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Heat Treating of Nickel and

Nickel Alloys
Abstract:

Nickel and nickel alloys may be subjected to one or more of five


principal types of heat treatment, depending on chemical
composition, fabrication requirements and intended service. These
methods include annealing, stress relieving, stress equalizing,
solution treating and age hardening.
Nickel and nickel alloys may be subjected to one or more of five principal
types of heat treatment, depending on chemical composition, fabrication
requirements and intended service.
These methods include:
Annealing.A heat treatment designed to produce a recrystallized grain structure and
softening in work-hardened alloys. Annealing usually requires temperatures
between 705 and 1205C, depending on alloy composition and degree of work
hardening.
Stress relieving. A heat treatment used to remove or reduce stresses in workhardened non-age-hardenable alloys without producing a recrystalized grain
structure. Stress-relieving temperatures for nickel and nickel alloys from 425 to
870C, depending on alloy composition and degree of work hardening.
Stress equalizing. A low-temperature heat treatment used to balance stresses in
cold worked material without an appreciable decrease in the mechanical strength
produced by cold working.
Solution treating. A high-temperature heat treatment designed to put agehardening constituents and carbides into solid solution. Normally applied to agehardenable materials before the aging treatment.
Age hardening (precipitation hardening). A treatment performed at intermediate
temperatures (425 to 870C) on certain alloys in order to develop maximum
strength by precipitation of a dispersed phase throughout the matrix.

Annealing
As applied to nickel and nickel alloys, annealing consists of heating the metal
at a predetermined temperature for a definite time and then slowly or
rapidly cooling it, to produce a change in mechanical properties - usually a
complete softening as a result of recrystalization.
Nickel and nickel alloys that have been hardened by cold working operations,
such as rolling, deep drawing, spinning or severe bending, require softening
before cold working can be continued. The thermal treatment that will
produce this condition is known as annealing, or soft annealing.
The differences in chemical composition among nickel and nickel alloys
necessitate modifications in annealing temperatures as well as in furnace
atmospheres. The precipitation-hardening alloys must be cooled rapidly after
annealing if maximum softness is desired.
Three soft-annealing methods in general commercial use - open, closed and
salt bath annealing - are described bellow (Table 2.).
Open annealing is used most often. The material to be annealed is heated at
the selected temperature and protected from oxidation by the products of
combustion in a fuel-heated furnace, or by a reducing gas introduced into an
electric furnace. Temperature control is critical because the annealing period
is short.
Closed (box) annealing requires more time than open annealing because of
the lower temperatures used. Temperature control is less critical than in
open annealing. In most instances, the weight of the container exceeds that
of the work; consequently, the amount of fuel required, heating time and
costs are greater than in open annealing.

Table 1. Nickel and nickel alloys


Material

Composition
Ni

Fe

Cu

Cr

Mo

Nickel 200

99.5

0.15

0.05

Nickel 201

99.5

0.15

0.05

Monel 400

66.0

1.35

31.5

Monel R-405

66.0

1.35

31.5

Monel K-500

65.0

1.00

29.5

Inconel 600

76.0

7.20

0.10

15.8

Inconel 601

60.5

14.1

23.0

Inconel 617

54.0

22.0

9.0

Inconel 625

61.0

2.5

21.5

9.0

Inconel 718

52.5

18.0

0.10

19.0

3.0

Inconel X-750

73.0

6.75

0.05

15.0

Hastelloy B

64.0

5.0

28.0

Hastelloy C

56.0

5.5

15.5

16.0

Hastelloy X

48.0

18.5

22.0

9.0

Table 2. Soft-annealing methods for nickel and nickel alloys


Material

Open
annealingC

Closed
annealingC

Stress
relievingC

Nickel 200

815 to 925

705 to 760

480 to 705

Nickel 201

760 to 870

705 to 760

480 to 705

Monel 400

870 to 980

760 to 815

540 to 565

Monel R405

870 to 980

760 to 815

Monel K500

870 to 1040

Not applicable

Inconel 600

925 to 1040

925 to 980

760 to 870

Inconel 601

1095 to 1175

1095 to 1175

Inconel 617

1120 to 1175

1120 to 1175

Inconel 625

980 to 1150

980 to 1150

Inconel 718

955 to 980

Not applicable

Inconel X750

1095 to 1150

Not applicable

Hastelloy B

1095 to 1185

1095 to 1185

Hastelloy C

1215

1215

Hastelloy X

1175

1175

Salt bath annealing is used for special work with small parts. Inorganic salts,
such as chlorides and carbonates of sodium, potassium and barium, which
are relatively stable at temperatures considerably above their respective
melting points, are fused in large metallic or refractory containers at
temperatures up to about 700C. At higher temperatures, heat-resisting FeNi-Cr alloy pots or refractory containers should be used. Excessive fuming of
the bath is an indication of its maximum usable temperature.
The material to be annealed is placed in molten salts and absorbs heat
rapidly. After being annealed, the work metal is quenched in water to free it
from particles of the salt mixture. The annealed material will not be bright
and may be flash pickled to achieve a bright surface.
Bright Annealing. The temperatures required for soft annealing of nickel
and nickel alloys are sufficiently high to cause slight surface oxidation unless
the materials are heated in vacuum or in a furnace provided with a reducing
atmosphere. Nickel 200, Monel 400 and similar alloys will remain bright and
free from discoloration when heated and cooled in a reducing atmosphere.
However, nickel alloys containing chromium, titanium and aluminum will
form a thin oxide film. Even if oxidation is not important, the furnace
atmosphere must be suitably sulfur-free and not strongly oxidizing.

