Of IN-100 ALLOY

Engineering Properties of IN-100 ALLOY

INTERNATIONAL NICKEL

CONTENTS

Page COMPOSITION ...... 1

SPECIFICATION ...... 1 STRESS-RUPTURE PROPERTIES ...... 1 TENSILE PROPERTIES ...... 1 HARDNESS ...... 1

PHYSICAL PROPERTIES ...... 2 DENSITY ...... 2 MELTING RANGE ...... 2 STABILITY ...... 2 THERMAL EXPANSION ...... 2 ELECTRICAL RESISTIVITY ...... 2

CHEMICAL PROPERTIES ...... 2 OXIDATION RESISTANCE ...... 2 Cyclic Test ...... 2 Static Test ...... 2 Dynamic Test ...... 2 SULFIDATION RESISTANCE ...... 5 Crucible Test ...... 5 Rig Test ...... 5

HEAT TREATMENT ...... 5

MECHANICAL PROPERTIES ...... 5 TENSILE PROPERTIES ...... 5 STRESS-RUPTURE PROPERTIES ...... 5 STRESS-RUPTURE PARAMETER ...... 8 CREEP RATE ...... 8 MINIMUM CREEP RATE ...... 8 DYNAMIC MODULUS OF ELASTICITY ...... 8

IMPACT PROPERTIES ...... 11

HOT HARDNESS ...... 11

FATIGUE ...... 11 MECHANICAL ...... 11 THERMAL ...... 14

MACHINING AND GRINDING ...... 14

APPENDIX ...... 16

REFERENCES ...... IBC Engineering Properties of IN-100 ALLOY

IN-100 alloy* is a nickel-base precipitation refractory metal content make IN -100 particularly hardenable, vacuum cast alloy possessing high attractive on a strength to density basis. The rupture strength through 1900 ºF. The high per- alloy has been successfully cast and utilized in a centages of aluminum and titanium and the low variety of shapes from turbine blades, vanes and nozzles to integral wheels.

COMPOSITION – WEIGHT PER CENT

Element Nominal Range (AMS 5397) Carbon 0.18 0.15 – 0.20 Chromium 10.00 8.00 – 11.00 Cobalt 15.00 13.00 – 17.00 Molybdenum 3.00 2.00 – 4.00 Titanium 4.70 4.50 – 5.00 Aluminum 5.50 5.00 – 6.00 Vanadium 0.90 0.70 – 1.20 Zirconium 0.06 0.03 – 0.09 Boron 0.014 0.01 – 0.02 Iron LAP** 1.00 max. Manganese LAP 0.20 max. Silicon LAP 0.20 max. Sulfur LAP 0.015 max. Nickel balance (60) balance

SPECIFICATION

The AMS 5397 specification for IN-100 alloy requires the following mechanical properties in the as-cast condition:

Stress - Rupture Properties – Minimum

Test Temp. Stress Life E long. ºF psi Hrs. % in 4D

1800 29,000 23 4

Tensile Properties – Minimum

0.2% Yield Tensile Test Temp. Elong. Strength Strength ºF % in 4D psi psi

70 95,000 115,000 5

Hardness

Rockwell C 30-44 or equivalent

There are many alternate specifications in existence and individual companies should be contacted as to their requirements.

* U.S. Patent #3,061,426; produced under license from The International Nickel Company, Inc. **Low as possible

PHYSICAL PROPERTIES

Density 0.280 lb./cu. in. (7.75 g/cu. cm)

Melting Range 2305 - 2435 ºF (1260 -1335 ºC)

Stability While long-time elevated temperature stability can be demonstrated only by long-time exposure, a mathematical analysis based on electron vacancy concentration (see Appendix) is useful in indicating the susceptibility of an alloy to form sigma. The electron vacancy number, Nv , of IN-100 of nominal composition is 2.46. Nv values over 2.50 generally indicate that an alloy is susceptible to sigma. When IN-100 was originally introduced, the suggested range for titanium extended from 4.5 to a maximum of 5.5 per cent. Compositions toward the top side of this range did exhibit sigma formation. For example, a 5.3 Ti alloy with an Nv of 2.70 contained sigma which detracted from rupture life.

