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N 7 3- 21 45 7
NASA CR-121189
FURTHER DEVELOPMENT
AND CHARACTERIZATION OF VM-103,
A NASA WROUGHT COBALT-BASE ALLOY
by R. A. Harlow and E. E. Ritchie
PHILCO-FORD CORPORATIONAERONUTRONIC DIVISION
prepared for
NATIONAL AERONAUTICS AND SPACE ADMINISTRATION
NASA Lewis Research CenterContract NAS 3-14329
https://ntrs.nasa.gov/search.jsp?R=19730012730 2018-06-11T09:50:43+00:00Z
1. Report No.
NASA CR-12 11892. Government Accession No. 3. Recipient's Catalog No.
4. Title and Subtitle
Further Development and Characterization of VM-103,A NASA Wrought Cobalt-Base Alloy
5. Report Date
December 15, 19726. Performing Organization Code
7. Author(s)
R. A. Harlow and E. E. Ritchie
8. Performing Organization Report No.
10. Work Unit No.9. Performing Organization Name and Address
Philco-Ford CorporationAeronutronic DivisionFord RoadNewport Beach, California 92663
11. Contract or Grant No.
NAS3-14329
12. Sponsoring Agency Name and Address
National Aeronautics and Space AdministrationNASA Lewis Research CenterCleveland, Ohio 44135
13. Type of Report and Period Covered
Contractor Report
14. Sponsoring Agency Code
15. Supplementary NotesProject Manager, Fredric H. Harf and J. C. FrecheMaterials and Structures DivisionNASA Lewis Research CenterCleveland. Ohio 44135
16. Abstract
The data obtained during this and previous programs indicate that the VM-103 alloy has usefulstrength at temperatures as high as 2200°F (1204°C), and can be considered as an alternatefor other wrought superalloys such as L-605. The addition of 10 percent nickel to the standardcomposition improves both the hot and cold fabricability, ductility, impact strength, andmetallurgical stability, while it only slightly reduces strength properties. Electroslag re-melting was effective in significantly increasing the fabricability of vacuum induction methodVM-103, both with and without the 10% nickel addition. A specification for wrought VM-103was developed and is included. Although thermomechanical processing improves lowertemperature properties, no improvement occurs at temperatures at or above 2000°F (1093°C).
17. Key Words (Suggested by Author(s))
Cobalt alloysHeat Resistant alloysThermomechanical processingElectroslag remelting
18. Distribution Statement
19. Security Classif. (of this report)
Unclassified
20. Security Classif. (of this page)
Unclassified
21. No. of Pages
63
22. Price*
$3. 00
: For sale by the National Technical Information Service, Springfield, Virginia 22151
TABLE OF CONTENTS
Section Title Page No.
1 Introduction 1
2 Procedure 4
Material 4
Ingot Reduction 7
Forging 7
Rolling 7
Heat Treatment 8
Solution Heat Treatment 8
Aging . 8
Mechanical Testing 8
Hardness Testing 8
Tensile Testing 10
High Strain Rate Tensile Testing 10
Impact 10
Metallurgical Analysis 12
Metallography 12
3 Results and Discussion . 12
Task I - Thermomechanical Processing 12
Background 12
Scope 13
Material 13
Thermomechanical Processing Studies . . . . 17
Task II - Alloy Improvement 21
Background 21
Scope 24
Material, Series "A" 24
Table of Contents (Continued)
Section Title Page No.
3 (Cont'd) Material, Series "B" . . . . . . . . . . . . V . 25 '
Evaluation 26
Chemistry 26
Mechanical Properties 27
Task III - Property Evaluation 27
Scope 27
Material . .. 27
Physical Properties 29
Thermal Expansion 29
Density . . . . . . . . . . 2 9
Mechanical Properties 29
Hardness Testing 31
Impact Evaluation • 31
Creep Rupture 31
Task IV - VM-103 Procurement Specification ... 37
4 Summary of Results . . . 41
5 Concluding Remarks . . . . . . 4 . : . . 42
References 44
Appendix A 46
LIST OF TABLES
Table Title Page No.
I Chemical Analyses of Task I Material 5
II Melting Practice and Chemical CompositionVariables Investigated 5
III Chemical Analysis of Standard and Modified VM-10.3Heats 6
IV High Strain Rate Tensile Properties of ESR Heat PF-11 . 16
V Hardness of VM-103 After Thermomechanical Processing 19
VI Tensile Data for Thermomechanically Processed VM-103 20
VII VM-103 High Strain Rate Tensile Data . . 22
VIII Conventional and High Strain Rate Tensile Propertiesof Solution Heat Treated VM-103 . ' . . . ' 23
IX Hardness of VM-103 Sheet as a Function of Chemistryand Cold Work ' ' . . . . . . . . 25
X Mechanical Properties of Standard and Modified VM-103. 28
XI Mechanical Properties of Standard and ModifiedVM-103 Heats Al, B3 and B4 32
XII Hot Hardness of VM-103, Heats B3 and B4 34
XIII Impact Strength of VM-103, Heats B3 and B4 35
XIV Creep Rupture Properties of Wrought and Cast VM-103 . 39
LIST OF ILLUSTRATIONS
Figure Title Page No.
1 VM-103 Alloy Development . 3
2 Aging Parameters and Resulting Hardness .9
3 VM-103 Sheet Tensile Specimen . 11
4 Hardness VS. Percent Cold Reduction of VM-103 ... 14
5 Effect of Aging Time at Indicated Temperature . . . . 15
6 Thermomechanical Processing Variables 18
7 Thermal Expansion of VM-103 30
8 . Mechanical Properties of VM-103 as a Function ofTest Temperatures 33
9 VM-103 Creep Rupture Specimens Casting . . . . . . . 36
10 Creep Rupture Properties of Wrought VM-103 . . . . 38
11 Creep Rupture Properties of Cast VM-103 . . . . . . 40
1. INTRODUCTION
During 1968 and 1969 in the interest of meeting the demands forhigher temperature, higher strength alloys created by advanced propulsionand ordnance programs, Aeronutronic conducted a development programinvolving NASA's high strength cobalt base superalloy (Co-25W-3Cr-lTi-. 5 Zr-. 5C), designated as VM-103. This alloy is one of a series of NASAalloys that shows potential for application to gas turbine engine components,i. e. , stator vanes, combustion chamber liners, and high temperature duct-ing. The alloy also appears competitive with conventional wrought nickeland cobalt base superalloys such as Rene 41, Hastelloy X, Waspaloy, andL-605 for advanced ramjet, scramjet, and rocket engine components. VM-103appeared particularly promising for short-term, high temperature applica-tions associated with advanced missile guidance systems, i. e. , hot gas valves,hydraulic power units, and steering fin actuators, and also for high cyclicrate gun components such as barrels, barrel-liners, or muzzle breaks.
Aeronutronic's program on the alloy consisted of an assessment of thealloy's capability to satisfy design requirements for various missile, propul-sion, and gun components. Conventional and high strain rate tensile tests,electron beam welding, preliminary hot and cold working of the alloy, andcold forming and testing of hot gas valve components were accomplished.The results confirmed the apparent applicability of the alloy for the afore-mentioned high temperature applications.
As an initial step toward advancing the alloy beyond its researchstatus, Aeronutronic then conducted alloy optimization studies for purposes ofdetermining castability and cast properties and to optimize carbon content.Following this, four heats of the alloy were produced utilizing two productionoriented melting processes, i. e. , vacuum arc remelting (VAR) and electro-slag remelting (ESR). The heats were characterized with respect tomicrostructure and composition, and preliminary forging trials were madewhich confirmed the adaptability of the alloy to production processes.
Under Contract NAS3-12421, "Development and Metallurgy Studyof a NASA Cobalt Base Superalloy, " an extensive effort was performed withthe objective of further advancing the status of VM-103 from that of researchtoward production. Hot and cold working parameters, and solution and agingheat treatments, were established; room and elevated temperature conven-tional and high strain rate tensile properties were developed, and a
microstructure and phase identification study was performed. Comparativefabricability and properties of two melting processes showed that ESR appearsmore favorable than the VAR process for this alloy.
A flow chart showing VM-103 development from the early NASA 1700 gheats through Contract NAS3-12421 is shown in Figure 1. All VM-103 R&Defforts were very encouraging and indicated that VM-103 had good potentialfor an ultimate production high temperature superalloy. However, during /-jthe earlier work, various areas requiring further development were identified*There were indications that further work to optimize chemical composition andprocessing parameters would be useful in efforts to further improve fabrica-bility and mechanical properties. Effects of selected alloying additions andof alloy impurities remained unknown. In addition, earlier data indicatedthat VM-103 might be responsive to thermomechanical processing .treatmentswhich was considered worthy of investigation for enhancing mechanicalproperties.
