DATASHEET org, Itmay be ‘ordered online, or serviceat 800/336-5152 Cost to ASM membersis $152. Common etchants for Irons and Steels Bruce L. Bramfitt Bethlehem Steel Corp. Bethlehem, Pennsyloania Arlan O. Benscoter Lehigh University Lehigh, Pennsyfoania Etchants for revealing macrostructures in iron and steel* Fichingreagent___Toreveal (Composition Remarks Hyeirochloricacid Segregation porosity, S0mL HO, ‘Temperature: 71-82°C (160-180 cracks, depthof 50mL HCL ‘Time: 1-60) min, depending on type of hardened 2onesin steel and type of structure tobe tool steels developed. Mixedacids Welds, segregation. S0mL HO. ‘Temperature: 93°C 20°F, cracks andhardened — 38mL, HCL, ‘Time: 15-45, or Temperature: 2°C 72°F), zones. VmbH:80, Time: -4hours ‘Ammonium | Welds ‘mL HO ‘Surface shouldbe rubbed with absorbent persulfate (Rawelon) TOL (NHY.S.0; cotton during etching. Time: etched to desired contrast Nitvic acid meas. 75mL HO. Use cold on large surfaces that cannot be hhydrochloricacid _25mLHNOs conveniently heated Oberhoffer's Developsdendritic 500ml HO Use atroom temperature. reagent patternin steel Iron 30gFeCh O5gSnCly Immerse about 20s. emmichedarensare 1 gCuCh 500ml. darkened. ethyl alcohol 500ml HO. Kalling’sreagent Developsdendritic—33mL HO. Eich to desired contrast patterninsteol;atiacks 15g CuCl, ferriticand martensitic 33mLmethyl stainlessstedls. Ferrite alcohol darkened;martensite mL HCL darker; austenite ight Humireysreagent Developsdendsitic 500ml. HO) Slight abrasion of surface after etching is segregation 25ml. HCL recommended 60g Cu (NH) Balls reagent Weldsinstainless 40mL10 Stainless seal cathode 5V (electrolytic) steel mL HNO, __Time:to desired contrast. Watertownarsenal For carbon and stainless 50mL HO ‘Temperature: 71-82°C (160-180 °F) steels, general structure 12mLH;50, ‘Time: 10-60-min Used with cut or ground 38mL HCL surfaces Dilute aqua regia Forhighalloysteels, — 25ml. HO. “Time: 10-15 min at room temperature FeCo high-temperature 25ml HNOs alloys 50ml HCL Picarcyand Maraging sted @mLlacticacid —_Useatroom temperature coworkers rmacrosiructure 20mL HNOs toml HAL Burgand Weiss Nitriding stedls a5mL HO ‘Temperature: 71°C (160 °F) macrostructure 415ml ammonium — Time: 10min persulfate Marblesreagent General etch for SOmL HO Solution canbe heated austenitic stainless steal 10g CuSO, 50mL HCL Millerand Houston Weldsand general 90mlL HO. Use electrolytically with polished surface. macrosiructureof 10 gCrOs Platinum or stainless steel cathode. austenitic stainless steel “Temperature: 16-38 °C (60-100°F) 6V. ‘Time: 2-7min ADVANCED MATERIALS & PF Continued CESSES/JUNE 2002Etchants for reventing macrostructures in iron and steel*, continued Etchingreagent _Toreveal ‘Composition Remarks Loria(nitrosulfuric Ascaststructureand 20m HO ‘Useat room temperature acil etch) grainsizein ast steels 20mL HNO; 20m SO, Nielsen Stress-corrosion cracks mL methyl ‘Temperature room inaustenitic stainless alcohol ‘Time: approx. 1h crack pattern vividly steal SL bromine revealed age soy apy cea, nati jy da ats (MSDS) abn eres Etchants for revealing phases and constituents in ferrous materials Etchingreagent Composition Remarks Ferrite grain 1to5mLHNOs ‘Theauthors recommend a 2% solution; usually samples are etched 10 0 20s witha boundaries: (nitticacta) gentle agitation and the polished surface facing upward toreveal the ferrite grain Nital 9 t095mLethyl Doundaties. To reveal al the grain boundaries, the last polishing step should be with silicon dioxide fr a least 60, and the sample should then be etched shortly after polishing before passive layer forms to prevent an even etch. Ifthe sample is to be ‘examined in theas polished condition it should be repolished for 10to 15s with silicon dioxide prior to etching, Note: A nital etch is not recommended for etching ppearlite, because it does not etch evenly, Forte grain ‘Stock solution A Excellent etchant to show both equiaxed and cold-worked micro-structares, Mix boundaries: 100mL HO stock solution A to equal parts of solution B just prior to etching, Place the polished Marshall'sreagent 8g oxalic acid face of the sample ons side during immersing in the etchant to prevent or SinLHSO, minimize pitting. Ifthe sample does not react tothe reagent, add 1 mL hydrofluoric (eulfrie acid) to 100ml of solution. Ifa haze covers the surface, remove by placing the sample Stock solution B ina 3% aqueous disodium ethylenediamine tetraacetate EDTA solution. Place the HO; 0%) sample and solution in an ultrasonic cleaner for several minutes. lush the sample (hydrogen peroxide) with water, thenalcobol, then dry. Ferrite grain 100mLH,0 Pro-etch for 3s with2%rnital, Etch in Beraha's reagent withthe polished side ofthe ‘boundaries: 10g NasO; sample face up for 45; do not agitate. Rinse with water lush withalcohol, and dey. Beraha's am thiosulfate) Ifthe sample is over-or under-etched, remove etchant by polishing with 03 10: aluminum oxile for 15 , followed by silicon dioxide for 45s, andre-etch. Pearlitestructure: 96mLethyLalcohol _Picrals one of few etchants that improves with use. A common practices toage the 40pical A gpicricacid ‘etchant by placing piece of a ground steel into the solution until the etchant urns a Sdrops 17% zephiran dark green. This technique makes the etching time constant, usually 0 s for pearlite (enzalkonitum chloride, or FesC carbides. The etchant canbe saved for future use. Samples with more than Sanofi Synthelabo Inc) | 0.5% Cr, add 5 drops of hydrochloric acid per 100ml of solution per75mL solution Peaslite structure: Stock solution A Excellent etchant to outline peatlite colony boundaries, Marshall'sreagent — 100mLHO 8 goxalic acid SL. HsSO, ‘Stock solution B HAO; (0%) Peaslite structure: 100mLH.O, Bring the solution to low boil; do not boil dry. ching time: 5-10 min, The olution Alkaline sodium 25gNaOH, ‘will attack Bakelite mounts; thermosetting epoxy mous are recommended. The picrate 2 gpicricacid solution will color cementite but will nt color carbides with high (10%) Cr content, ‘Thesolution will also attack sulfides and delineate grain boundaries in steels that ave been cooled slowly. Peatlitestructure: 50mL. H:O ‘Tint etches pearlite. Etching time: 40-120. Etch in Klemm's reagent with the Klemm’sreagent —NajS,O; enough for _ polished side of the sample face up, do not agitate Ferrite appears black brown, but saturation, ‘carbides, nitriles, ane phosphicles remain white. Phosphorus distribution can be La kOs detected more sersitively than with phosphorus reagents based on copper sats ADVANCED MATERIALS & PROCESSES /JUNE 2002 00