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ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsAddressing Problems with RevealingPrior Austenite Grain BoundariesWalt Moorhead and Ick KayafasProduct Evaluation Systems, Inc.Chris BagnallMCS Associates, Inc.November 17, 20101
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsBackground“PAGS” INFLUENCED BY: Carbon content, Thermo-mechanical history, Austenitizing temperature/time2
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsPAGS MEASUREMENT METHODSSeven different methods in ASTM E112, Annex A3 forestablishing Prior Austenite Grain Size1.2.3.4.5.6.7.Correlation ProcedureCarburizing method (Mcquaid-Ehn)Mock-Carburizing methodHypoeutectoid Steels -two-step methodOxidation methodFull-Hardening ( tempering) methodHypereutectoid Steels -slow cool (cementite) method3
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsBackground (cont.) No issues with AISI 1045, 1050,4140, 4340, 4150 Or are there issues?Problems arise when C contentfalls below 0.25%C4
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:AISI 4140/43404140 Chemistry: 0.4C, 1.0Mn, 1.0Cr, 0.2MoLollipop SectionAs-Received AISI 4140; Picral/Nital etch5
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:4340 Chemistry:AISI 4140/43400.4C, 0.8Mn, 0.9Cr, 2.0Ni, 0.3MoAs-Received, Nital Etch6
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:4340 Chemistry:AISI 4140/43400.4C, 0.8Mn, 0.9Cr, 2.0Ni, 0.3MoAs-Received, Stepan-Nacconol Etch7
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:AISI 4150, (1045)Chemistry: 0.5C, 1.0Mn, 1.0Cr, 0.2MoMock-Carburizing Procedure Heat treat per ASTM 3.2.1.3 Hold above A3 /1 hour (non-carburizing) W/Q to form martensite Mount, polish, etch with selected reagent8
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:AISI 4150Chemistry: 0.5C, 1.0Mn, 1.0Cr, 0.2MoMock-Carburizing Procedure1,470 F/1h/Q.Highly unstableboundaries;considered to besub-grains andnot PAGBsEtch: Picric Stepan-Nacconol9
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:4140 Chemistry:4340 Chemistry:AISI 4140/43400.4C, 1.0Mn, 1.0Cr, 0.2Mo0.4C, 0.8Mn, 0.9Cr, 2.0Ni, 0.3MoCarburizing ProcedureMcQuaid-Ehn Test: Packed in active carbon 1700 F/8 hours A/C Mount, polish, etch with selected reagent10
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:AISI 43404340 Chemistry: 0.4C, 0.8Mn, 0.9Cr, 2.0Ni, 0.3MoCarburizing ProcedureOxidizing Procedure1575 F/1h/WQ. ASTM 811
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:Chemistry:“4340” Bar Product0.4C, 0.45Mn, 0.3Si, 1.8Cr, 4.0Ni, 0.45Mo, 0.03VAs ReceivedStepan-Nacconol Etch. ASTM 712
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsLOW CARBON STEELS13
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:Chemistry (MAX):ASTM A336 (Alloy F22)0.15C 0.6Mn 0.5Si 2.6Cr 1.13MoMcQuaid-Ehn Test: 1700F/8h25X100XEtch: Picric Acid Stepan-Nacconol14
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:Chemistry (MAX):ASTM A336 (Alloy F22)0.15C 0.6Mn 0.5Si 2.6Cr 1.13MoMcQuaid-Ehn Test: 1700F/8h200XASTM 8500XEtch: Picric Acid Stepan-Nacconol15
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:Chemistry (MAX):ASTM A336 (Alloy F22)0.15C 0.6Mn 0.5Si 2.6Cr 1.13MoMcQuaid-Ehn Test: 1700F/8hSEISEINo carbide at gbs2kX20kX#30Elt.SiCrFeLineKaKaKaAt. %8.60.690.8Wt. %4.50.694.916
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:ASTM A336 (Alloy F22)Chemistry (MAX):0.15C 0.6Mn 0.5Si 2.6Cr 1.13MoOxidation v CarburizationSample cut from a casting runnerCarburized10 microns removedSmall (sub?)grains ASTM 8 1/217
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:Chemistry (MAX):ASTM A336 (Alloy F22)0.15C 0.6Mn 0.5Si 2.6Cr 1.13MoMcQuaid-Ehn Test: 1700F/8hProblems:SEI Depth of carburization 0.050” Si content very high at gbs Carbon will “diffuse” away from, or berepulsed by high-Si locations Are we measuring grains-orsub-grains?SEI18
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:ASTM A336 (Alloy F22)Chemistry (MAX):0.15C 0.6Mn 0.5Si 2.6Cr 1.13MoOxidation v CarburizationSample Cut from a Casting RunnerAs OxidizedCarburized10 microns removed19
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:ASTM A336 (Alloy F22)Low Carbon SteelProblems: Time required for evaluation Uncertainty of results Lollipop V Runner20
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsOTHER PAGS MEASUREMENT METHODS Fracture Grain Size MethodShepherd Standard Hydrogen Embrittlement Method Patented “Burning” Method21
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsOTHER PAGS MEASUREMENT METHODS Fracture Grain Size Method:Shepherd Standard22
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsOTHER PAGS MEASUREMENT METHODS Fracture Grain Size Method:Shepherd StandardASTM 425XASTM 923
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsOTHER PAGS MEASUREMENT METHODS Fracture Grain Size MethodShepherd Standard Hydrogen Embrittlement Method24
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsOTHER PAGS MEASUREMENT METHODS Hydrogen Embrittlement MethodMachined from Cast Slug and H charged25
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsOTHER PAGS MEASUREMENT METHODS Hydrogen Embrittlement MethodMachined from Cast Slug and H-charged26
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsOTHER PAGS MEASUREMENT METHODS Hydrogen Embrittlement MethodMachined from Cast Slug and H-charged27
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsOTHER PAGS MEASUREMENT METHODS Fracture Grain Size MethodShepherd Standard Hydrogen Embrittlement Method Patented “Burning” Method28
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:AISI 1022Chemistry: 0.23C, 1.0MnBurning Method Lollipop sample cut withoutusing coolant.29
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:AISI 1022Chemistry: 0.23C, 1.0MnLollipop Sample: Burning MethodOnly area “safe”for measurementEtch: Picric Acid Nital30
ASTM Subcommittee E04.08 Workshop:Grain Size Determination According to ASTM E112, E930, E1181, E1382 and Other MethodsMaterial:AISI 1022Chemistry: 0.23C, 1.0MnBurning MethodStepan-NacconolNital31
Seven different methods in ASTM E112, Annex A3 for establishing Prior Austenite Grain Size. 1. Correlation Procedure 2. Carburizing method (Mcquaid-Ehn) 3. Mock-Carburizing method 4. Hypoeutectoid Steels -two-step method 5. Oxidation method 6. Full-Hardening ( tempering) method 7. Hypereutectoid Steels -slow cool (cementite) method . 4. Background (cont.) ASTM Subcommittee