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  • Color Tint Etching For Multiphase Steels

    Încărcat de

    Joselo HR
    143 vizualizări4 pagini
    COLOR ETCHING

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    Color Tint Etching for Multiphase Steels

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    COLOR ETCHING

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    143 vizualizări4 pagini

    Color Tint Etching For Multiphase Steels

    Încărcat de

    Joselo HR
    COLOR ETCHING

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    © All Rights Reserved
    Descărcați ca PDF sau citiți online pe Scribd
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    din 4
    COLOR -ETCHING for Multiphase Steels Asimple step-etching procedure with comaion etching solutions has been applied to reveal individual iticrostructural constituents in some of the high-strength steels of current industrial interest. ‘Amar K. De, John G. Speer*, and David K. Matlock* Colorado School of Mines Golden, Colorado hase identification not possible with stan dard black and white micrographs is often possible with color micrographs. In spite Of this, the high cost associated with color processing and perceived difficulties in sample preparation, have prevented color metalopraphy from becoming standard quality control tcol to support product assessment during production. fowover, the cost reductions associated with digital photography now enable color metallog, raphy to be incorporated into laboratory assess- ments of production-dependent microstructural variations. Improvements in digital data storage systems for standard light-optical microscopes en- able acquisition of quality color micrographs at rea sonable cost. Furthermore, color metallographic ‘echiniques have been developed and applied to as- sess microstructures in a variety of systems, Toillustrate potential applications of color met- allography, this article considers microstructural constituent identification in DP and TRIP high: strength steels. It summatizesa simple color etching procedure that has been found to consistently re- veal the distinct microstructural constituents with the help of light optical microscopy. The color mi- crographs are reproduced here with the help of a digital data storage system. Advanced steels High-strength shoot stee! products such as dnal- phase (DP) and austenite containing transforma- tion induced plasticity (TRIP) steels are now gaining *Memberof ASM International ADVANCED ‘Tempertare “Time scond| Time ons Fig ‘TRIP microti significant industrial importance for acivanced au tomotive applications, Dual-phase steels contain a fine dispersion of martensite ina fertite matrix, al- though the microstructure is often quite variable and may contain martensite, retained austenite, peatlite, and bait. TRIP sheet steels consist of ferit,bainite, marten site, and substantial amounts of retained austenite Allof these constituents are critical for developing the forming.and service properties of DP and TRIP steels, and hence accurate phase identification is needed to characterize the important effects of al- Joying and processing ‘Three different steel microstructures representa- tiveof typical multiphase steal families were selected for study. A conventional C Mn Si sheet steel for production of both DP/TRIP microstructures, and ‘a medium-carbon low alloy steel bar were included. As summarized in Table 1, several color etchants or etching tecliniques have been developed for these high strength stools, and they form the basis or the approach reviewed here. The limitations described inthe table are based on the authors’ experiences. ‘Multiphase microstructures The base steel (0.19C, 1.5Mry 1.58i) for DP and TRIP microstructures was available in the form of 1.2mm cold rolled sheet, * Dua-phuse stel: The DP microstructure (ferrite + martensite) is usually procluced by annealing the steel at an inter-critical temperature (e+ region) and then rapidly cooling to room temperature. In the present study, three different duual-phase mi- MATERIALS & PROCESSES/FEBRUARY 2003 ‘Shel meat eyes forthe production of a) dual phase and (8) Table 1 — Common tint etchants for multiphase steels and some limitations ‘Htching solutions Tinting effects on microstructure Limitations 2.5% Nital followed by 10% aqueous Fenite off white, bainite, martensite Bainite, pearite, carbides and martensite appear sodium metabistlite" and peartedark austenite white. dark. LePea® Terrteyellow /blue, bainite brown, Austenite and nudensitenct separately Equal postions of solitons setained austenite and identifiable. Adltional hest treatment or seaming, (@)!eaqueous sodium metabisullite martensite white electron microcopy ‘needed for identifying (0)496Dieral ‘mustensite and austenite 494 Picraland Deaqueoussodiuin __ Ferte brown, maitensiteand ‘Austenite and mariensit not separately delineated rmetabisulite austenite white. 