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Production of Aluminide Layers on AISI 304 Stainless

Steel at Low Temperatures Using the Slurry Process
Rafael Magalhães Triani, Lucas Fuscaldi De Assis Gomes, Ricardo Junior Tadeu Aureliano, Amadeu Lombardi Neto, George Edward Totten,
and Luiz Carlos Casteletti

(Submitted October 28, 2019; in revised form February 27, 2020)

Intermetallic compounds, such as iron aluminides exhibit excellent oxidation and corrosion resistance, as
well as metallurgical bonding with excellent adhesion to the substrate. In this work, aluminizing treatments
were carried out using the dipping into slurry process to produce iron aluminide coatings on stainless steel
substrates. In this process, AISI 304 stainless steel samples were immersed in a slurry consisting of poly-
vinyl butyral, ethyl alcohol and a powder composed of Al, AlCl3 and Al2O3, dried and then placed in sealed
crucibles without further protection. These samples were treated at temperatures of 500 and 650 °C for 2,
4, 6 and 8 h and then air-cooled. Flat and homogeneous layers were obtained over the substrate with
increased thickness observed with increasing temperature and treatment time. Considering that the tra-
ditional treatments of aluminization by the pack process are carried out at temperatures close to 900 °C
and use larger amounts of material, the low temperature treatments used in this work offer potential cost
savings.

layer of transition metal aluminides (Ref 1). In this process,

Keywords AISI 304, FeAl, kinetic growth, low temperature,
slurry aluminizing some parameters influence the formation of aluminide layers,
such as (i) reactivity of Al in the powder and on the substrate,
(ii) influence of the treatment atmosphere and (iii) particle size
(Ref 1). Zhan et al. (Ref 3) studied the combination of surface
grain refinement with powder aluminization, reducing the
temperature of the aluminizing process by increasing the
1. Introduction amount of grain boundaries on the surface, which act as a
pathway for faster atomic diffusion. In these tests, the
Iron, chromium and nickel aluminides have excellent prop- researchers aluminized samples of carbon steel (0.21 wt.% C)
erties against oxidation and some types of corrosion. When and Fe-5 Cr-Mo in the temperature range of 440-600 °C with
applied as protective layers over metal substrates, they increase treatment time of 25 min to 2 h in a cylindrical furnace filled
the service time of materials in high temperatures environments with FeCrAl and the aluminizing powder. The formation of
(Ref 1). The production of aluminide layers can be achieved by layers was observed in all the studied temperature range, with
several processes, such as chemical vapor deposition (CVD), layers reaching 104 lm thick in carbon steel treated at 600 °C
physical vapor deposition (PVD) or pack aluminizing, among for 2 h. Xue et al. (Ref 4) evaluated the deposition of zinc and
other techniques (Ref 2). In pack aluminizing, different aluminum simultaneously to improve resistance to corrosion
chemical compounds such as Al, AlCl3 (or NH4Cl) and and oxidation. In this study, samples of 1020 steel were treated
Al2O3, respectively, acting as Al source, activator and inert with a powder with 50 wt.% Zn, 20 wt.% Al, 2 wt.% NH4 Cl
compound (Ref 1), are typically combined. During the and 28 wt.% alumina at 460 °C for 4 h. A layer with a
treatment, reactions between Al and the activator form gaseous thickness of approximately 45 lm and two regions were
products such as chlorides (or other halides) that move through formed, the internal one being rich in Zn with 40 lm thickness
the pores in the powder mixture. Upon contact with the and the external one rich in Al with 5 lm thickness.
diffusing substrate react with the elements present and form a As the mechanism of formation of the layers occurs in a gaseous
process, it is often necessary that the treatment be made above 900-
1000 °C. It must be noted that between 550 and 800 °C the
This article is an invited submission to JMEP selected from sensitization of the stainless steels may occur due to the formation
presentations at the 30th Heat Treating Society Conference and of chromium carbides (Cr23C6) at the grain boundaries, which
Exposition held October 15-17, 2019, in Detroit, Michigan, and has decrease the corrosion and oxidation resistance of these materials
been expanded from the original presentation.
(Ref 5). Thus, the treatment temperature range is a challenge and
Rafael Magalhães Triani, Lucas Fuscaldi De Assis Gomes, some authors have been studying the process of powder aluminiz-
Ricardo Junior Tadeu Aureliano, and Luiz Carlos Casteletti, ing at low temperatures so that the sensitization is avoided or its
Materials Engineering Department, São Carlos School of Engineering, level diminished. For example, Majumdar et al. (Ref 6) studied the
University of São Paulo, São Carlos, São Paulo, Brazil; formation of layers of iron aluminides in SS 316 steel, performing
Amadeu Lombardi Neto, Department of Materials, Universidade the treatment in argon atmosphere in the temperature range of 450-
Tecnológica Federal do Paraná, Londrina, Paraná, Brazil; and
700 °C with treatment times from 4 to 16 h and in the temperature
George Edward Totten, Department of Mechanical and Materials
Engineering, Portland State University, Portland, OR. Contact e-mail: range of 800-1000 °C with treatment times from 2 to 6 h, to verify
[email protected]. the formation kinetics of the aluminide compounds during the

