REVISTA DE METALURGIA, 47 (1)

ENERO-FEBRERO, 38-47, 2011

ISSN: 0034-8570
eISSN: 1988-4222
doi: 10.3989/revmetalmadrid.1001

Annealing of a ferritic stainless steel 409 stabilized with titanium and

zirconium additions(•)
J.L. Cavazos*, M.P. Guerrero-Mata* and P. Zambrano*

Abstract A ferritic stainless steel 409 stabilized with titanium and zirconium was subject to thermomechanical processing. It
was heated at 1210 °C for one hour, followed by a 75 % hot reduction in three passes, this rolling schedule ended
at 980 °C. Samples were cooled to 600 °C by water spraying followed by air-cooling. The alloy was pickled, and
was reduced 80 % by cold rolling. The alloy was annealed at different temperatures for 105 s. Additional annealing
treatments were carried out at temperatures of 800, 850 and 900 °C for different times. Mechanical testing and texture
were made to corroborate the degree of annealing and formability. Mechanical properties and Texture analyses showed
that the alloy annealed at 850 °C for 14 min was both completely recrystallized and a very good formability.

Keywords Ferritic stainless steel; Stabilized; Texture; Zr.

Recocido de una aleación de acero inoxidable ferrítico 409 estabilizado con

adiciones de titanio y zirconio
Resumen Un acero inoxidable ferrítico 409 estabilizado con titanio y zirconio fue sujeto a procesos termomecánicos. El acero
fue calentado a 1210 ºC durante una hora, seguido por un laminado en caliente del 75 % en tres pases, el proceso
terminó a los 980 ºC. Las muestras fueron enfriadas hasta 600 ºC por agua atomizada seguido de enfriamiento al aire.
La aleación fue decapada y laminada en frío un 80 %. Posteriormente de desarrollaron tratamientos térmicos de reco-
cido a diferentes temperaturas por un tiempo de 105 s. Adicionalmente se desarrollaron tratamientos de recocido a
temperaturas de 800, 850 y 900 ºC a diferentes tiempos. Pruebas mecánicas y textura fueron realizadas para corro-
borar el grado de recocido y su formalidad. El análisis de las propiedades mecánicas y la Textura mostraron que la
aleación recocida a 850 ºC por 14 min (840 s) fue completamente recristalizada obteniendo la mejor formabilidad.

Palabras clave Acero inoxidable ferrítico; Estabilizado; Textura; Zr.

1. INTRODUCTION Due to increasing restrictions to minimize air

pollution, the automotive industry has been requested
Ferritic stainless steels are alloys of iron and chromium to guarantee a 10 years lifetime for exhaust systems.
containing 15 - 30 % Cr with additions of Mo, Mn, Therefore, it is necessary to design new alloys with
Si, Al, Nb, Ti, and essentially free from nickel. Table I improved formability and corrosion resistance.
The main problem with stainless steels is
shows typical compositions of these alloys, particularly
sensitization, which is caused by the formation of
one of the most used for catalytic exhaust systems.
chromium carbides or nitrides at grain boundaries.
The exhaust systems of practically all passenger This phenomenon leaves a depleted chromium zone
cars produced in the United States are made from around the precipites that makes the steel
stainless steels. About 23 kg (50.6 lbs) of stainless susceptible to intergranular corrosion. Addition
steels are currently used per vehicle. This level of elements that scavenge carbon and nitrogen
translates to an annual consumption of approximately rather than chromium solves this problem. The
400,000 tons of stainless steels in a market of 15 elements that have been found to be most useful are
million vehicles per year[1]. titanium and niobium. When sensitization is

Trabajo recibido el día 12 de enero de 2010 y aceptado en su forma final del día 5 de agosto de 2010.
(•)

* Universidad Autónoma de Nuevo León, Facultad de Ingeniería Mecánica y Eléctrica, Avda. Universidad S/N, Cd. Universitaria, San
Nicolás de los Garza, Nuevo León, 66450 MEXICO. E-mail: [email protected].