294 Nita followed by heat tinting Feit, bainiteare beige, austenite purple, martensite darkblue, ‘Additional heat treatment steps. {EGR Vir Voor angst Pro” ASM Dl, Mats Pt tn 199 Bruce, Bon en O Rowe aalagapr Gal towel > fr dr ara Ses" ASM in, 202 FS. Leou ural of Mea, 2, 190, cL 3. Tn, P11 Baad EV Pra CayProf TIP Sleds a, B- ‘som 0, crostructures were produced by annealing the sam- ples at three different temperatures (750,775, and 800°C) for 300 seconds, and then quenching in water. This procedure was expected to result in controlled variations in the phase fractions and compositions within the a+ yfield, * Transformation-induced plasticity stels: To de- velop the TRIP microstructure, the steel was an- nealed at 775°C for 300 seconds and then cooled rapidly to an intermediate temperature of 400°C (above the Ms). The sample was then held for 300 seconds to allow for bainitic ferrite formation ac. companied by carbon-rejection into the interlath austenite, which stabilizes the austenite during rapid cooling to room temperature. The schematic annealing cycles followed are shown in Figute 1. ‘The low alloy steel bar was normalized at 840°C for one hour after hot rolling. Etching solutions andl procedure ‘The following etching solutions were selected: 14% picral (4 gm diy picricacid in 100 ml ethan col), mixed with few drops of concentrated hydro- hltieacid (1m poe 100m of piral solution) and 10% aqueous sodium metabisullite solution. ‘The purpose of the hydrochloric acid was to im- prove grain boundary etching and sharpen the ap- pearance of iton carbides. ‘The steel cross-sections were mounted in phe nolic resin (bakelite), mechanically ground with 120 through 600 grit paper, polished with 6 um dia~ mond and then finally polished to. scratch sree condition with 1 rm diamond. After polishing with diamond paste the surfaces were cleaned with soap solution, water, and then alcohol. The surfaces were dried with hot air. Ina two-stage step-eiching procedure, the sam ples were first clipped in the picral solution for 18 fo 20seconds for DPand TRIP steels, and 45 to 60 seconds for the alloy steel. During the whole etching, process, the samples were gently oscillated. After etching in picral, the samples were immediately washed with water followed by ethancl and then were blown diy in hota Picral waschosen over nital because of better de- lineation of carbides and bainite with picral. Nital attacks ferrite grains and grain boundaries, but pi «ral attacks interfaces between ferrite and carbide. ‘Therefore, the carbides are better revealed by picral ‘Once the microstructural observation was com- pleted afier the first stage of etching, the samples ‘wore further dipped in freshly prepared sodium metabisulfte solution for six to eight seconds. They ‘were immediately washed with water followed by cethanol,and then dried in hot air. The soaking time ‘withsodiumn metabisulfite was critical, because over- ‘exposure to the solution led to excessive tinting, of martensite and eventual blackening ofthe ferrite, Microscope observations ‘The samples were examined with an Olympus PMG: light optical microscope equipped witha high resolution DP-12 digital camera (35 mm) ystem. The digital camera is directly interfaced th a computer that allows the color micrographs to be downloaded in digital formats (jpeg, tiff) ‘The color micrograph files can either be printed by color printers, or can be taken to any commercial photo-shop for color printing, For examination with the scanning electron mi- ‘roscope (SEM) at higher magnification, selected samples previously examined in alight microscope were further etched with 2% nital solution (2 ml concentrated nitric acid in 98 mi ethanol), without an intermediate polishing step. The amount of re- tained austenite was measured in some instances by X ray diffraction by copper Ka radiation. Thoin tegrated intensities of diffraction peaks 220}, (311), (21 Tjq and (200)_ were measured and the volume fraction of austenite was then calculated by the di- rect comparison method. In addition, individual shases were measured for microhardness witha ‘ickers 10 gf load, to confirm the metallographic phase identification results, DPsteel microstructure Figure 2a shows the microstructure