The maximum titanium level then was reduced to the current AMS specification value of 5.0 percent. This change eliminated the deleterious effects of sigma on material properties without sacrificing any of the material's desired properties.

Thermal Expansion (See Figure 1)

Mean Mean Test Temp. Coefficient Test Temp. Coefficient oF per oF oF per oF 70 - 200 7.2 x 10-6 70 – 1200 8.0 x 10-6 70 - 400 7.2 70 – 1400 8.3 70 - 600 7.3 70 – 1600 8.8 70 - 800 7.5 70 – 1800 9.3 70 - 1000 7.7 70 – 2000 10.1

Electrical Resistivity 143.0 microhm-cm at R.T.

CHEMICAL PROPERTIES

OXIDATION RESISTANCE

Cyclic Test (See Figure 2)

Samples were given a cyclic exposure by heating in air at 1900 ºF for 16 hours and then cooling for 8 hours.

Alloy Wt. Change, % in 208 Hrs. IN -100 –.80 Alloy 713LC –.10

Static Test (See Figure 3) The static oxidation tests, performed by General Electric, were conducted by placing specimens in open zircon cup-type crucibles and oxidizing them in the static atmosphere of electric box furnaces.(1)

Dynamic Test (See Figure 4) The dynamic oxidation tests were performed by General Electric in a natural gas-fired flame tunnel. Test specimens were placed in a rotating fixture positioned in the hot zone of the flame tunnel perpendicular to the gas flow.(1)

Figure 1. Thermal – Expansion of IN-100 Alloy. Figure 2. Oxidation Resistance of IN-100 Alloy. and 713C: Cyclic Test 16 Hours At 1900 ºF, Cool In Air For 8 Hours.

Figure 3. Comparison of Oxidation Kinetics of IN-100 and Alloy 713C at 1600 and 2000 ºF. Note the Decreasing Oxidation Rates at 2000 ºF (t>100 min.).

3 Figure 4(a). Weight Change During Oxidation In High Velocity Natural Gas Combustion Products at 1600 ºF.

Figure 4(b). Weight Change During Oxidation In High Velocity Natural Gas Combustion Products at 2000 ºF.

Figure 4(c). Sulfidation Resistance of Nickel Base Alloys In A Com- bustion Rig Test. Reference: Quarterly Progress Report No. 1 (July-Sept. 1966) "Study of the Hot Corrosion of Superalloys" by Lycoming Division of AVCO Corp. under Air Force contract AF33(615)-5212, Project No. 7381.

4 SULFIDATION RESISTANCE

Crucible Test – 90% Na2SO4/10% NaCl 1700 ºF

Alloy Wt. Loss, % in 1 Hr. Wt. Loss, % in 2 Hrs. IN-100 0 2 Alloy 713 LC 12.8 13 IN -162 0 14

Rig Test (See Figure 4(C))

Paddle specimens with an airfoil configuration were rotated in and out of a furnace fired with JP-4 fuel (.04 w/o S) for 120 hours on a cyclic basis. During the heating cycle, a controlled amount of synthetic seawater was sprayed into the combustion exit and mixed with the gas stream. The temperature profile on the airfoil ranged from 1600-1750 ºF with the maximum on the trailing edge.

HEAT TREATMENT

The properties shown in this bulletin are for IN- a partial solutioning. If the coating is to be dif- 100 in the as-cast condition. In many applications, fused at 1900-1950 ºF, it is suggested that the IN-100 components are given a protective coating material receive a preliminary high temperature to enchance corrosion resistance. This treatment solutioning at 2100-2150 ºF. An aging treatment at generally includes a diffusion cycle at a 1500-1600 ºF is recommended after the coating temperature between 1800-2100 ºF for 2-8 hours. cycle. This should provide material with a In effect, this treatment provides the material with capability of maintaining a consistently high level of mechanical properties.