The objective of the program covered in this report was to furtherevaluate the effects of the chemistry variation and processing variables o.nthe mechanical and physical properties of NASA alloy VM-103. A secondaryobjective was to develop sufficient data so that a procurement specificationfor VM-103 could be prepared.
The program was divided into four tasks, briefly described below:
Task I - Thermomechanical Processing
. The goal of this task was to develop thermomechanicalprocessing parameters to enhance the mechanicalproperties of VM-103, particularly in the 1800-2200°F(982-1204°C) range.
Task II - Alloy Improvement
This task was designed to investigate the effects of meltingtechnique, impurities, and alloy additions on the fabrica-bility and properties of VM-103. Further improvement of .electroslag remelted (ESR) material properties were alsoinvestigated.
Task III - Property Evaluation
This task was to determine additional design propertydata on VM-103 such as impact strength, hot hardness,coefficient of thermal expansion, density, and creeprupture.
BASELINE NASA RESEARCH DATA ON Co-W ALLOY SYSTEMS
1700 g INDUCTION HEATS WERE USED FORESTABLISHMENT OF Co-25W-3Cr-.5 Zr-.4C COMPOSITION
- CAST TENSILE AND STRESS RUPTURE- HOT AND COLD WORKABILITY DATA- LIMITED WROUGHT TENSILE DATA- PRELIMINARY TIG WELDING DATA
H I G H STRAIN TEST [FABRICATION OF 0.012" FOIL |COMPARING WITHL-605 AtJD RENE 41
RT - 2200°F (1204°C) COLD FORMING HOT GAS
VALVE DIAPHRAGM
COLD CYCLE FATIGUE
ELECTRON BEAM WELDING TRIALS
IJTENSILE, RT [
CARBON CONTENT INVESTIGATION5 Ib. (2.3 kg) VACUUM INDUCTION HEATS
CAST PROPERTIES TENSILERT to 2200°F (1204°C)
HOT AND COLDWORKABILITY STUDIES
[RECOMMENDATION FOR o.sc CONTENT
PRODUCTION OF 4 In. (10 cm) DIA. 25 Ib. (11.3 kg)VACUUM INDUCTION MELTED +VACUUM ARC REMELTED HEATS
PRODUCTION OF 4 in. (10 cm) DIA. 50 Ib. (22.6 kg)INERT ATMOSPHERE INDUCTION +
ELECTROSLAG REMELTED HEATS ^
FABRICATION AND TESTINGOF HOT GAS VALVEr
RESTRICTORS AND GUN BARRELS
ESTABLISHMENT OF OPTIMUMS.H.T. PARAMETERS
ESTABLISHMENT OF COLD.WORKING PARAMETERS
[ PRELIMINARY FATIGUE I-
PRELIMINARY ESTABLISHMENTOF AGING EFFECTS
PRELIMINARY ESTABLISHMENT OF
RECRYSTALLIZATION BEHAVIOR
PRELIMINARY- FORGING TRIALS
HOT WORKING STUDIES
(CONTRACT NAS3-12421)
FORGE TO 1 in. (2.5 cm)ROLL TO 0.1 in. (25 cm)
ESTABLISHMENT OF OPTIMUMHOT WORKING PARAMETERS .[..
COLD WORKING STUDIESCOLD ROLL TO 0.012 in. (0.03 cm)
- HARDNESS VS. 7. C.W.
MECHANICAL PROPERTY EVALUATION
CONVENTIONAL AND HIGH STRAINRATE TENSILE DATA ON
ANNEALED AND COLD WORKEDMATERIAL RT TO 2200°F (12048C)
METALLURGY STUDYX-RAY DIFFRACTION, OPTICAL
AND ELECTRON MICROSCOPYPHASE IDENTIFICATION
RECOMMENDATIONS FOR ESR VS. VAR PROCESS
RECOMMENDATIONS FOR FURTHER DEVELOPMENTAND ALLOY IMPROVEMENT
(CONTRACT NAS3-12421)
FIGURE 1. VM-103 ALLOY DEVELOPMENT
Task IV - VM-103 Procurement Specification
The objective of this task was to prepare procurementspecifications for wrought VM-103 based on existinginformation and additional data developed by Tasks I,II and III of this program.
2. PROCEDURE
Material
The early work on VM-103 was conducted on small 3-4 pound (^2 kg)vacuum or inert atmosphere, single induction melted laboratory type heats.The melting practices were upgraded by Contract NAS3-12421 to more con-ventional superalloy production, i. e. , duplex melting practices consistingof vacuum induction melting (VIM) plus vacuum arc remelting (VAR) andvacuum induction melting (VIM) plus electroslag remelting (ESR). ESR is arelatively new process that is similar in principle to the VAR process. Bothprocesses start with a VIM cast electrode, the VAR material is arc remeltedin a vacuum to reduce microsegregation inherent in VIM material. To reducevolatile type impurities by allowing the molten material to outgas: the ESRmaterial is also arc remelted from VIM material; however, the melting occursin a specially prepared molten slag blanket which reacts with the volatilematerials and some of the nonvolatile impurities. The ESR melting practicehas been shown to generally improve such properties as ductility, fabrica-bility, fatigue strength and fracture toughness of various steels and nickelbase superalloys. ( ' '.
The Task I thermomechanical processing phase of the current programwas conducted on residual material (Heats PF-11 and PF-288) from ContractNAS3-124213. Heats PF-11 and PF-288 were 50 pound (23 kg) ESR materialsupplied by ESCO Corporation, Portland, Oregon. Chemistry analyses ofthe two heats are presented in Table I; all metallic elements reported weredetermined by X-ray spectroscopy, the carbon was determined by gas analysis.Although these heats did not meet the VM-103 target analyses for tungstenand zirconium the material was considered acceptable for the thermomechanicalprocessing portion of the program.
The Task II Alloy Improvement phase of the program was designedto evaluate the effect of melting processes and of selective alloy additions onthe fabricability and mechanical properties of the basic VM-103 alloy. Eight5-10 pound (2. 3 - 4. 5 kg) heats listed in Table II were melted during theTask II phase of the program. Two additional heats of the B3 compositionwere melted by the VIM process and cast directly into round tensile speci-mens for creep rupture evaluation during Task III. Table III shows thechemical analyses of all the heats used in the program.
TABLE I .
CHEMICAL ANALYSES OF TASK I MATERIAL(Weight Percent)
Elements
TungstenChromiumTitaniumZirconiumCarbonIron
^Cobalt
Target Analysis
25310.50.50.1 Max.Balance
Heat Number
PF-11
24.132.510.950.250.501.08
Balance
. PF-288
28.153.001.060.240.450.16Balance
TABLE II
MELTING PRACTICE AND CHEMICAL COMPOSITION VARIABLES INVESTIGATED
Heat.'Number
Al
A2
A3
Bl
B2
B3
B4
MeltingPractice
VIM(a)
VIM
VIM
VIM
VIM
VIM + ESR^
VIM + ESR
(c)Target Composition
Standard VM-103
Standard VM-103 +
Standard VM-103 +
Standard VM-103 +
Standard VM-103 ++ 0.25-0.507, Mn .
Standard VM-103 +
Standard VM-103
107, Ni
107, Ni + 57, Fe
0.25-0.507, Si + 0.25-0.507, Mn
107, Ni + 0.25-0.507, Si
107, Ni
(a)
(b)
(c)
VIM = Vacuum Induction Melti
ESR = Electroslag Remelt
Standard VM-103 Composition 257, W, 37, Cr, 17, Ti, 0.57, Zr, 0.57, C,0.1 max Fe and balance Co. • .
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Ingot Reduction
Forging
The cast ingots were conditioned for forging by grit blasting toremove any surface impurities and allow assessment of the ingot quality.Surface imperfections were removed by hand grinding of local defects or roughturning to remove more severe conditions. The pipe or suckback on the top ofthe ingot was removed by sectioning and hand grinding as required.
The forging was conducted at West Coast Forge, Compton,California, with a 3500 pound (15, 900 N) hammer forge. The 4 inch (10 cm)diameter ingots were forged to 1 x 1 inch (2. 5.x 2. 5 cm) bar using the para-meters developed on Contract NAS3-12421 and listed below:
(1) Soak at 2175°F (1190°C) for 1/2 hour.
(2) Forge in radial direction to 3 x 3 in.(7. 6 x 7. 6 cm) square using reductions ofapproximately 8-10 percent.