38
 ANNEALING OF A FERRITIC STAINLESS STEEL 409 STABILIZED WITH TITANIUM AND ZIRCONIUM ADDITIONS
RECOCIDO DE UNA ALEACIÓN DE ACERO INOXIDABLE FERRÍTICO 409 ESTABILIZADO CON ADICIONES DE TITANIO Y ZIRCONIO

controlled, the alloy is fully stabilized. Addition 2. EXPERIMENTAL PROCEDURE

of titanium and niobium increase the corrosion
resistance[2], improves formability[3 and 4] and allows The chemical composition of the alloy was obtained
weld toughness in the produced steel[5]. from laboratory ingots; the results are presented along
A ferritic stainless steel with zirconium and with the nominal alloy values in table I. The ingots
titanium additions was designed to stabilize the alloy; were sectioned into pieces of 25.4 mm (thick) by
good corrosion resistance and very good formability 76.2 mm (wide) by 101.6 mm (long). A thermocouple
by thermomecanical processing was obtained [6]. was placed into the center of each sample. The
The term texture is used in reference to the specimens were heated at 1210 °C for one hour,
distribution of crystal orientations in a polycrystalline followed by a 75 % reduction in three passes (25.4 to
aggregate[7 and 8]. In the usual sense, it is a synonymous 6.35 cm). The temperature at the exit of the first pass
to a preferred orientation, in which the distribution was 1160 °C; at the exit the second pass was 1075
of crystal orientations is not random. A polycrystalline °C, and at the exit of the third pass was 980 °C. At
aggregate with a preferred orientation is anisotropic this point the alloys were cooled to 600 °C by water
in nature [9], i.e., it shows different properties in spray followed by air-cooling, this schedule was for
different directions. This dependence of properties avoiding martensite formation, no martensite was
on direction could be either beneficial or detrimental, found after hot rolling. The alloy was pickled in a
depending upon the intended use of the material. solution of HCl in water to remove the oxide layer.
Also, a texture that is beneficial for a particular The material was then reduced 80 % by cold rolling
application could be detrimental in another one. in four passes (6.1 mm to 1.12 mm). Table II shows
Materials that are designed to be formed are processed the rolling schedules.
to achieve a high value of rm (normal anisotropy); The samples were annealed at different
the ideal crystallographic orientation to maximize rm temperatures in the range from 300 to 900 °C with
in bcc metals would be a sheet texture with <111> intervals of 100 °C during 105 s. This procedure is
in the direction normal to the sheet and {111} the conventional treatment in a continuous
oriented randomly in the plane of the sheet [10] . annealing line. Additional heat treatments were made
The correct texture gives the proper orientation of at temperatures of 800, 850 and 900 °C at different
slip systems so that the strength in the normal times (3.5, 7 and 14 min). The temperatures were
direction (ND) is greater that than in the plane of measured in the samples using a thermocouple.
the sheet. To improve the properties of ferritic Microhardness was measured using a load of 500 g
stainless steels, one of the factors is to create a for 15 s.
desirable texture after cold rolling and annealing for Quantitative metallographic analyses were
improving deep drawability. That is to develop a performed on specimens cut from cold rolled and
strong texture <111> // ND. annealed samples using image analyzer system, to get
The objective of this work is to determinate the the average grain size and aspect ratio. A minimum
adequate temperature and time to obtain a full of 300 grains were measured for each specimen to
annealing in a ferritic stainless steel 409 with obtain a true picture of the bulk sample and obtain
zirconium and titanium additions to improve the a proper statistical distribution of the grains.
formability. Full annealing will be related by texture Texture on a local basis was obtained in a scanning
analyses and mechanical testing. electronic microscopy adapted with the TSL

Table I. Chemical Composition for alloy 409 (ASTM 240)[17] and the one selected
for this work

Tabla I. Composición Química de la aleación 409 (ASTM 240)[17] y la seleccionada

para este trabajo

C N Mn P S Si Cr Ni Ti Zr Ta

0.08 —- 1.00 0.045 0.030 1.00 10.5-11.75 0.50 6xCmin. —- —-

Nominal
max. max. max. max. max. max. 0.75 max.