MECHANICAL PROPERTIES

Tensile Properties (See Figure 5)

Test 0.2% Yield Tensile Temp. Strength Strength Elong. Reduction ºF psi psi % of Area

70 123,000 147,000 9.0 11.0 1000 128,000 158,000 9.0 11.0 1200 129,000 161,000 6.0 7.0 1350 127,000 159,000 6.5 7.2 1500 118,000 144,000 6.0 7.2 1700 73,000 107,000 6.0 7.2 1900 41,000 64,000 6.0 8.0

Creep – Rupture Properties Coarse grain (≥1/8") and fine grain (≤1/16") castings have exhibited nearly identical creep rupture properties. These are summarized as follows:

Stress – Rupture Properties (See Figures 6 and 7 and raw data in Table I)

Test Stress, psi, for Rupture in Temp. ºF 10 Hr. 100 Hr. 1,000 Hr. 1350 - 97,000 83,000 1500 90,000 73,000 55,000 1700 52,000 38,000 25,000 1800 38,000 25,000 15,000 1900 - 16,000 8,500

5 Figure 5. Typical Tensile Properties of Figure 7. Stress Rupture Data for As Cast IN-100 As Cast IN-100 Alloy Alloy.

Figure 8. Larson-Miller Stress Rupture Parameter Curve for IN-100.

Figure 6. Typical Stress Rupture Properties of As Cast IN-100 AIloy.

6 TABLE I

STRESS RUPTURE DATA ON AS CAST IN-100 ALLOY

Coarse Grain (≥1/8")

Temp. Stress Life Elong. R.A. ºF psi Hrs. % %

1900 15,000 115 9 13 12,000 278 9 17 9,000 705 11 14

1800 29,000 45 11 12 25,000 82 11 12 13,000 1779 9 15 12,000 2440 12 23

1700 50,000 15 7 7 19,000 3468 13 18

1650 30,000 1322 6 11

1500 85,000 16 6 10 75,000 82 5 6 55,000 806 9 9 40,000 4355* 6 13

1400 85,000 202 6

1350 100,000 52 2 5 90,000 355 3 6 80,000 1468 3 8

Fine Grain (≤1/16")

1800 29,000 43 14 16 18,000 526 12 19

1700 35,000 183 11 12 25,000 1013 11 16

1650 30,000 970 7 14

1500 90,000 9 7 6 60,000 771 7 10 50,000 1584 8 14

*Subsize bar machined from broken rupture bar showed the following properties:

Temp. 0.2% Yield Tensile Elong. R.A. ºF Strength, psi Strength, psi % % 1400 109,000 136,000 3 3.5

7 Stress – Rupture Parameter (See Figure 8)

Creep Rate (See Figures 9 - 13 and Table 11) Test Stress, psi, for Designated Creep Rate Temp. ºF .0001%/hr. .001 %/ hr. .01%/hr. 1350 - 77,500 95,000 1500 (47,000) 55,000 70,000 1700 (12,000) 22,500 34,000 1800 ( 6,500) 14,500 22,500 1900 - 5,000 13,500 ( ) Denotes extrapolated values

Minimum Creep Rate (See Figures 9 - 13 and raw data in Table II)

TABLE II LONG - TIME CREEP DATA ON AS CAST IN-100 ALLOY

Coarse Grain (≥1/8") Temp. Stress Time, Hours, for Total Creep Strain of . . . Minimum ºF psi 0.1% 0.2% 0.5% 1.0% Creep Rate %/Hr.