(3) Return to furnace after each reduction; soak .at temperature for 15 minutes.
(4) Forge to 1 x 1 in. (2. 5 x 2 . 5 cm) squareusing 15-20 percent reductions.
(5) Return to furnace after each reduction; soakat temperature for 10 minutes.
(6) After last pass, soak at 2200°F (1204°C) for10 minutes and water quench.
(7) Inspect after each reduction; grind or cropany surface defects as required.
Rolling
The 1x1 inch ( 2 . 5 x 2 . 5 cm) forged bar was further reduced to0. 10 inch. (0. 25 cm) at Aeronutronic by the optimum hot rolling techniquesdeveloped on Contract NAS3-12421. 3 The bars were preheated at 2175 F(1190°C) for 30 minutes and rolled on a 2 high - 4 high rolling mill. Theinitial passes were limited to 12-15 percent with subsequent reductions of15-35 percent. The material was reheated between passes at 2175°F (1190°C)for 3 to 10 minutes, depending.on the material thickness and soaked at 2200°F(1204°C) for 10 minutes and water quenched after the last pass. Test sampleswere given additional reductions by combinations of hot and cold rolling toinvestigate the effect of thermomechanical processing on the VM-103 alloy.Cold reductions of up to 40 percent were evaluated.
Heat Treatment
Solution Heat Treatment
The optimum solution heat treatments with respect to minimumhardness, minimum grain growth and minimum matrix or grain boundarycarbide precipitation was established during Contract NAS3-12421. Theoptimum solution heat treatment was 2200°F (1204°C) for 30 minutes followedby a water quench. The samples were processed in a circulating air atmos-phere furnace and subsequently grit blasted to remove the oxide scale.
The VM-103 alloy was designed to be a solid solution strengthenedalloy; however, preliminary NASA data and data generated on Contract NAS3-12421 indicated a potential aging phenomenon. Aging studies were used inconjunction with prior annealing or cold reduction to investigate thermo-mechanical processing as a useful strengthening mechanism for elevatedtemperature 2000-2200°F (1093-1204°C) service. Samples were encapsulatedin quartz tubes, evacuated to 10"-* torr and sealed to prevent oxidation duringaging at the time-temperature combinations shown by Figure 2. Hardnessmeasurements, metallography and mechanical testing of selected sampleswere utilized to evaluate the aging effects.
Mechanical Testing
Hardness Testing
Room temperature hardness tests were conducted with a standardRockwell hardness tester. Samples were evaluated throughout the program asan indication of the effects of processing on the VM-103 material.
Hot hardness measurements were taken at 1000, 1200, 1400 and1600°F (538, 649, 760 and 871°C) with a standard Wilson Rockwell hot hard-ness tester on samples from two VM-103 heats (B3 and B4) in the followingconditions:
(1) Solution heat treated.
(2) Solution heat treated plus aged.
(3) Solution heat treated plus 25 percent reductionat 75°F (24°C). \
(4) Solution heat treated plus 25 percent reduction at75°F (24°C) plus aged.
Solution heat treated = 2200°F (1204°C) for-1/2 hour, water quench
Aged = 1300°F (704°C) for 10 hours.
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Samples approximately 1/2 x 2 x 0. 100 inch (1. 3 x 5. 1 x 0. 25 cm)with an 0. 125 inch (0. 317 cm) diameter hole drilled approximately half waythrough the specimen were used in the evaluation. The specimen tempera-ture was measured with a thermocouple inserted in the hole. Each samplewas heated to 1000°F (538°C) held for 15 minutes and evaluated using astandard Wilson hot hardness tester , then raised to the next higher tempera-ture.
Tensile Testing
The room and elevated tensile properties of annealed and thermallyprocessed material were determined on a 10, 000 pound (44, 500 N) capacityInstron testing machine equipped with a 2200°F (1204°C) resistance furnace.The specimens were brought from ambient to test temperature in about 30minutes, soaked at temperature for an additional 15 minutes and then testedat a strain rate of 0. 005/minute to 0. 4 percent offset yield followed by0. 05/minute to failure. An extensometer was used for measuring strainuntil about 1 percent elongation. The specimens were machined to the con-figuration shown in Figure 3.
High Strain Rate Tensile Testing
Rectangular sheet specimens, 4 x 0. 25 inch (10 x 0. 6 cm) werefabricated from 0. 040 inch (0. 1 cm) thick sheet material with various ,amounts of thermomechanical processing. The specimens were tested ona "Gleeble" machine at a strain rate of 5/minute at temperatures of 75,1200, 1600, 1800, 2000 and 2200°F (23, 649, 871, 982, 1093 and 1204°C).The samples were electrically self-resistance heated at a rate of approximately500°F (260°C)/second, and held at temperature either for 5 or 30 seconds priorto application of the load.
Impact
Standard V notch Charpy impact specimens were machined frommaterial from heats B3 and B4 in the following conditions:
(1) Solution heat treated.
(2) Solution heat treated plus aged.
(3) Solution heat treated plus 25 percent reduction at75°F (24°C).
(4) Solution heat treated plus 25 percent reduction at75°F (24°C) plus aged.
Solution heat treated = 2200°F (1204°C) for1/2 hour, water quench
Aged = 1300°F (704°C) for 10 hours.
Duplicate specimens were evaluated at room temperature and -65°F (-54 C).
10
0.375 -±0.010
0.50 R
W +0.002+0.001
0.250 ±0.005
3.500 ±0.010
0.125 DRILL2 HOLES
0.500±0.010
FIGURE 3. VM-103 SHEET TENSILE SPECIMEN.(ALL DIMENSIONS IN INCHES)
"- 0.040±0.003
11
Metallurgical Analysis
Metallography
Selected samples were prepared for metallographic observa-tion using the following method:
(1) Successive grinding on 180, 240, 360 and 600grit silicon carbide.
(2) Polish on 6 micron diamond followed by1 micron diamond.
(3) Final polish on 0. 05 micron alumina.
(4) Etch by swabbing for 4 to 8 seconds withhydrochloric acid saturated with ferric chloride-
(5) Ultrasonically clean for 2 to 3 minutes indistilled water.
A Leitz MM-5 metallograph was used for optical microscopy andphotographed using bright field illumination. Observations were made atmagnifications from 100 to 1000X. Grain size measurements were obtainedusing the ASTM-E-112 linear intercept method. The reported grain sizesrefer to the calculated "diameter" of an average grain with a mean standarddeviation of +_ 10 percent.
3. RESULTS AND DISCUSSION
Task I - Thermomechanical Processing
Background
. One of the state-of-the-art methods for improving the mechan-ical properties of metallic systems is through thermomechanical processing.The majority of thermomechanical processing studies have been related tosteels, ^» -> although some work has been conducted on aluminum^"" andsuper alloys"" . Basically, thermomechanical processing involves combina-tion of thermal and deformation treatments that result in a rearrangement ofthe defect and minor phase structure with corresponding changes in themechanical properties. Strengthening effects result from an increased andmore uniform dislocation density which is achieved through thermomechanicalprocessing by different mechanisms depending on the alloy system and priortreatment*. In steels, thermomechanical processing increases dislocationdensity primarily through working; precipitates increase this effect but to aminor extent.
In other systems such as the aluminum alloys an increased numberof nucleation sites for the precipitation hardening reaction are generated inaddition to the more uniform and increased matrix strengthening'. Moreuniform matrix precipitates can also be achieved in cobalt-base alloys suchas L-605 by aging deformed material^ . By selection of proper thermomechan-ical processing parameters for deformation and aging treatments it is possibleto obtain an alloy with a uniform secondary phase distribution. .The processmay result in increased alloy strength by hindering dislocation motion throughinteraction with other dislocations or phases. However, the ductility is notnecessarily reduced to the. same degree as for conventionally processedmaterials of the same strength. This can be explained by the fact that a moreuniform deformation occurs by the movement of a greater number of dis- ,locations over a small area per dislocation.
Data generated on Contract NAS3-124213 indicated that VM-103may be responsive to thermomechanical treatments as a means for achievingimproved mechanical properties. In particular the data showed:
(1) Rapid work hardening characteristics as shownin Figure 4. •
. (2 ) . Response of cold worked and solution heat treated,material in aging treatments as shown in Figure 5.
(3) Beneficial effects of aging solution heat treatedmaterial resulting in an increase in 2200°F(1204°C) yield strength from 4. 1 to 10. 1 ksi(28. 4 to 69. 7 N/mm2) or 140 percent.
(4) A possible rapid aging effect evidenced by vary-ing the holding times on elevated temperaturehigh-strain rate tests, Table IV.