This Work 0.021 0.02 0.13 —- —- 0.39 11.73 0.15 0.12 0.15 0.016

Rev. metal. 47 (1), ENERO-FEBRERO, 38-47, 2011, ISSN: 0034-8570, eISSN: 1988-4222, doi: 10.3989/revmetalmadrid.1001 39
J.L. CAVAZOS, M.P. GUERRERO-MATA AND P. ZAMBRANO

Table II. Rolling schedules Where r is given by the ration of strain along the
width direction (ε ω) to that along the thickness
Tabla II. Plan de Laminado direction (ετ), after tensile deformation of about 15

Hot Rolling
percent, the subindex refers to the tests conducted

Laminado en Caliente
on samples cut at 0,45 and 90° with respect to the
rolling direction

Pass ho hf T Reduction
(mm) (mm) (°C) (%) 3. RESULTS AND DISCUSSION
1 25.4 16.0 1.160 37
2 16.0 10.1 1.075 60
Cold rolled steel samples were annealed at different
3 10.1 6.35 980 75
temperatures for 105 s, as this is the standard time
used in continuous annealing[11]. Figure 1 shows the
microhardness variation as a function of the annealing
Cold Rolling
temperature. No recrystallization occurs below
Laminado en Frío
600 °C, as the hardness remains constant, but
between 600 and 750 °C the hardness decreases,
which can be attributed to recovery. Recrystallization
Pass ho (mm) hf (mm) Reduction (%) starts at 800 °C, when a maximum drop in hardness
is achieved. An increase in hardness at 900 °C was
1 6.1 4.3 30 detected. This phenomenon is originated as the alloy
2 4.3 3.1 50 reaches the two-phase region caused by the gamma
3 3.1 2.0 67 loop region of the Fe–Cr phase diagram, (Fig. 2) [12].
4 2.0 1.5 75 At this temperature austenite will be formed and will
5 1.5 1.12 81 transform into martensite along ferrite grain
boundaries during cooling. Two phases were identified
by means of Vickers’s microhardness indentation,
which were ferrite and martensite. The figure 3 a)
transducer to obtain the orientation by EBSD. It is shows a sample of microstructure obtained at 900 °C.
known that frictional forces at the metal and work- It can see incipient martensite in grain boundaries.
rolls interface affect the texture at the surface, which Figure 3 b) shows a micro indentation in a martensite
differs from that at the bulk of the sample. Hence, zone. Results of the micro hardness for the ferrite and
specimens of 25 mm by 20 mm by the thickness of martensite zones are HV = 130 and HV = 270
the strip were polished by mechanical means until
mid-thickness was reached; texture analyses were
carried out on this surface.
A hydraulic machine was used for tension testing.
The samples were an ASTM E8 standard (gage length
25.4 mm, width 6.25 mm, thickness 1.12 mm, length
of reduced section 31.65 mm, radius of fillet 6.25 mm,
overall length 101.4 mm) that were cut in directions
parallel, perpendicular and 45° to the rolling
direction. It was not possible to make duplicated tests
due to the small amount of material available.
Mechanical properties such as yield strength (YP),
ultimate tensile strength (UTS) and elongation (e %)
were obtained by tension testing using samples
parallel to the rolling direction. Normal anisotropy
(r-value) and planar anisotropy (∆r) were obtained
by means of:

rm = (r0 + 2r45 + r90) / 4 Figure 1. Annealing heat treatment at different

temperatures for 105 s.
(1)

and
Figura 1. Tratamiento térmico de recocido a dife-
∆r = (r0 - 2r45 + r90) / 2 (2) rentes temperaturas por 105 s.

40 Rev. metal. 47 (1), ENERO-FEBRERO, 38-47, 2011, ISSN: 0034-8570, eISSN: 1988-4222, doi: 10.3989/revmetalmadrid.1001
 ANNEALING OF A FERRITIC STAINLESS STEEL 409 STABILIZED WITH TITANIUM AND ZIRCONIUM ADDITIONS
RECOCIDO DE UNA ALEACIÓN DE ACERO INOXIDABLE FERRÍTICO 409 ESTABILIZADO CON ADICIONES DE TITANIO Y ZIRCONIO

Figure 2. Cr-Fe phase diagram.