1350 100,000 1.0 2.0 8.0 26 .0291 90,000 5.0 l0 44 135 .0050 80,000 25 175 500 800 .0014

1500 85,000 – 0.2 1.9 5.6 .1300 75,000 2.0 2.5 7.7 28 .0185 55,000 50 170 395 560 .0010

1700 50,000 0.4 1.8 2.9 5.8 .0320 19,000 80 200 1000 1760 .0004

1800 29,000 1.5 7.0 16 25 .0310 25,000 2.5 7.0 19 35 .0350 13,000 60 175 625 1175 .0006 12;000 75 195 750 1380 .0005

1900 15,000 2.7 6.0 25 58 .0144 12,000 8.0 20 62 140 .0060 9,000 4.0 15 90 270 .0028

Fine Grain (≤1/16") 1500 90,000 0.10 0.15 0.40 1.85 .28 60,000 7.5 40.0 170 340 .0025

1650 30,000 55 190 440 570 .00091

1700 35,000 5.0 15 45 79 .001 25,000 60 120 260 480

1800 18,000 30 88 165 2850 .003

Dynamic Modulus of Elasticity (See Figure 14) Test Dynamic Test Dynamic Temp. Modulus Temp. Modulus ºF psi ºF psi 70 31.2 x 106 1000 27.1 200 30.7 1200 26.0 400 29.9 1400 25.1 600 28.9 1600 23.5 800 28.1 1800 21.9

8 Figure 9. Creep Rupture Curves for IN-1OO Alloy at 1350 ºF

Figure 10. Creep Rupture Curves for IN-100 Alloy at 1500 ºF

9 Figure 11. Creep Rupture Curves for IN-100 Alloy at 1700 ºF

Figure 12. Creep Rupture Curves for IN-100 Alloy at 1800 ºF

10 Figure 13. Creep Rupture Curves for IN-100 Alloy at 1900 ºF

IMPACT PROPERTIES (See Figures 15 and 16)

Unnotched Charpy impact values (ft-lb) when tested at room temperature after various elevated temperature exposures are as follows:

Holding Grain Holding Temperature Time, Hr. Size R.T. 1200 ºF 1500 ºF 1700 ºF 0 1/16” 79, 73 1/4 45, 67

500 1/16 55, 89 45, 35 24, 25 1/4 53, 48 38, 32 23, 36

1000 1/16 69, 60 44, 19 28, 24 1/4 39, 45 39, 45 31, 24

HOT HARDNESS (See Figure 17)

Test Test Temp. Hardness Temp. Hardness ºF Rc ºF Rc 70 38.0 1200 35.5 600 37.5 1400 34.5 800 37.5 1600 29.0 1000 35.5 1800 16.0

FATIGUE

MECHANICAL

Plain and notched samples were axial fatigue tested at 1112 ºF (600 ºC) in Vibrophore machines at 196 cycles per second with 0 or 33,600 psi mean load. Results are shown in Figure 18.

11 Figure 15. Charpy V-Notch Impact Properties of IN-100 Alloy at Various Temperatures.

Figure 14. Dynamic Modulus of Elasticity of IN-100 Compared to 713C and 713LC.

Figure 16. Average Impact Data of IN-100 Alloy On Unnotched Charpy Bars Tested at R. T. After Elevated Temperature Exposure. Figure 17. Hot Hardness of IN-100 Alloy.

12 Figure 18. Axial Stress Fatigue Test Results for Alloy IN-100 Stress Form 33, 600 psi±P. Test Temperature 1112 ºF (600ºC).

Figure 19. Variation of Thermal Endurance with Temperature For Some Cast High Temperature Alloys.

THERMAL (See Figure 19)

The thermal fatigue resistance of several nickel base alloys was determined using the fluidized bed technique.(2) This method involved alternate immersion of 1-5/8 in. diameter tapered disc specimens, with 0.010 in. edge radius, in hot and cold beds.