Scope
Task I was designed to develop thermomechanical processingparameters to enhancing the mechanical properties of VM-103, in the 1800to 2200°F (982 to 1204°C) range.
Material
As indicated above, residual material from Contract NAS3-12421was utilized for the Task I thermomechanical processing evaluation. Two50-pound (23 kg) electroslag remelted heats (PF-11 and PF-288) were suppliedby ESCO Corporation, Portland, Oregon. The chemical analysis of the twoheats are presented in Table I. The cast ingots were forged from a 4 inch(10 cm) diameter to a 1 x 1 inch (2. 5 x 2. 5 cm) square bar and solution heattreated at 2200°F (1204°C) for 1/2 hour and water quenched without coolingfrom the forging operation. The material was subsequently hot rolled tovarious thicknesses and resolution heat treated to provide starting materialfor the thermomechanical processing study.
13
Symbol
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A
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Percent Cold Reduction
Melting Process
VAR
VAR
ESR
ESR
Heat Number
20-1
20-5
PF-11
PF-13
VAR: Vacuum Arc Remelt
ESR: Electroslag Remelt
FIGURE 4. HARDNESS VS. PERCENT COLD REDUCTION OF VM-103(3)
14
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0 (Unaged) 1 10 100 1000Aging Time, Hours
FIGURE 5A. EFFECT OF AGING TIME AT INDICATED TEMPERATUREON THE HARDNESS OF SOLUTION HEAT TREATED VM-103
1000°F (538°C)
400 (Unaged) 1 10 100 1000
Aging Time, Hours
FIGURE 5B. EFFECT OF AGING TIME AT INDICATED TEMPERATUREON THE HARDNESS OF 15% REDUCTION 75°F (24°C) VM-103
400 (Unagea) 1 10 100 1000
Aging Time, Hours
FIGURE 5C. EFFECT OF AGING TIME AT INDICATED TEMPERATUREON THE HARDNESS OF 25% REDUCTION (75°F (24°C) VM-103
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Thermomechanical Processing Studies
Early NASA data indicated an aging phenomenon in VM-103 par-ticularly in the 1600°F (871°C) range, resulting from the precipitation of a Co-^Wphase. One goal of the NAS3-12421-3 program was to achieve a better under-standing of this effect and to determine if aging would be useful as a strength-ening mechanism. Specimens representing annealed and 25 percent cold workedsheet were encapsulated in evacuated quartz tubes and aged for one, ten and100 hours at temperatures of 700, 1000, 1300 and 1600°F (371, 538, 704 and871°C). The current program expanded the previous work to include 15 percentcold worked material and lengthened the exposure periods to 1000 hours. Thecomplete test matrix and results obtained from both programs on heat PF-11are shown in Figure 2, the results are also presented graphically in Figure 5A,B and C.
Based on the hardness results, the aging studies showed that thealloy is significantly responsive to age hardening at 1300°F (704°C) both in thesolution treated and cold worked conditions. The 25 percent cold workedmaterial exhibited a decrease in hardness when aged for extended periods at1600°F (871°C). Material with 15 percent cold worked showed a similar,behavior when aged at 700, 1000 and 1300°F (371, 538 and 704°C), the hardnesswas about two Rockwell "C" points below that obtained for the 25 percent coldworked material.
Samples of VM-103 sheet from heat PF-288 were subjected toapproximately 40 variations in thermomechanical processing combinations ofcold, warm and hot rolling, aging at various times and temperatures. Figure 6shows a flow sheet for the thermomechanical process and the resulting roomtemperature hardness values are shown by Table V. Some of the processingparameters increased the hardness from approximately Rc 35 to Rc 57. 5 andabove. The nine processes, (3, 7, 13, 21, 29, 37, 41, 42 and 43, Table VI)resulting in the maximum room temperature hardness were selected fortensile testing and compared to solution treated material.
Tensile specimens of the configuration shown by Figure 3 wereevaluated at 2000 and 2200°F (1093 and 1204°C). The test parameters includeda soak period of 5 minutes and a strain rate of 0. 005/minute to yield followedby 0. 05/minute to failure. The results shown by Table VI did not reveal anysignificant improvements under these test conditions indicating that anybeneficial effects of aging or thermomechanical processing were annealed awayrather quickly at 2000 and 2200°F (1093 and 1204°C) and the resulting strengthswere not significantly different from the solution treated material. Effects ofaging or thermomechanical processing for very short times and under high strainrate conditions at 2000 and 2200°F (1093 and 1204°C) were also determined.The samples previously processed for evaluation of the thermomechanical pro-cesses were subjected to 5 and 25 second soak times in a salt bath at 2000 and2200°F (1093 and 1204°C) followed by a water quench. The resulting roomtemperature hardness values are presented in Table V. Five processes (4,24, 32, 42 and 45) were selected for additional testing under high strain-rate
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conditions, i. e. , 5/minute with a heating rate of 500°F/ second (260°C/ second)and a soaking time of 5 seconds. The processes listed above and the resultingdata are shown by Table VII. The results showed no real benefit from thethermomechanical processing of VM-103. However, for comparison, L-605specimens were tested under similar conditions (Table VII) and the solutiontreated VM-103 showed 40 percent higher yield strengths. The data indicatedthat although thermomechanical processing provides little or no benefit atthese temperatures, solution treated VM-103 still appears attractive as areplacement for L-605 for various high temperature applications.
The final testing effort for Task I involved the generation of con-ventional and high strain rate tensile data on solution heat treated VM-103.Based on the results discussed above, solution heat treated VM-103 wasselected and evaluated at 75, 1200, 1600, 1800, 2000 and 2200°F (24, 649,871, 982, 1093 and 1204°C). The results are shown by Table VIII.
Task II Alloy Improvement
Background
Although VM-103 appeared very promising, the data indicatedthe possibility that slightly more exploratory development with respect tocomposition and impurity level could yield even a more promising alloy. Itis also important to understand more fully the effects of impurities andcompositional tolerances in order to ultimately write a procurement spec-ification that can be met with minimum cost. Such information is alsoimportant as a basis for any other future superalloy development work.
So far, little attention had been paid to sulphur, potassium,manganese or silicon contents of VM-103, the philosophy being to keep theseelements as low as possible on a best efforts basis. Earlier work on L-605incicated that silicon aggravates an embrittling effect resulting from precip-itation of a Laves phase (Co2W) after prolonged exposure to 1600°F (871°C)12> 13
Because early NASA research and Contract NAS3-12421^ work showed a similaragi-ng phenomenon in VM-103, resulting primarily from 003W precipitation,the effects of silicon appeared worthy of investigation. Where short termproperties are of particular interest the silicon content could be adjusted totake advantage of the increased mechanical properties.
Other data have shown possible beneficial effects of manganesewith respect to fabricability of L-605. The manganese content of L-605 isspecified a.s 1 to 2 percent, and published data, although inconclusive,indicated that the higher region of this range was desirable for increasedfabricability^. The beneficial effect of manganese in steels is also wellknown and it was believed that similar effects might occur on the VM-103 alloy.
Wlodek has indicated that high iron contents are beneficial in L-605with respect to retarding long term embrittlement. NASA data have shown thatiron stabilizes the face centered cubic to hexagonal transition, thereby reducing
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the tendency for hexagonal stacking faults which serve as nucleation sites forembrittling precipitates. NASA data have also indicated detrimental effectson cast VM-103 with iron and nickel in excess of 3 percent with respect to1850°F (1010°C) stress rupture strength* . Based on this information it wasconsidered that small iron or nickel additions on the order of 2 percent mightbe of value in retarding long term embrittlement without a sacrifice in shorttime high temperature properties.
Early NASA data showed slightly better mechanical propertiesresulting from inert atmosphere induction melting compared to vacuum melting.Differences in properties and fabricability resulting from vacuum arc remeltingand electroslag remelting have also been observed. These effects indicate apossible gas content variation as a function of melting practice which may affectthe properties of the alloy.
This task was designed to investigate the effects of melting tech-niques, impurities, and alloy additions on the fabricability and properties ofthe VM-103 alloy. This was to be accomplished by melting, processing andevaluating two series of heats designated as "A" and "B", each including thestandard VM-103 composition and selected alloying additions.
Material, Series "A"
Three 5-10 pound (2. 3 - 4. 5 kg), 2 inch (5. 1 cm) diameter heatswere vacuum induction melted at Aeronutronic. The heats were designated asAl, standard VM-103 composition; A2, standard VM-103 composition plus 10percent nickel; and A3, standard VM-103 composition plus 10 percent nickel and5 percent iron. The target compositions were achieved with reasonable success,the chemical analyses of the ingots are presented by Table III. The iron lossduring the melting of heat A3 was greater than anticipated, yielding only 4. 1percent instead of the target 5 percent.
