Iron-Nickel-Cobalt Sealing Alloy: Standard Specification For
Iron-Nickel-Cobalt Sealing Alloy: Standard Specification For
Iron-Nickel-Cobalt Sealing Alloy: Standard Specification For
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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150×
150×
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TABLE 1 Chemical Requirements 8.2 Rolled and Annealed Tempers—Hardness tests when
Element Composition, % properly applied can be indicative of tensile strength. Hardness
Iron, nominal 53 A scales and ranges for these tempers, if desirable, shall be
Nickel, nominal 29 A negotiated between supplier and purchaser.
Cobalt, nominal 17 A
Manganese, max 0.50
Silicon, max 0.20 9. Tensile Strength
Carbon, max 0.04
Aluminum, max 0.10 B
9.1 Sheet and Strip:
Magnesium, max 0.10 B 9.1.1 Tensile strength shall be the basis for acceptance or
Zirconium, max 0.10 B rejection for the tempers given in Table 2 and shall conform
Titanium, max 0.10 B
Copper, max 0.20
with the requirements prescribed.
Chromium, max 0.20 9.1.2 Tension test specimens shall be taken so the longitu-
Molybdenum, max 0.20 dinal axis is parallel to the direction of rolling and the test shall
A
The iron, nickel, and cobalt requirements listed are nominal. They shall be be performed in accordance with Test Methods E8.
adjusted by the manufacturer so that the alloy meets the requirements for
coefficient of thermal expansion given in Table 4. 9.2 Wire and Rod:
B
The total of aluminum, magnesium, zirconium, and titanium shall not exceed 9.2.1 Tensile strength shall be the basis for acceptance or
0.20 %.
rejection for the tempers given in Table 3. and shall conform to
the requirements prescribed.
TABLE 2 Tensile Strength Requirements for Sheet and Strip 9.2.2 The test shall be performed in accordance with Test
Method E8.
Temper
Temper Name Tensile Strength, ksi(MPa)
Designation
10. Surface Finish
A annealed 82 max (570 max)
B ⁄ hard
14 75 to 90 (520 to 630) 10.1 The standard surface finishes available shall be those
C half hard 85 to 100 (590 to 700)
D 3⁄4 hard 95 to 110 (660 to 770)
resulting from the following operations:
E hard 100 min (700 min) 10.1.1 Hot rolling,
10.1.2 Forging,
10.1.3 Centerless grinding (rod),
10.1.4 Belt polishing,
6.4 Wire and Rod— These forms shall be supplied in one of 10.1.5 Cold rolling, and
the tempers given in Table 3 as specified. Unless otherwise 10.1.6 Wire drawing.
specified, the material shall be bright annealed and supplied in 11. Thermal Expansion Characteristics
temper A (annealed).
11.1 The average linear coefficients of thermal expansion
7. Grain Size shall be within the limits specified in Table 4.
7.1 Strip and sheet for deep drawing shall have an average 12. Test for Thermal Expansion
grain size not larger than ASTM No. 5 (Note 1), and no more
than 10 % of the grains shall be larger than No. 5 when 12.1 Heat the specimen in a hydrogen atmosphere for 1 h at
measured in accordance with Test Methods E112. 900°C, followed by 15 min at 1100°C. Between the 900 and
1100°C heat-treatment periods, the specimen may be cooled to
NOTE 1—This corresponds to a grain size of 0.065 mm, or 16 grains/in.2 room temperature if desired. Cool the specimen from 1100 to
of image at 100 × . 200°C in the hydrogen atmosphere at a rate not to exceed
5°C/min.
8. Hardness
12.2 Determine the thermal expansion characteristics in
8.1 Deep-Drawing Temper—For deep drawing, the hardness
accordance with Test Method E228.
shall not exceed 82 HRB for material 0.100 in. (2.54 mm) and
less in thickness and 85 HRB for material over 0.100 in. in NOTE 2—For critical glass sealing applications, it is recommended that
thickness when determined in accordance with Test Methods the user conduct functional testing in accordance with Practices F14, F140
or F144. Such tests circumvent possible problems with thermal expansion
E18. See also Test Method E92 for Vickers Hardness and Table measurements and glass setting point estimates.
3, E140 for the appropriate conversion between various hard- NOTE 3—The thermal treatment described in this section is for purposes
ness scales. of the thermal expansion test only. Consult the non-mandatory appendix
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of this document for guidance on annealing conditions for various product 15. Dimensions and Permissible Variations
forms.