THERMAL FATIGUE CYCLES TO FIRST CRACK

Peak Temperature 1472 ºF 1652 ºF 1832 ºF Alloy (800 ºC) (900 ºC) (1000ºC)

IN -100 > 1372 107 29 Alloy 713C > 1462 107 27 M22 138 50 12

MACHINING AND GRINDING (See Figure 20)

Although the nickel base superalloys are relatively difficult to machine as compared to carbon and stainless steels, proper use of speeds, feeds, tools and procedures will produce satisfactory results. Information on machining and grinding IN-100 alloy is given in reference 3.

14 FIGURE 20

RECOMMENDED CONDITIONS FOR MACHINING IN-100 ALLOY

Depth Width Cutting Wear- Tool Tool Tool Operation Tool Geometry of Cut of Cut Feed Speed land Cutting Fluid Material Used for Tests Life inches inches ft./min. inches BR: -5º SCEA: 15º 1/4” square .009 Highly C-3 SR: -5º ECEA: 15º 12 Turning throwaway .075 – in. / 30 .015 Sulphurized Carbide Relief: 5º min. insert rev. Oil NR: .030”

118º split point 1/4” diameter .003 Highly M-42 .250 25

15 Drilling 7º clearance drill – in. / 5 .015 Chlorinated HSS thru holes angle 2-1/2” long rev. Oil

118º plain point 1/4” diameter .003 Highly C-2 .250 21 Drilling 7º clearance drill _ in. / 14 .015 Chlorinated Carbide thru holes angle 2” long rev. Oil

SURFACE GRINDING

Wheel Speed Table Speed Down Feed Cross Feed Operation Wheel Grade Grinding Fluid Ft./Min. Ft./Min. In./Pass In./Pass G Ratio

Finishing 32A46J8VBE Highly Sulphurized Oil 3000-4000 60 .0005 .050 3.5

Roughing 32A46J8VBE Highly Sulphurized Oil 3000-4000 60 .001 .050 4.5

APPENDIX

METHOD FOR CALCULATION OF ELECTRON VACANCY NUMBER = NV

1. Convert the composition from weight per cent to atomic per cent.

2. After long time exposure in the sigma forming temperature range, the MC carbides tend to transform

to M23C 6 or M6 C. Assume one-half of the carbon forms MC in the following preferential order TaC, CbC, TiC.

a. Assume the remaining carbon forms M23C 6 with the M comprising 21 atoms of Cr and 2 atoms of Mo.

b. If the total weight per cent of Mo + 1/2 W exceeds 6.0%, M6 C will form ranging in composition

from M4 Mo2 C to M3 Mo3 C where M may be iron, chromium, cobalt or combinations thereof.

1 3. Assume the boron is primarily tied up as M2 M B 2 where M may be Mo, Ti or Al or combinations thereof and M1 may be Cr, Fe, or Ni and combinations thereof.

4. The gamma prime is considered to be Ni3 (Al, Ti, Ta, Cb).

5. Assume the residual matrix will consist of the atomic per cent minus those atoms tied up in the carbide reaction, boride reaction, and the gamma prime reaction. The total of these remaining atomic percentages gives the atomic concentration in the matrix. Conversion of this on a 100% basis gives the atomic per cent of each element remaining in the matrix. It is this percentage that is used in order to calculate the electron vacancy number.

6. The formula for calculation of the electron vacancy number is as follows:

N v = .66 Ni + 1.71 Co + 2.66 Fe + 4.66 (Cr + Mo + W) + 5.66 V + 6.66 Zr

REFERENCES

1. "Nickel-Base Superalloy Oxidation", Interim Progress Report #2, Air Force Contract No. AF33(615)-2861 for Research and Technology Division, Air Force Systems Command USAF by MDL-FPD General Electric, Cincinnati, Ohio.

2. M. J. Fleetwood, P. J. Penrice and J. E. Whittle, "Thermal-Fatigue Resistance of Cast Nickel-Base High-Temperature Alloys" to be published in the Foundry Trade Journal.

3. Inco-sponsored program at Metcut Research Associates on Machinability of Superalloys to be published.