The ingots were machined into round-corner-square configurationsand hot rolled to 0. 100 inch (0. 25 cm) thick sheet using identical rollingschedules, as established under Contract NAS3-1242 1-^and discussed inSection 3 of this report. The material was s.olution heat treated at 2200°F(1204°C) for one-half hour and water quenched after the hot rolling. Thematerial was subsequently hot and cold rolled to provide 0. 040 inch (0. 1 cm)thick sheet with 0, 15, 25 and 40 percent cold work for tensile testing. Althoughall three heats could be cold reduced as much as 25 percent with no difficulty,the standard VM-103 composition heat, Al, showed edge cracking at coldreductions of about 40 percent. The nickel and iron additions improved boththe hot and cold workabilities of the VM-103 alloy. In general the fabrica-bilities could be rated from best to poorest as A3, A2, and Al, respectively.The hardness data shown by Table IX as a function of cold work indicated thatthe two modified heats were considerably softer than the standard VM-103composition, which correlates with their improved workabilities.
24
TABLE IX
HARDNESS OF VM-103 SHEET
AS A FUNCTION OF CHEMISTRY AND COLD WORK
HeatNo.
Al
A2
A3
Bl
B2
B3
B4
NominalComposition
Std. VM-103
Std. VM-103 +10% Ni
Std. VM-103 +10% Ni = 5% Fe
Std. VM-103 +~ . 35 Si +~ . 35 Mn
Std. VM-103 +10% Ni +~ . 35 S+ ~ . 35 Mn
Std. VM-103 +10% Ni
Std. VM-103
MeltingProcess
VIM
VIM
VIM
VIM
VIM
ESR
ESR
SolutionHeat
TreatedR c
34. 5
25
24
33
27
31
35
Gold Work
15% Rc
47
41
40
46. 5
30
46
48
25% Rc
48
45
43
49
43. 5
48
50. 5
40% Rc
49. 5
47
45
52
48
50. 5
52. 5
Solution Heat Treat = 2200°F (1204°C), 1/2 hours water quench
VIM = Vacuum Induction Melted
ESR = Electroslag Remelted
Material, Series. "B"
Four 5-10 pound (2. 3 - 4. 5 kg), 2 inch (5. 1 cm) diameter heats werevacuum induction melted at Aeronutronic. The heats were designated asBl, standard VM-103 composition + 0. 25-0. 50 Si + 0. 25-0. 50 Mn; B2, standard
25
VM-103 composition + 10 percent Ni + 0. 25-0. 50 Si + 0. 25-0. 50 Mn; B3, stand-ard VM-103 composition + 10 percent Ni; and B4, standard VM-103. The 2 inch(5. 1 cm) diameter vacuum induction melted B3 and B4 material was electro -slag remelted into 4 inch (10. 2 cm) diameter ingots. All the ingots wereconditioned for forging by O. D. machining and local grinding to remove minorsurface impurifications. The "B" series material was forged to a 1 inch (2. 5 cm)square bar using the techniques developed on Contract NAS3-1242l3 and dis-cussed in Section 3, "Ingot Reduction. " The Bl ingot showed the usual edgecracking but forged reasonably well. Heat B2 caused considerable difficultyduring forging and was almost completely lost during subsequent hot rolling.The problems were partially attributed to porosity in the cast ingot; therefore,a new heat with the same nominal composition designated B2-2 (Table III) wasmelted. The ingot was machined to a round-cornered-square and hot rolledusing the same parameters that were successful in processing the Series Aheats. Nearly all of the material was lost due to breakup during rolling,indicating poor hot workability. However, sufficient quantities were salvagedfor a partial evaluation. The electroslag remelted material, heats B3 and B4forged very well with a 100 percent yield, thus again, indicating the superiorhot workability of the electroslag remelted material.
The hardness as a function of cold work reported in Table IXindicated that the work hardening characteristics of the standard VM.-103composition were slightly reduced by the addition of 10% nickel as shown bya comparison of heats Al and A2 and heats B3 and B4. This lowering effect .was further accentuated by adding 10% nickel plus 5% iron, as shown by heatA3. Although the hardness values for heats Bl and B2 do not indicate anyincrease in the cold work hardening characteristics, these heats showedextremely poor fabricability during hot forging and rolling.
Evaluation
Chemistry
Samples from the various ingots were chemically analyzed forthe alloying components of VM-103 as well as the elements used in the modifiedcompositions. The metallic elements were analyzed by X-ray spectroscopyand the gas and carbon by vacuum techniques. The results, shown by Table III,indicate reasonable success in controlling composition during melting and cast-ing the VM-103 alloy by induction and electroslag remelting. The effect ofinterstitial content on the VM-103 alloy was considered in the evaluation;however, no provisions were made to purposely increase the interstitial con-tent of the various heats during the melting cycle. The chemistry resultsshown by Table III indicate that the various levels obtained were consistentfrom heat-to-heat and did not indicate any significant trends in the data.
26
Mechanical Properties
Tensile specimens were fabricated from each of the seven heatsfor testing in the following conditions:
Condition
SHT
SHT + Aged
SHT + 25% Reduction
Test Temperature
75°F (24°C)
X
X
X
2000°F (1093°C)
X
X
SHT: Solution Heat Treated 2200°F (1204°C), 1/2 hour, water quench
Aged: 1300°F (704°C) 10 hours, air cool
25% Reduction: 25% Reduction at 75°F (24°C)
The results of the evaluation (Table X) showed a significant increase inductility for heats A2 and B3 with the 10 percent nickel addition with only asmall decrease in strength. No significant increase in tensile strengthresulted from the additions of silicon and manganese to heats Bl and B2iHeats Al, B3 and B4 were selected for additional evaluation.
Task III Property Evaluation
Considerable data have been generated on VM-103, particularlyshort time tensile data as reported in NASA CR-72726 . For high tempera-ture applications of the alloy, additional properties such as tensile strength,creep rupture, hardness, thermal expansion and thermal conductivity overthe temperature range from 1200°F to 2000°F (649 to 1093°C) were requiredfor design purposes.
The scope of this task was to determine additional design propertydata on standard and modified compositions of the VM-103 alloy. The standardcomposition and the 10 percent nickel modification were selected as the mostpromising alloys from Task II.
Material
The material required for this phase of the program was producedduring the Alloy Improvement phase by the techniques discussed in Task II.Heat Al induction melted standard VM-103 composition, heat B3 inductionplus electroslag remelted standard VM-103 + 10% nickel composition andheat B4 electroslag remelted standard VM-103 were selected for evaluation.The chemical analysis of the three heats are presented in Table III.
27
TABLE X
MECHANICAL PROPERTIES OF STANDARD AND MODIFIED VM-103
Condition
SHT
SHT
SHT + AGE
SHT + AGE
SHT + 25% Red
HeatNo.
AlA2A3BlB2B3B4
AlA2A3BlB2B3B4
AlA2A3BlB2B3B4
AlA2A3BlB2B3B4
AlA2A3BlB2B3B4
Test Temp
°F
75757575757575
2000200020002000200020002000
75757575757575
2000200020002000200020002000
75757575757575
°C
242424'24242424
1093109310931093109310931093
24242424242424
1093109310931093109310931093
24242424242424
0.2% OffsetYieldStrength
psi
88.273.372.186.476.676.590.5
17.316.914.111.811.110.213.7
144.4114.586.2149.9129.4110.9133.1
12.511.611.510.610.210.513.2
152.9172.8170.2150.9154.7166.3165.7
N/mm2
608505497595527527624
1191169781767094
9957895941033892764917
86807973707291
1053119111731040106611461142
UltimateTensileStrength
ksi
138.7140.8133.4149.5144.7156.2150.8
20.420.616.716.116.416.718.7
174.8159.7133.1176.9177.7176.0167.2
19.317.317.417.115. .616.119.6
204.1202.2198.0237.7206.8204.9251.4
N/mm2
956970919103099710761039
141142 '•115111113115129
120411009171218122412131152
133119119118107111135
1406139313641638'142514121732
Elongationin 1 in . or2.5 cm, %
9.523.522.517.527.335.515.0
11.512.311.839.527.041.031.5
2.511.713.05.0
13.513.23.0
23.530.530.546.035.533.522.0
4.35.35.02.85.810.02.5
SHT = Solution heat treat, 2200°F (1204°C), 1/2 hour water quench
AGE = 1300°F (704°C), 10 hours air cool
25% Red = 25% Reduction at 75°F (24°C
Heat Nos: Al - Standard VM-103, (VIM)A2 . - Standard VM-103 + 10% Ni, (VIM)A3 - Standard VM-103 +10% Ni, (VIM)Bl - Standard VM-103 + ~ .35 Si + ~ .35 Mn (VIM)B2 - Standard VM-103 + 10% Ni.+ ~ .35 Si +~ .35 Mn (VIM)B3 - Standard VM-103 + 10% Ni (ESR)B4 - Standard VM-103 (ESR)
28
Physical Properties
Thermal Expansion
The thermal expansion of a sample of induction melted standardVM-103 composition from heat Al was determined with a standard Leitz Dila-tometer using a 1. 97 inch (50. 00 mm) long specimen at a heating rate of 7°F/minute (4°C/minute) in a nitrogen atmosphere. The graph of percent expan-sion versus temperature shown by Figure 7 indicates almost linear behaviorover the entire temperature range. The average coefficient of linear thermalexpansion is 7. 75 x lQ-6/°F (13. 95 x 10-6/°C) over the range of 77 to 1832°F(25 to 1000°C).