The protective atmosphere most commonly used in heating nickel and nickel
alloys is that provided by controlling the ratio between the fuel and air
supplied to burners firing directly into the furnace. A desirable reducing
condition may be obtained by using a slight excess of fuel so that the
products of combustion contain at least 2% carbon monoxide plus hydrogen
(preferably 4%) with no more than 0.05% uncombined oxygen.
Another method of maintaining desired conditions of furnace atmosphere is
to introduce a prepared atmosphere into the heating and cooling chambers.
This can be added to the products of combustion in a direct-fired furnace;
however, introduction of prepared atmospheres is more commonly practiced
with indirectly heated equipment.
Prepared atmospheres suitable for use with nickel and nickel alloys include:
dried hydrogen, dried nitrogen, dissociated ammonia, and cracked or
partially reacted natural gas.
Dead-Soft Annealing. When the nickel alloys are annealed at higher
temperatures and for longer periods, a condition commonly described as
"dead-soft" is obtained, and hardness numbers will result that are 10 to 20%
lower than those of the "soft" condition. This cannot be accomplished
without increasing the grain size of the metal. Therefore, this treatment
should be used only for those few applications in which grain size is of little
importance.

Torch Annealing. Some large equipment is hardened locally by fabricating


operations. If the available annealing furnace is too small to hold the work
piece, the hardened sections can be annealed with the flames of oil or
acetylene torches adjusted so as to be highly reducing.
The work should be warmed gently at first, with sweeping motions of the
torch, and should not be brought to the annealing temperature until
sufficient preheating has been done to prevent cracking as a result of sudden
release of stress. (Note: Torch annealing is a poor method for general use,
because it provides irregular and insufficient annealing and produces heavily
oxidized surfaces.)
Among the more important process-control factors in annealing nickel and
nickel alloys are selection of suitably sulfur-free for heating, control of
furnace temperature, effects of prior cold work and of cooling rates, control
of grain size, control of protective atmospheres, and protection from

contamination by foreign material.

Age hardening
Age-hardening practices for several nickel alloys are summarized in the Table
3. In general nickel alloys are soft when quenched from temperatures
ranging from 790 to 1220C, however, they may be hardened by holding at
480 to 870C or above and then furnace or air-cooling. Quenching is not a
prerequisite to aging; the alloys can be hardened from the hot worked and
cold worked conditions, as well as from the soft condition.

Table 3. Age-hardening practices for nickel and nickel alloys


Alloy

Solution treated
Temperatu Cooling
re
method

Monel K-500

Inconel 718

980 C

980 C

Age hardening

WQ

Heat to 595C, hold 16h; furnace


cool to 540oC, hold 6h; furnace
cool to 480C, hold 8h; air-cool

AC

Heat to 720C, hold 8h; furnace


cool to 620C, hold until furnace
time for entire age-hardening cycle
equals 18h; air cool

Inconel X-750

Hastelloy X

AC

Heat to 845C, hold 24h; air cool;


reheat to 705C, hold 20h; air cool

980 C

AC

Heat to 730C, hold 8h; furnace


cool to 620C, hold until furnace
time for entire age-hardening cycle
equals 18h; air cool

1175 C

AC

Heat to 760C, hold 3h; air cool;


reheat to 595C, hold 3h; air cool

1150 C

Hardening Techniques. Nickel alloys usually are hardened in sealed boxes


placed inside a furnace, although small horizontal or vertical furnaces
without boxes may be used also. The box or furnace should hold the parts
loosely packed, yet afford a minimum of excess space. Electric furnaces
provide the optimum temperature uniformity of 6C and the freedom from
contamination required for this work. Gas-heated furnaces, particularly those
of the radiant-tube type, can be made to give satisfactory results. It is difficult
to obtain good results from oil heating, even with the muffle furnaces. All
lubricants should be removed from the work before hardening.
Because of the long time of aging and the difficulty of excluding air from the
box or furnace, truly bright hardening cannot be accomplished commercially.
For semibright hardening, dry hydrogen or cracked and dried ammonia
should be used. When bright or semibright hardening is not required, other
atmospheres may be used, such as nitrogen, cracked natural gas free of
sulfur, cracked city gas, cracked hydrocarbons, or a generated gas. The use of
sulfur-free gases is necessary to avoid embrittlement.
Salt baths are used occasionally for small parts. The hardened material is
never bright, and must be fresh pickled to restore the natural color. Inorganic
salts are used, such as chlorides and carbonates of sodium or potassium,
which are relatively stable at temperatures considerably above their
respective melting points. It is extremely important that the salts be free of
all traces of sulfur, so that the work does not become embrittled.
Date Published: Dec-2001

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