after the first etching step of the dual-phase steel quenched from ‘SIPC. The micrograph clearly reveals undissolved carbides and traces of pearlite within some carbide structures. Martensite or austenite is not revealed at this siage, though these constituents appear as relief at the grain boundaries. Figure 2h isthe sec- ‘ondary electron image of the same sample from the SEM, revealing the same microstructure details. igure 2c shows the microstructure after the ADVANCED MATERIALS & PROCESSES/FEBRUARY 2003 Fig. 2— Microstructure of dua-phasestet quenched from 750°C (a afer rst stage etching reoealing pearte and wssotoe ones in the fer- rite matrix, JOOOX, () searing electron image ofthe same sane and (c) microstructure afer second etdring step with sodium metabsulfite re- ealing martensite (sraw-eoloed), ustette (ite), pearlte and undiseloed caries (bu second stage of etching, It clearly reveals straw-colored martensite at the grain boundaries and also within the carbide regions, Retained austenite appears as small white particles at grain bound- aries and also within the carbide- pearlite conglomerate. The micrograph in Figure 2calso reveals that the tintetch distinctly distinguishes the martensite from austenite in some of the M-A con- stituent islands as marked in the micrograph. After the two-stage etching process, Fig. 3a and 3b reveal the microstriic- tures of two other dual- phase steels, quenched from. 775 and 800°C, respec- tively. The straw-colored martensite is distinctly revealed, and the retained austenite appears as small bright white particles mostly associated with marten- site. Carbides were hardly detected in these two steels. The distinct color con- ‘rast between the martensite and the fer- rite matrix also enabled meastirement of the volume fraction of marter through image analysis, and the ‘martensite fractions were found to be 43% and 52% respectively. Retained austenite was measured by X-ray diffraction and was found to be 18 to 2%, (One important revelation from the above etching experiment with three different DP steels is that the characteristic tinting of martensite was quite con sistent despite significant differences in the com- position and volume fraction of the martensite. TRIP steel microstructure Figures da and 4b show the TRIP steel mi- crostructure after the two etching stages. The bai- nite is clearly delineated in the form of angular or acicular patterns. (In these silicon-containing steels, carbicie-free austenite containing bainite mi- crostructures re found. They consist of bainitie fer- rite laths, not apparent in Fig. 4, and interlath austenite, which is apparent and highlights the aci cular morphology.) Martensite and austenite are not differentiated clearly at this stage. ‘Thesecond siage etching with sodium metabisul- fite tints the martensite, and the austenite remains unaffected, The final microstructure (Figure 4b) shows the martensite in its typical straw color, and therefore martensite can be identified separately ADVANCED Fig. 3— Microstructures of dual-yhase steels quenched from (a) 77 secondetching step receaing mumtensit (strxo-oloed) ane fne retained austenite grains (whit) itv the ferrite matrx, 10Q0X. No carbides are present in these spe lack, 1000X. from austenite. Overexpostre to the second stage of etching darkens the martensite and makesit dif- ficult to distinguish from bainite ‘The austenite is somewhat brighter or whiter than the ferrite andl listinetly delineated from the fertite due to the addition of hydrochloric acid. The volume fraction of retained austenite was measured, to be about 10% by X-ray diffraction in this steel Low-alloy steel ‘The effectiveness of the step etching procedure ‘was further substantiated during microstructure characterization of an alloy steel. Figure 5a shows the microstructure of the medium-carbon alloy steo! after the first stage of etching, The steel apparently represented complex ferritic pearlitic bainitic mi- crostructure, The picral-etching distinctly revealedt the pearite (massive dark regions) and bainite (ina granular bainite morphology) constituents ‘The microstructure observable at this etching stage also revealed the presence of a band con: taining some other constituents that are not clearly identifiable at this stage. The second stage tint etching revealed these constituents to include martensite, identified by its characteristic straw. MATERIALS & PROCESSES/FEBRUARY 2003 75 ane (6) BPC eer the te ard martestesterie cud (1) afr the second etcang step realty martensite (stnew-

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