Density
The density of a sample from the above heat of material wasdetermined by the displacement method. The density of induction melted,forged and hot rolled standard VM-103 was 0. 357 lb/in3 (9. 89 g/cm3).
Mechanical Properties
Tensile specimens from heats Al, B3 and B4 were tested in thefollowing conditions:
Condition
SHT
SHT + Age(a)
SHT + Age*b*
SHT + 25% Red.
Test Temperature
75°F(24°C)
X
X
X
X
1200°F
(649°C)
X
1600°F
(871°C)
X
X
1800°F
(982°C)
X
2000°F
(1093°C)
X
X
SHT = Solution heat treat, 2200°F (1204°C), 1/2 hour water quench
Age^a^ = 1300°F (704°C), 10 hours, air cool
Age^b^ = 1600°F (871°C), 192 hours, air cool
25% Red. •= .25% reduction at 75°F (24°C)
29
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The results of the mechanical properties evaluation shown by TableXI confirmed the previous results obtained during Task II. The previousresults for heats Al, B3 and B4 have been relisted for comparison. Heat B3with the 10 percent nickel addition shown as increase in ductility with only asmall decrease in tensile strength. The mechanical properties of solutionheat treated material as a function of test temperature is shown by Figure 8.Solution heat treated samples from heats Al, B3 and B4 were encapsulatedin evacuated glass tubes and exposed for 192 hours at 1600°F (871°C) andair cooled. Heat B3 with 10 percent nickel indicated a significant increasein ductility as measured by the room temperature elongation after the longterm exposure in the 1600°F (871°C) embrittlement range compared to thestandard composition VM-103, heats Al and B4.
Hardness Testing
Samples from heats B3 and B4 in the conditions shown by Table XIIwere prepared for hot hardness testing at temperatures up to 1800 F (982 C).The samples, approximately 1/2 x 2. 0 x 0. 100 inch (1. 2 x 5. 1 x 0. 23 cm)with ground surfaces, were evaluated in a standard Wilson hot hardness tester.The hardness values obtained for the B3 heat material with 10 percent nickelare slightly lower than for the standard VM-103 composition heat B4 and alsolower than the vacuum induction melted material heat A2 reported earlier,with the same composition as heat B3. The hardness trends indicate that thehardening effects of cold work, and to a lesser extent the effects of aging, areretained reasonably well at temperatures up to 1400°F (760°C).
Impact Evaluation
Standard V-notch Charpy impact specimens were machined from heatB3 and B4 material in the conditions shown by Table XIII. Both heats wereinduction melted plus electroslag remelted. The solution treated condition ofboth heats showed, the best impact strengths with drastic reductions in impactstrength for the cold reduced material, increasing the transition temperatureabove ambient. Heat B3 with the 10 percent nickel exhibited better impactstrength than the standard VM-103 composition in all conditions evaluated.
Creep Rupture
Wrought specimens from heats B3 and B4 and cast specimens fromheat B3 were evaluated in creep rupture at 1600, 1800, 2000 and 2200°F (871,982, 1093 and 1204°C) in a nitrogen atmosphere. The 2200°F (1204°C) testswere heated by induction heating of specimen and the lower temperature testswere performed with standard creep techniques with resistance furnace heating.The wrought specimens were machined from hot rolled, solution treated ESRmaterial approximately 0. 040 inch (1. 0 cm) thick. The cast specimens werecast directly from an induction melt into a ceramic test specimen mold andsubsequently solution heat treated. Figure 9 shows one of the castings.
31
TABLE XI
MECHANICAL PROPERTIES OF STANDARD AND MODIFIED VM-103 HEATS Al, B3 AND B4
(Average of Duplicate Specimens)
Condition
SHT
SHT + AGE '*'
SHT + 25% Red.
SHT + AGE
.'teatNo.
AlB3B4
AlB3B4
AlB3B4
AlB3B4
AlB3B4
AlB3B4
AlB3B4
AlB3B4
AlB3B4
AlB3B4
Test Temp
°F
757575
120012001200
160016001600
180018001800
200020002000
757575
200020002000
757575
757575
160016001600
°C
242424
649649649
871871871
982982982
109310931093
242424
109310931093
242424
242424
871871871
0.2% OffsetYieldStrength
ksi
88.276.590.5
79.961.785.1
63.248.453.7
33.723.627.9
17.310.213.7
144.4110.9133.1
12.510.513.2
152.9166.3165.7
99.380.592.4
48.039.851.4
N/mm2
608527624
551425586 .
435333370
232.163192
1197094
995764917
867291
105311461142
684555637
331274354
UltimateTensileStrength
ksi
138.7156.2150.8
109.4.97.8101.2
82.152.468.1
47.638.541.9
20.416.718.7
174.8176.0167.2
19.316.119.6
204.1204.9251.4
156.7127.5155.4
77.364.180.6
N/mm2
95610761039
754674697
566361469
328265289
141115129
120412131152
133111135
140614121732
10808781071
533442555
Elongationin 1 in. or2.5 cm, %'
9.535.515.0
9.012.04.8
3.310.89.5
22.521.032.0
11.541.031.5
2.513.23.0
23.533.522.0
4.310.02.5
1.54.71.2
10.516.010.8
SHT
AGE(a)= Solution heat treat, 2200°F (1204°C), 1/2 hour water quench
= 1300°F (704°C), 10 hours, air cool
25% Red. = 25% reduction at 75°F (24°C)
AGEOO = 1600°F (871°C), 192 hours, air cool
Heat Nos: Al - Standard VM-103 (Vacuum Induction Method)B3 - Standard VM-103 + 10% Ni (Electroslag Remelted)B4 - Standard VM-103 (Electroslag Remelted)
32
200
150
100
HEAT NO.I
O Al Standard VM-103 (VIM)
D B3 Standard VM-103 (ESR)A B4 Standard VM-103 (ESR)
100
2000
FIGURE 8. MECHANICAL PROPERTIES OF VM-103 AS A FUNCTION OF TEST TEMPERATURES
33
TABLE XII
HOT HARDNESS OF VM-103, HEATS B3 AND B4
Heat
B3
B4
B3
B4
B3
B4
B3
B4
Condition
SHT
SHT
SHT + Age
SHT + Age
SHT + 25% Red.
SHT + 25% Red.
SHT + 25% Red. + Age
SHT + 25% Red. + Age
Test Temperature
Ambient
R 31cR 38
cR 35. 5
cR 42cR 48. 5cR 49cR 55
cR 54
c
1000°F(538°F)
R b 9 2
R b 9 6
R b 9 9
RC 35
R 41cR 48
cR 47cR 47
c
1200°F(649°F)
R b 9 0
R b 9 5
R b 9 8 . 5
R 30cR 39cR 43cR 40. 5
cR 41
c
1400°F(760°F)
R, 86b
R b 9 2
R, 86b
R, 100bR 31cR 29cR 24
cR 28
c
Conditions:
SHT
Age
25% Red.
= Solution heat treat, 2200 F, 1/2 hour, water quench
= Age, 1300°F, 10 hours, air coolo.
= 25% Reduction at 75°F (24 C)
Heat Nos: B3 - Standard VM-103 + 10% Ni (ESR)B4 - Standard VM-103 (ESR)
34
TABLE XIII
IMPACT STRENGTH OF VM-103, HEATS B3 AND B4
Heat
B3
B4
B3
B4
B3
B4
B3
B4
Condition
SHT
SHT
SHT + Age
SHT + Age
SHT + 25% Red.