Figura 2. Diagrama de fases Cr-Fe.

Figure 3. Microestructure of alloy annealed at 900 °C during 1.45 min (105 s): a) incipient
martensite in grain boundaries, b) micro hardness indentation into a martensite zone.

Figura 3. Microestructura de la aleación recocida a 900 °C durante 1,45 min (105 s): a) inicio
de formación de martensita en las fronteras de grano, b) Indentación de microdureza dentro

respectively. It is worth mentioning that the gamma defined as the ratio between the grain size measured
loops varies according to the chemical composition, on the longitudinal direction over the size measured
however for the current case it could be neglected. along the transversal one (Table III). This ratio is
Changes in microstructure as function of annealing related to the degree of recrystallization. Therefore,
temperature are presented in figure 4. The early stages it was necessary to perform additional annealing
of recrystallization at 700 °C can be observed. treatments for longer times.
The steel after annealing at 800 °C for 105 s shows The alloy showed improved behavior when it was
a microstructure with a large aspect ratio, which is annealed for 14 min at 800, 850, and 900 °C. Grain

Rev. metal. 47 (1), ENERO-FEBRERO, 38-47, 2011, ISSN: 0034-8570, eISSN: 1988-4222, doi: 10.3989/revmetalmadrid.1001 41
J.L. CAVAZOS, M.P. GUERRERO-MATA AND P. ZAMBRANO

Figure 4. Microstructures of alloy at different temperatures of annealing during105 s (→Rolling

Direction).

Figura 4. Microestructura de la aleación a diferentes temperaturas de recocido durante 105 s

(→Dirección del laminado).

Table III. Average size (d) and aspect ratio

after annealing for 105 s at 800 and 900 °C
It can be considered that an alloy is fully recrystallized
when almost the grains boundaries have a misorientation
Tabla III. Tamaño de grano (d) y razón de
angle higher than 15°, which means that the grains are
aspecto después del recocido por 105 s a 800
in their stable state. If the alloy is kept at a high
y 900 °C
temperature for longer times, the grain size will increase,
a process that has been called abnormal grain growth
800 °C 900 °C
or secondary recrystallization[13 and 14]. Care was taken
to avoid this problem, as there was not time enough
d (µm) Aspect. ratio d (µm) Aspect. ratio
for such a phenomenon to take place, as the
17.6 ± 13.1 1.62 ± 0.7 18.1 ± 9.6 1.44 ± 0.5
metallographic results indicate that the changes in
grain size are kept within a small range.
When two grains have a misorientaion angle less
than 15°, they can be in an unstable state, and are
size increased marginally with temperature (Table IV), known as subgrains, with time and temperature; they
showing a smaller standard deviation than when the will recrystallize by subgrain rotation and coalescence
samples were annealed for 105 s, and smaller aspect mechanisms.
ratio. These observations may be indicative that the An effective method of evaluating the degree of
alloy achieved complete recrystallization. recrystallization in a given sample is to calculate the

42 Rev. metal. 47 (1), ENERO-FEBRERO, 38-47, 2011, ISSN: 0034-8570, eISSN: 1988-4222, doi: 10.3989/revmetalmadrid.1001
 ANNEALING OF A FERRITIC STAINLESS STEEL 409 STABILIZED WITH TITANIUM AND ZIRCONIUM ADDITIONS
RECOCIDO DE UNA ALEACIÓN DE ACERO INOXIDABLE FERRÍTICO 409 ESTABILIZADO CON ADICIONES DE TITANIO Y ZIRCONIO

Table IV. Average size (d) and aspect ratio after annealing for 14 min
(840 s) at 800, 850 and 900 °C