15.1 Cold-Rolled Strip—Cold-rolled strip shall conform to
13. Transformation the permissible variations in dimensions prescribed in Table 5,
13.1 The temperature of the gamma-to-alpha transformation Table 6, and Table 7.
shall be below −78.5°C when the material is tested in accor- 15.2 Round Wire and Rod—Wire and rod shall conform to
dance with Section 14. However, for material whose smallest the permissible variations in dimensions prescribed in Table 8.
dimension is over 7⁄8 in. (22.2 mm), some localized 15.3 Cold-Drawn Tubing—Cold-drawn tubing, available ei-
transformation, acceptable to the purchaser, may be tolerated. ther as seamless or welded, shall conform to the permissible
NOTE 4—Lower transformation temperatures, ranging to as low as
−196°C, may be negotiated between supplier and purchaser. The −196°C
variations prescribed in Table 9.
transformation temperature corresponds to immersing a sample (prepared
according to 14.1) in liquid nitrogen for a minimum of 1 h. 16. General Requirements
16.1 The material shall be commercially smooth, uniform in
14. Test for Transformation cross section, in composition, and in temper; it shall be free of
14.1 Cut the specimen from any part of the material, but scale, corrosion, cracks, seams, scratches, slivers, and other
preferably including the entire cross section, degrease it, then defects as best commercial practice will permit.
heat treat it as described in 12.1. When cool, polish the cross
section of the specimen and etch (Note 5) it in accordance with 17. Packaging and Marking
Method E3. Then subject the specimen to the temperature 17.1 Packaging shall be subject to agreement between the
produced by an excess of dry ice in acetone (−78.5°C) for at purchaser and the seller.
least 4 h. After the low-temperature treatment, examine the
17.2 The material as furnished under this specification shall
specimen at a mangification of 150× for the presence of the
be identified by the name or symbol of the manufacturer and by
acicular crystals characteristic of the alpha phase. Because
melt number. The lot size for determining compliance with the
these crystals may occur only in small localized areas, examine
requirements of this specification shall be one heat.
carefully the entire polished cross section.
14.2 Specimens that show no transformation and that show 18. Investigation of Claims
partial transformation are illustrated in Fig. 1 and Fig. 2, 18.1 Where any material fails to meet the requirements of
respectively. this specification, the material so designated shall be handled in
NOTE 5—A suggested etchant is a solution of three parts by volume of accordance with a mutual agreement between the purchaser
concentrated hydrochloric acid and one part of concentrated nitric acid and the seller.
saturated with cupric chloride (CuCl2·2H2O). This etchant is more
effective when allowed to stand for 20 min after mixing. After several 19. Keywords
hours it loses its strength and should be discarded at the end of the day.
Etching is best accomplished by swabbing the specimen with cotton 19.1 controlled expansion alloy; glass to metal sealing;
soaked with the etchant. Etching is usually complete when the surface of iron-nickel-cobalt alloy; UNS #K94610; vacuum electronic
the metal appears to have turned dull. applications
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TABLE 6 Permissible Variations in Thickness Across Width of Strip
Maximum Variation in Thickness Across Width of Strip, Within Those Provided for in
Specified Thickness
Table 4 for Edge Measurements for Widths and Thicknesses Given, in. (mm)
Over 12 to 24 (300 to
5 (127) and Under Over 5 to 12 (127 to 300)
in. mm 600), incl
in. mm in. mm in. mm
0.005 to 0.010, incl 0.17 to 0.03, incl 0.00075 0.0191 0.001 0.025 0.0015 0.038
Over 0.010 to 0.025, incl 0.03 to 0.06, incl 0.001 0.025 0.0015 0.038 0.002 0.051
Over 0.025 to 0.065, incl 0.06 to 0.16, incl 0.0015 0.038 0.002 0.051 0.0025 0.064
Over 0.065 to 3⁄16 , excl 0.16 to 0.48, excl 0.002 0.051 0.0025 0.064 0.003 0.076
A
Any two of the three dimensional tolerances listed may be specified.
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APPENDIX
(Nonmandatory Information)
X1. Detailed Thermal Expansion Data; Annealing Conditions and Grain Growth in Piece Parts and Components
X1.1 Coeffıcient of Thermal Expansion (CTE) at Elevated TABLE X1.2 Coefficient of Thermal Expansion to Both Elevated
Temperatures— For various applications, the high- and Cryogenic Temperatures (On-Cooling Data)
temperature CTE is required for the alloy defined by this Average Linear Coefficient of
Temperature Range, °C
Thermal Expansion µm/m –°C
specification. The data provided in Table X1.1 are for material 30 to–268 4.9
produced in the early 1970s. It is important to note that the 30 to–196 6.1
CTE values cited are for annealed temper material. 30 to–163 6.4
30 to–100 6.5
30 to–78 6.5
X1.2 On-Cooling Data from 1000°C to –268°C, Using 100 to 30 6.3
30°C as Reference Temperature —The CTE data in 200 to 30 5.7
Table X1.2 is provided by a producer of the F-15 alloy. 300 to 30 5.2
400 to 30 5.0
450 to 30 5.3
X1.3 Statistical Information on CTE Requirements as Sup- 500 to 30 6.1
plied by Materials Producers—Two producers of the 600 to 30 7.8
alloy defined by this specification have provided statistical 700 to 30 8.9
800 to 30 10.1
information regarding the CTE requirements defined in Table 900 to 30 11.3
X1.3. Producer A provided both average CTE and associated 1000 to 30 12.2
standard deviation for an unspecified number of heats, which it
had produced during the past several years. All of this
information has been generated in the on-heating mode. That TABLE X1.3 Producer B Information on 30–400°C CTE Data (On-
information is shown in Table X1.4. Producer B provided Cooling DataA )
histogram information showing the distribution of CTE values, Range of CTE (µm/m –°C) Frequency of Occurrence
4.60–4.70 0.045
obtained in the on-cooling mode, for both of the temperature 4.70–4.80 0.100
ranges (30–400°C and 30–450°C) required in Table X1.3. This 4.80–4.90 0.175
information covers heats that have been produced and deter- 4.90–5.00 0.230
5.00–5.10 0.180
mined to conform to this specification in the past several years. 5.10–5.20 0.270
That information is shown in Table X1.3 and Table X1.5. A
The average of this data is 4.97 (µm/m –°C).