SHT + 25% Red.
SHT + 25% Red. + Age
SHT + 25% Red. + Age
Test Temperature
-65°F (-54°C)
ft-lbs
27. 1
18. 4
26. 9
14. 5
5. 8
4. 4
5. 3
3.0 (a )
Joules
36. 7
25. 0
36. 5
19. 7
7. 9
6. 0
7. 2
4. 1
75°F (24°C)
ft-lbs
30. 4
17. 7
30. 5
20. 8
7. 3
4. 5
2. 7
1. 7
Joules
41. 2
24. 0
41. 4
28. 2
9. 9
6. 1
3. 7
2. 3
Conditions:
SHT
Age
= Solution heat treated, 2200°F (1204°C), 1/2 hour, water quench.
= Age 1300°F (704°C), 10 hours, air cool
25% Red. = 25% reduction at 75°C (24°C)
(a)One specimen failed during machining
Heat Nos:
B3 Standard VM-103 + 10% Ni (ESR)
B4 Standard BM-103 (ESR)
35
FIGURE 9. VM-103 CREEP RUPTURE SPECIMENS CASTING
36
The results are shown graphically by Figure 10 and tabulated inTable XIV. The 10 percent nickel addition to heat B3 did not show any sig-nificant degradation of the creep rupture properties, particularly at thehigher temperatures. The cast specimens exhibited higher creep ruptureproperties (Figure 11) than the wrought material.
Task IV, VM-103 Procurement Specification
The objective of Task IV was to prepare a specification for theprocurement of wrought VM-103 products including material conditionsrestrictive requirements and quality control limits. The procurementspecification generated during this task entitled, "Corrosion and HeatResistant Alloy Bars, Forgings, Plate and Sheet - Cobalt Base - 25W-3Cr-1 Ti-0. 5 Ar-0. 5 C, " is presented in Appendix A. The basic AerospaceMaterial Specification (AMS) format was utilized for this specification.
The approach for preparing this specification consisted of accum-ulating and reviewing the pertinent data from the various heats of VM-103that were considered to be of highest quality. The information consideredincluded compositional and purity variations, melting techniques, fabricationand processing parameters, mechanical properties and microstructure.
A comparison of data from thre'e electroslag remelted heats, PF-11,PF-288 and B4 (Tables I and III) indicated that the compositional variationsdemonstrated by these heats had no significant effect upon mechanical proper-ties or fabricability of wrought VM-103. This indicated that a rather broadrange of compositional variations is acceptable for VM-103 and that specifiedtolerances typical of other wrought cobalt base alloys such as L-605 are alsovalid for the VM-103 alloy. Therefore, the composition tolerances specifiedin paragraph 3. 1 (Appendix I) were purposely selected to be no more restrictivethan AMS 5759 for L-605. . .
The various melting techniques utilized for the production of nickeland cobalt base superalloys have been evaluated during the several investiga-tions of VM-103. The single vacuum induction melting technique used to produceseveral small heats provided material with acceptable properties but withfabricability definitely inferior to vacuum arc remelted or electroslag remeltedmaterial. Double vacuum melting processes are used for melting of commer-cial superalloys to achieve improved homogenity to reduce microsegregation andimprove microcleanliness. These benefits were also shown for VM-103. Theelectroslag remelted VM-103 showed significant improvement in both ductilityand fabricability over vacuum arc remelted material. Based on these results,vacuum induction plus VAR or ESR processes were specified.
The processing parameters presented in this specification wereestablished by work performed on Contract NAS3-12421 as well as this contract.These processing parameters have repeatedly demonstrated that the specifiedmechanical properties, grain size and hardness requirements can be readilyobtained.
37
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40
4. SUMMARY OF RESULTS
The following major results were obtained from an investiga-tion to develop a procurement specification for the NASA VM-103 alloy:
(1) The strength properties of VM-103 up to 2200°F (1204°C)and its fabricability make this alloy a useful alternatefor conventional wrought cobalt and nickel base super-alloys.
(2) The strength properties of VM-103 produced by vacuuminduction melting and by vacuum induction melting pluselectroslag remelting are essentially identical. Electro-slag remelting significantly improves the fabricabilityand ductility of VM-103.
(3) The addition of 10 percent nickel to the standard VM-103composition improves (a) ductility, (b) hot and coldfabricability, and (c) impact strength. The nickeladdition is also effective in reducing the 1600 F (871 C)long term embrittlement characteristics of VM-103without significantly reducing its tensile or creep ruptureproperties.
(4) Thermomechanical processing is very effective in increas-ing the room temperature hardness of VM-103 andprobably its room and intermediate temperature strengths.Tensile tests conducted between 2000 and 2200°F (1093and 1204 C) showed no beneficial effects.
41
. • 5. CONCLUDING REMARKS
The development of VM-103 has progressed considerably as a result oftwo NASA contracts (NAS3-12421 and NAS3-14329) and internally fundedwork at Philco-Ford. Since 1968, the research status of VM-103 whichprimarily entailed characterization of 1700 g heats has progressedthrough fabrication and evaluation of 50 pound heats and development ofan initial procurement specification for wrought VM-103 products. Com-position, melting process, heat treating parameters, hot and cold workingprocesses, physical and mechanical properties, and physical metallurgyof the alloy have been investigated to varying degrees. The alloy, in itspresent state of development, could be easily scaled up to productionquantities of wrought or cast products.
In wrought form, VM-103 offers high temperature strength properties to2200°F (1204°C) that exceed other widely used nickel and cobalt basealloys such as Rene 41 and L-605. This makes it attractive for hot gasvalve components associated with guidance systems of various missilesystems. Preliminary tests at Aeronutronic were encouraging on selectedwrought components, and further testing has been recommended pendingavailability of additional developmental funding.
VM-103 has demonstrated considerable high temperature gas erosion re-sistance and thus shows potential as a liner for high performance barrelssuch as those associated with aircraft machine guns. VM-103 has alreadybeen tested and/or delivered to the Air Force for testing on three AirForce contracts. A fourth contract presently in progress also requiresdelivery of VM-103 lined test barrels, bringing the total to approximately12 which includes both solution treated and 20% cold worked conditions.The alloy is well suited to this application, but lacks adequate machine-ability for large production quantities. Under Air Force funding, anelectrochemical machining technique was successfully developed forrifling the alloy. Electrode discharge machining has been utilizedsuccessfully to gun drill VM-103, since conventional gun drilling is noteconomically attractive. A goal for future composition modificationsshould be to improve the machineability of VM-103.
The alloy appears to be very castable based on the results mentioned inthis report, and previously reported by NASA and Philco-Ford. Again,the hot gas valve ducting and housings are obvious potential applicationsfor cast VM-103 as well as various gas turbine engine components. Fur-ther development effort to more thoroughly characterize castability andcast properties would be useful.
42
As indicated, the 10% Ni addition to VM-103 significantly reduces the em-• o obrittling effect of prolonged exposure in the 1600 F (871 C) range whichsignificantly extends the usefulness of the alloy. In addition, fabricability,ductility and impact strength are improved with little sacrifice in strengthor creep rupture properties. Further studies to optimize nickel contentin modified VM-103 appear worthwhile.
To summarize, VM-103 and/or modifications thereof appear to offersignificant promise for existing and future aerospace and ordnance hightemperature applications, and could be produced in production quantitieswith minimum scale-up efforts. It is believed that additional alloymodification studies would result in an alloy that is even more attractive.
43
REFERENCES
1.. Bhat, G. K. , and Tobias, J. B. , "Development .of a ManufacturingProcess for the Electroslag Melting and Casting of Materials, "Quarterly Progress Reports, Numbers 5-8, for AF Contract NumberAF33(615)-5430, Mellon Institute, September 1967.- June 1968.
2. Pridgeon, J. W. , Paper regarding ESR of Superalloys at StelliteDivision of Union Cabide, Vacuum Metallurgy Conference, LosAngeles, California, 1968.
3. Harlow, R. A. , and Gold, E. , "Development and Metallurgy Studyof a NASA Cobalt-Base Superalloy, " NASA CR-72726, Philco-FordCorporation, April 15, 1970.
4. Johari, O. , and Thomas, G. , "Structures and Strength of AusformedSteel, " Trans. ASM, 58, 563, 1965.
5. Koppenaal, T. J. , "The Current Status of Thermomechanical Treat-ment of Steel in the Soviet Union, " Trans. ASM, 62, 24, 1969.
6. McEvily, A. J. , Clark, J. B. , Utley, E. C. , and Hernstein, W, H. ,"Evidence for Reversion During Cyclic Loading of an AluminumAlloy," Trans. AIME, 227, 1093, 1963.