Tabla IV. Tamaño de grano (d) y razón de aspecto después del

recocido por 14 min (840 s) a 800, 850 y 900 °C

800 °C 850 °C 900 °C

d (µm) Aspect. ratio d (µm) Aspect. ratio d (µm) Aspect. ratio

15.31 ± 6.81 1.21 ± 0.04 15.81 ± 5.15 1.28 ± 0.02 16.64 ± 5.84 1.05 ± 0.01

Table V. Area fraction of grain boundary

misorientation of samples annealed at 900 °C
volume fraction of recrystallized grains. There is an

and different times

ideal grain boundary distribution whose frequency is
random[15]. As the area fraction of grain boundary
Tabla V. Fracción de área de la desorientación
misorientation approaches the normal distribution,
de las fronteras de granos de muestra
the volume fraction of recrystallized grains increases.
recocidas a 900 °C y diferentes tiempos
Full recrystallization is achieved when both
distributions are similar.

Time (min) % Area fraction

Figure 5 shows the area fraction of recrystallized
grains annealed at 900 °C for different times versus

1.45 61.9
random distribution. It shows that, with increasing

3.5 66.4
time, the fraction area moves toward grain boundaries

7 79.7
with higher misorentation, approaching a random

14 80.6
distribution, which means that recrystallization
increases with time. Table V shows the percentage
of area fraction for the curves showed in figure 5. The

condition of the highest recrystallization at 900 °C

was found at a 14 min period.
Since the annealing at 14 min showed the
optimum results, other tests were performed at
different temperatures in order to find a higher
recrystallization.
Figure 6 shows the area fraction of samples
annealed for 14 min at different temperatures versus
random distribution. It can be seen that the behavior
between temperatures of 800 and 900 °C is almost
the same, although, the results are better for 850 °C.
Table VI shows the percentage of area fraction for
the curves showed in figure 6. The alloy at 850 °C
and at a period of 14 min time showed the best
recrystallization.
Figure 5. Comparison of the intensity of the grain Figures 7 and 8 (corresponding to {100} and {111}
boundary misorientation area fraction as function planes) show pole figures obtained from samples
of constant temperature of 900 °C at different annealed at different temperatures for constant
annealing times. holding time (14 min). This test proves that at 850 °C

Figure 9 shows an ODF section at φ2 = 45°, Bunge

the alloy has a very good fiber texture.
Figura 5. Comparación de la intensidad de la
fracción de área de la desorientación de las fron- notation, of the material annealed for 14 min at
teras de grano como función de temperatura different temperatures. The diagrams indicate an
constante a 900 °C para diferentes tiempos de
recocido.
improved gamma fiber texture in the samples
annealed at 850 °C (Fig. 9 b)).

Rev. metal. 47 (1), ENERO-FEBRERO, 38-47, 2011, ISSN: 0034-8570, eISSN: 1988-4222, doi: 10.3989/revmetalmadrid.1001 43
J.L. CAVAZOS, M.P. GUERRERO-MATA AND P. ZAMBRANO

Table VI. Area fraction of grain boundary

misorientation of samples annealed for 14 min
at different temperatures

Tabla VI. Fracción de área de la

desorientación de las fronteras de granos de
muestra recocidas por 14 min a diferentes
temperaturas

Temperature °C % Area fraction

800 77.1
850 85.0
900 80.6
Figure 6. Comparison of the intensity of the grain
boundary misorientation area fraction as function
of different annealing temperature at constant
ASTM specifications (A 240) [16], for ferritic time of 14 min (840 s).
stainless steels 409 indicate that their minimum
mechanical properties must be 205 MPa for yield Figura 6. Comparación de la intensidad de la
stress, 380 MPa for ultimate tension stress, and 20 % fracción de área de la desorientación de las fron-
of total elongation. teras de grano en función de diferentes tempe-
A major portion of ferritic stainless steel raturas de recocido a un tiempo constante de
production is cold rolled into sheet. A very substantial 14 min (840 s).

Figure 7. Resulting pole figures for alloy after annealing at different

temperatures at constant holding time 14 min (840 s){100}.

Figura 7. Resultados de la figura de polos para la aleación después del

recocido a diferentes temperaturas a tiempo constante de 14 min (840 s)
{100}.