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TABLE X1.6 Effect of Isothermal Annealing Cycles on Grain Growth and Microhardness of F15 Alloy Lead WireA
ASTM Grain Size Number Grain Size Number for
for Mill Annealed Material Mill Annealed Material: Cold Worked Material Cold Worked Material:
Material Condition (Range of ASTM Grain Size Knoop MIcrohardness (50 (Range of ASTM Grain Knoop Microhardness (50
Numbers Based on Log- or 100 g load, as indicated) Size Numbers Based on or 100 g load, as indicated)
Normal Analysis) Log-Normal Analysis)
Starting Condition > 9.0 161 (±9.9) 5 g (N/A-cold worked 254 (±6.5) 50 g
condition)
900°C, 1 h, Wet Hydrogen 7.7 (11.1-5.9) 162 (±1.2) 50 g 7.9 (10.0-6.4 153 (±2.5) to g
Atmosphere 160. (±2.1) 100 g 156. (±4.9) 100 g
1000°C, 1 h, Wet Hydrogen 6.3 (9.0-4.3) 152 (±2.2) 50 g 6.1 (9.8-4.2) 152 (±1.3) 50 g
Atmosphere 153 (±1.5) 100 g 151. (±1.5) 100 g
1100°C, 1 h, Wet Hydrogen 5.0 (7.5-3.4) 150. (±0.5) 50 g 4.3 (7.3-2.5) 149 (±1.0) 50 g
Atmosphere 151 (±1.2) 100 g 152 (±1.8) 100 g
A
Hardness data represent the average of 10 indentations. The “range of grain size numbers” represents the intercept lengths in the range between the 10 and 90
percentiles, respectively, based on the log-normal distribution.
TABLE X1.7 Effect of Isothermal Annealing Cycle (Argon Atmosphere) on Grain Growth and Microhardness of 0.018 in. diameter F15
Alloy Lead Wire
Range of ASTM Grain Size Mill Annealed Material: Range of ASTM Grain Cold Worked Material:
Material Condition Numbers for Mill Annealed Knoop MIcrohardness (100 Size Numbers for Cold Knoop Microhardness ( 100
Material g load) Worked Material g load)
Starting Condition 8-9 177 ± 2.8 (N/A-cold worked 282 (±5.4)
condition)
900°C, 1 h, Argon Atmosphere 4-8 162 ± 9.2 6-8 163.9 ± 8.1
1000°C, 1 h, Argon Atmosphere 4-6 159 ± 9.2 5-7 159.9 ± 7.6
1100°C, 1 h, Argon Atmosphere 1-5 155 ± 5.0 0-4 154.8 ± 8.2
atmosphere. Knoop hardness values (50 g or 100 g loads) for Both cold worked and mill annealed material were examined.
both types of material are shown in Table X1.7.3 The 0.018 in. diameter wire was processed using typical
X1.4.2 Additional data, supplied by a materials producer of fabrication processing to obtain wire.
the F15 alloy, are shown in Table X1.7. Their study examined X1.4.3 The data shown in both Table X1.6 and Table X1.7
the effect of the same thermal processes, using an Argon indicate that annealing process cycles in excess of 1000°C, 1 h,
atmosphere, on the grain size and Knoop microhardness. Thus, will lead to significant grain growth in lead wire. The 1100°C,
a direct comparison could be made with the data in Table X1.6.
1 h, anneal produces coarser grain sizes that should be avoided,
if possible. It should be noted that there are some applications
3
Further details on this study can be found in the proceedings paper: Stephens, (for example, when brazing with OFHC Copper) that necessi-
J. J., Greulich, F. A., and Beavis, L. C., , “High Temperature Grain Growth and tate 1100°C process cycles. In these cases, it is important to
Oxidation of Fe-29Ni-17Co (Kovar™) Alloy Leads,” published as pages 79–112 in
the book Low Thermal Expansion Alloys and Composites, Stephens, J. J., and Frear, minimize the total time spent in excess of 1050°C in order to
D. R., eds., TMS, Warrendale, PA, 1994. avoid excessive grain coarsening.
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