7. McEvily, A. J. , Snyder, R. L. , and Clark, J. B. , "The Effect ofNonuniform Precipitation on the Fatigue Properties of an AgeHardening Alloy, " Trans. AIME, 227, 432, 1963.
8. McEvily, A. J. , Clark, J. B. , and Bond, A. P., "Effect of Thermal-Mechanical Processing on the Fatigue and Stress-Corrosion Pro-perties of an Al-Zn-Mg Alloy, " Technical Report SL 66-111, FordMotor Company, Dearborn, Michigan, 1966.
9. Herchenroeder, R. B. , and Ebikors, W. T. , "In-Process Metallurgyof Wrought Cobalt-Base Alloys, " Metals Engineering Quarterly, 9,30, 1969.
10. Sandrock, G. D. , and Leonard, L. , "Cold Reduction as a Means ofReducing Embrittlement of Cobalt-Base Alloy (L-605), " NASATND-3528, 1966.
11. Blankenship, Charles P. , "Thermomechanical Processing of Nickel-Base Alloy U-700, " Aerospace Structural Materials Conference,NASA-Lewis Research Center, November 1969.
44
REFERENCES (CONTINUED)
12. Sandrock, G. D. , Ashbrook, R. L. , and Freche, J. C. , "Effect ofVariations in Silicon and Iron Content on Embrittlement of a Cobalt-Base Alloy (L-605), " NASA TND-2989, September 1965.
13. Nejedlik, J. F. , "The Embrittlement Characteristics of a Low-Silicon Modified Cobalt-Base Alloy (L-605) at 1200 and 1600°F, "TRW ER 6870, 15 June 1966.
14. Harlow, R. A. , "Manufacturing Methods for Producing L-605Hardware," AFML-TR-67-414, January 1968.
15. Wlodek, S. T. , "Embrittlement of a Co-Cr-W (L-605) Alloy, "Trans. ASM, 56, September 1963.
16. Dreshfield, R. L. , Frecke, J. C. , and Sandrock, G. D. , "Modifi-cation of High Temperature Cobalt-Tungsten Alloys for ImprovedStability, " NASA TND-6147, February, 1971.
45
APPENDIX A
CORROSION AND HEAT RESISTANT ALLOY BARS, FORCINGS,PLATE AND SHEET - COBALT BASE - 25W - 3Cr - 1 Ti - 0, 5 Zr - 0. 5 C
1. Scope
The purpose of this specification is to establish material conditions,restrictive requirements and quality control procedures for VM-103cobalt base forging stock, bars plate, and sheet. VM-103 is pri-marily for parts and assemblies that require service temperatureup to 2200°F (1204°C).
2. Applicable specifications and standards, of the issues in effect ondate of invitation for bids, or as stated on the purchase order, form apart of this specification.
2. 1 AMS 2261; Tolerances - Nickel, Nickel Base and Cobalt BaseAlloy Bars and Forging Stock.
2.2 AMS 2262; Tolerances - Nickel, Nickel Base and Cobalt BaseAlloy Sheet, Strip and Plate.
2.3 AMS 2269; Chemical Check Analysis Limits, Wrought Nickeland Nickel Base Alloys.
2.4 AMS 2630; Ultrasonic Inspection.
2. 5 ASTM E-45; Recommended Practice for Determining theInclusion Content of Steel.
2. 6 ASTM E-112 - Methods for Estimating the Average Grain Sizeof Metals.
2. 7 Federal Test Method Standard No. 151a - Metals; Test Methods.
46
3. Technical Requirements
3. 1 Composition - The composition of the alloy shall conform tothe following:
Min
Tungsten 24
Chromium 2.5
Titanium 0.75
Zirconium 0.4
Carbon 0.48
Iron - 0. 1
Cobalt Balance
Check Analysis: Composition variation shall meet the requirements ofthe latest issue of AMS 2269.
3. 2 Melting Practice - Material shall be produced by vacuuminduction melting plus vacuum arc remelting or vacuum inductionmelting plus electroslag remelting.
3. 3 Forging Practice - Forging parameters shall be chosen suchthat following solution heat treatment the forgings shall meet therequirements of Sections 3. 6, 3.7, 3.8, 3.9, and 3. 10. Ingots shallbe reduced sufficiently in cross section to assure proper uniformrefinement of structure in the forged billet.
3.4 Heat Treatment - All material shall be solution treated byheating at 2200 + 25°F (1204 + 14°C), holding at temperature for 1/2hour and quenching in agitated water. These parameters may be variedas required to meet requirements of Sections 3. 6, 3. 7, 3. 8, and 3. 10.
3. 5 Condition - All material shall be supplied in the solution heattreated and descaled condition.
3.6 Hardness - The material shall have a hardness not higher thanBrinell 363 or equivalent.
47
3. 7 Tensile Properties - Minimum tensile properties in the solutionannealed condition shall be:
Tensile Strength 135,000 psi (960 MN/mm2)
Yield Strength, 0.2% offset 80,000 psi (550 MN/mm2)
Elongation, % in 4D 7%
3. 8 Grain Size - The grain size as determined by ASTM E-112shall be predominantly number three of finer with occasional grainsas large as number one permissible.
3. 9 Macro structure - Flow line patterns of forged parts shall beas specified on the forging drawing.
3.10 Microcleanliness - The procedure for determining the inclu-sion rating shall be in accordance with ASTM E-45, Method D. Thisrating based on specimens representing the worst area of inclusionsshall not exceed the following:
Inclusion Rating
Type Inclusion A B_ C_ D_
Thin 1 . 5 1 . 5 1 . 2
Thick 1 1 1 1.5
In addition, the material shall be substantially free of grain boundaryprecipitates when examined at 500X magnification after electrolyticallyetching with a solution of the following proportions: 100 ml H_O, 40 mlacetic acid, 40 ml HC1, 15 ml H2SO4> 40 ml HNC>3, and 25 g FeCl3.
3. 11 Ultrasonic Inspection. - The method of ultrasonic inspectionshall be by the immersion process in accordance with AMS 2630. Allmaterial (100 percent) shall be inspected to the discontinuity indicationIimitsof3.11.1, 3.11.2, 3.11.3, and 3. 11.4.
3.11.1 No discontinuity indications shall be in excess of thereponse obtained from a 3/64-inch diameter, flat-bottomed hole locatedat the depth of the estimated discontinuity.
3. 11. 2 Multiple indications in excess of the response from a 1/32inch diameter flat-bottomed hole located at the depth of the estimateddiscontinuity shall not have centers closer than one inch.
48
3. 11. 3 Indications from a single discontinutiy equal to or greaterthan the response from a 1/32 inch diameter flat-bottomed hole at theestimated discontinutiy depth shall not be more than one inch in length.
3. 11.4 Multiple indications shall not be of such size or frequencyas to reduce the back reflection pattern to 50 percent or less of the backreflection pattern of normal material of the same geometry, with thecrystal parallel to the front and back surface.s to insure that the.lossof back reflection is not caused by surface roughness or part geometryvariation.
3. 12 Workmanship - The material shall be uniform in quality andcondition, free from pipe, flakes or heat cracks. It shall be free ofdefects such as seams, laps, cracks, slag, hard spots, porosity,rolled in scale, fissures, gas cavities, and undue segregation whichmay be detrimental to the fabrication or performance of parts.
4. Identification
Material shall be identified as indicated on the purchase order.
5. Quality Assurance
5. 1 Lot - A lot is defined as all material produced in one runfrom the same heat of material and heat treated in the same furnace load.
5. 2 Chemical Analysis - A sample from each heat of materialrepresented in the shipment shall be analyzed to determine conformanceto the chemical composition requirements of Section 3. 1.
5. 3 Tensile Properties
5.3.1 Two each room temperature tensile tests shall be made inaccordance with Federal Test Method Standard 151 on each each lotrepresented in the shipment.
5. 3.2 The test specimens shall be generated from coupons, asspecified on the purchase order or applicable drawing.
5.4 Micro-Examination - One sample from each lot shall beprepared and examined to determine grain size and microcleanliness.
5. 5 Hardness - Each lot shall be checked for hardness.
49
6. Reports
Unless otherwise specified, the vendor of the product shall furnishwith each shipment three copies of a report of the results of tests forchemical composition of each heat in the shipment and the results oftests on each size heat to determine conformance to the technical require-ments of this specification. This report shall include the purchase ordernumber, material specification number, heat number, size, and quantityfrom each heat. If forgings are supplied, the part number .and size ofstock used to make the forgings shall also be included.
50
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