retained austenite or MA island
The maximum slide calliper rule diameter statistical distribution on table 2 retained austenite or MA island
The demonstration and the quantitative detecting method on retained austenite or MA island in a kind of TRIP steel, its step is as follows:
(1) by the sampling standard with TRIP steel sample to be checked intercepting after, inlay with phenolics edge material heat and to be prepared into metallographic specimen;
(2) described metallographic specimen is after grinding, polishing, and with the light etch of nital of 3% (wt.), the etch time is 5 seconds earlier, gently polishing again, promptly a water is light on the flannelette polishing disk threw 1 second, utilized 3% (wt.) Sodium Metabisulfite (Sodium Metabisulfite, molecular formula Na then
2S
2O
5) aqueous solution and 2% (wt.) picral evenly is mixed and made into corrosive liquid for 1:1 by volume, and described metallographic specimen is put into described corrosive liquid etch 65 seconds;
(3) tissue of observation TRIP steel under metaloscope: ferrite is blue yellow, and austenite or MA island are white in color, and bainite is brownish black;
(4) utilize Analy SIS quantitative analysis software to each carries out quantitative test mutually in the tissue.
Embodiment 3
The demonstration and the quantitative detecting method on retained austenite or MA island in a kind of TRIP steel, its step is as follows:
(1) by the sampling standard with TRIP steel sample to be checked intercepting after, inlay with phenolics edge material heat and to be prepared into metallographic specimen;
(2) described metallographic specimen is after grinding, polishing, and with the light etch of nital of 2% (wt.), the etch time is 6 seconds earlier, gently polishing again, promptly a water is light on the flannelette polishing disk threw 1.5 seconds, utilized 2% (wt.) Sodium Metabisulfite (Sodium Metabisulfite, molecular formula Na then
2S
2O
5) aqueous solution and 4% (wt.) picral evenly is mixed and made into corrosive liquid for 1:1 by volume, and described metallographic specimen is put into described corrosive liquid etch 60 seconds;
(3) tissue of observation TRIP steel under metaloscope: ferrite is blue yellow, and austenite or MA island are white in color, and bainite is brownish black;
(4) utilize Analy SIS quantitative analysis software to each carries out quantitative test mutually in the tissue.
Described in the above-mentioned steps (2) earlier with the light etch of nital of 2% (wt.), the etch time is when being 6～7 seconds, the etch better effects if.In the described step (2) described metallographic specimen is put into described corrosive liquid etch in the time of 60 seconds, can obtain better effect.
Claims (3)
1, retained austenite or island martensite body-austenitic demonstration and quantitative detecting method in a kind of TRIP steel, its step is as follows:
(1) by the sampling standard with TRIP steel sample to be checked intercepting after, inlay with phenolics edge material heat and to be prepared into metallographic specimen;
(2) described metallographic specimen is after grinding, polishing, the first light etch of nital with 1%～3% (wt.), the etch time is 5～8 seconds, gently polishing again, promptly a water is light on the flannelette polishing disk threw 1～2 second, utilize 1%～3% (wt.) Sodium Metabisulfite aqueous solution and 2%～6% (wt.) picral evenly to be mixed and made into corrosive liquid for 1:1 by volume then, described metallographic specimen is put into described corrosive liquid etch 55～65 seconds;
(3) tissue of observation TRIP steel under metaloscope: ferrite is blue yellow, and retained austenite or MA island are white in color, and bainite is brownish black;
(4) to each carries out quantitative test mutually in the tissue.
2, retained austenite or island martensite body-austenitic demonstration and quantitative detecting method in the TRIP steel as claimed in claim 1, the first light etch of nital described in the described step (2) with 1%～3% (wt.), the etch time is 6～7 seconds.
3, retained austenite or island martensite body-austenitic demonstration and quantitative detecting method in the TRIP steel as claimed in claim 1 or 2 in the described step (2) are put into described metallographic specimen described corrosive liquid etch 60 seconds.
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