44 Rev. metal. 47 (1), ENERO-FEBRERO, 38-47, 2011, ISSN: 0034-8570, eISSN: 1988-4222, doi: 10.3989/revmetalmadrid.1001
 ANNEALING OF A FERRITIC STAINLESS STEEL 409 STABILIZED WITH TITANIUM AND ZIRCONIUM ADDITIONS
RECOCIDO DE UNA ALEACIÓN DE ACERO INOXIDABLE FERRÍTICO 409 ESTABILIZADO CON ADICIONES DE TITANIO Y ZIRCONIO

Figure 8. Resulting pole figures for alloy after annealing at different

temperatures at constant holding time 14 min (840 s){111}.

Figura 8. Resultados de la figura de polos para la aleación después del

recocido a diferentes temperaturas a tiempo constante de 14 min (840 s)
{111}.

Figure 9. ODF section at φ2 = 45º of alloy annealing for 14 min (840 s),
at different temperatures.

Figura 9. Sección de ODF a φ2 = 45º de la aleación recocida a 14 min

(840 s) a diferentes temperaturas.

Rev. metal. 47 (1), ENERO-FEBRERO, 38-47, 2011, ISSN: 0034-8570, eISSN: 1988-4222, doi: 10.3989/revmetalmadrid.1001 45
J.L. CAVAZOS, M.P. GUERRERO-MATA AND P. ZAMBRANO

portion of this sheet is subsequently formed by Table VIII. Texture and rm values

Tabla VIII. Valores de Textura y rm

deep drawing or stretch forming and thus good sheet
formability is a very important property of ferritic
stainless steels.
The mechanical properties of 409 ferritic stainless Planes 800 °C 850 °C 900 °C
steel that support good sheet formability are low yield
stress (YP), low ultimate tensile stress (UTS), high {111}/{100} 1.48 2.41 1.25
percent elongation (e%), normal anisotropy (r-value) rm 1.22 1.94 1.2
greater than 1.5, and planar anisotropy (Dr) equal to
zero[17].
Table VII presents the results of the mechanical
additions understudy was of 850 °C during 14
properties of the samples investigated. Comparing
min. It is due to its high values of rm and texture
the current results against the values obtained from
obtained.
the annealing standard, it has been noted that the
— This annealing cycle allows the formation of a
mechanical properties (i.e. YS, UTS and e%) present
strong fiber texture which enhances the
similarities among all temperatures used during test. formability of the steel.
Nevertheless, it is important to find out among other — The mechanical properties such as YS, UTS and
properties such as anisotropy (rm) and texture, which e% present similar values in a range of 800 to
can be the key properties influencing the 900 °C for a 14 min period. These values achieve
improvement of the formability process (i.e. the annealing standard.
drawability or stretching).
Based on the current results the optimal
Acknowledgements
formability properties were achieved after a 14 min
period of annealing at 850 °C. It is due to its high
value of planar anisotropy (Table VII) and also a high
intensity ratio {111} /{100} and a strong fiber texture The authors acknowledge the advisory support
(Fig. 9 b)). Table VIII shows the texture influence provided by Professors I. C. Garcia and Q. J. DeArdo
on the rm values. The higher the intensity, the higher from University of Pittsburgh, and the financial
the rm values, it has been also reported in the case of support from Universidad Autónoma de Nuevo León,
other steels[18]. Paicyt and CONACYT.

4. CONCLUSIONS REFERENCES

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46 Rev. metal. 47 (1), ENERO-FEBRERO, 38-47, 2011, ISSN: 0034-8570, eISSN: 1988-4222, doi: 10.3989/revmetalmadrid.1001
 ANNEALING OF A FERRITIC STAINLESS STEEL 409 STABILIZED WITH TITANIUM AND ZIRCONIUM ADDITIONS
RECOCIDO DE UNA ALEACIÓN DE ACERO INOXIDABLE FERRÍTICO 409 ESTABILIZADO CON ADICIONES DE TITANIO Y ZIRCONIO

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Rev. metal. 47 (1), ENERO-FEBRERO, 38-47, 2011, ISSN: 0034-8570, eISSN: 1988-4222, doi: 10.3989/revmetalmadrid.1001 47