Journal of Materials Engineering and Performance

process after the heat treatment of solution annealing. It was layer deposited in a vapor-exposed Super304H steel tube with a
observed the formation of the compound Fe2Al5 in the range of flow rate of 100-120 mL/s at 650 °C. After 1000 h of testing, a
450-650 °C and at 900 °C the formation of layers with the FeAl thin layer of Al2O3, less than 100 nm, was observed. Evalu-
compound, which in addition to presenting a smaller thickness ating the mass gain due to oxidation showed that the
than the Fe2Al5 layer, it has lower resistance to corrosion and aluminized sample gain was much lower when compared to
oxidation. Guo et al. (Ref 7) studied the powder aluminization the untreated substrate, which at 500 h had a mass gain of
combined with the surface mechanical attrition treatment (SMAT) approximately 5 mg/cm2, whereas the treated sample had a
process in the ferritic–martensitic steel P92, in order to obtain gain of only 0.1 mg/cm2.
layers using lower process temperatures. They used a powder In addition, low temperature aluminization combined with
mixture consisting of 50 wt.% Al, 2 wt.% NH4Cl (activator) and other steps and techniques, simplifies the process, which is
48 wt.% Al2O3 (inert compound) for the treatment, which was another important objective. To this end, researchers have been
carried out at the temperature of 520-640 °C, yielding Fe2Al5 working with the aluminizing process of metals by means of the
layers with up to 40 lm thick at 600 °C for 4 h. Sakidja et al. (Ref chemical combination of aluminizing powders, polymer and
8) evaluated the low-temperature aluminization pack process for some liquid medium, in order to form a slurry solution.
NF709 stainless steel. The treatment was carried out at a Therefore, the current challenge in the production of aluminides
temperature of 650 °C for 20 h in an argon atmosphere, with a is to obtain layers at low processing temperatures, as well as, in
powder mixture of 15 wt.% Al, 10 wt.% AlCl3 (activator) and some situations, to reduce the presence of Al-rich phases due to
75 wt.% Al2O3. Two layers were formed, an outer layer of Al3Fe their brittleness.
with 5% Cr and Ni and another having the same intermetallic In this work, samples of AISI 304 stainless steel were
compound, but with twice Cr, that when exposed to high aluminized in order to study the growth kinetics of the layers
temperatures for long times was transformed into AlFe plus during low temperatures treatments.
precipitates rich in Cr. Even with this phenomenon, the oxidation
resistance at high temperatures was improved. Wang et al. (Ref 9)
evaluated the effect of adding Y2O3 as an inert compound to
aluminize AISI 309 stainless steel at low temperature. Three
2. Experimental Methods
compositions of powder (75 wt.% Al, 20 wt.% inert compound (1-
100 wt.% Al2O3, 2-50 wt.% Al2O3 + 50 wt.% Y2O3 and 3- Samples of AISI 304 stainless steel were sanded up to 600-
100 wt.% Y2O3), 5 wt.% NH4Cl activator) with treatment tem- mesh sandpaper, ultrasonically cleaned in acetone prior to the
perature at 700 °C for 6 h in an argon atmosphere. Compound 1 application of the coating and then dried and coated by
presented a layer of aluminides with a thickness of 160 lm, and the immersion in a slurry, with subsequent heat treatment for the
addition of Y2O3 in compound 3 (100 wt.% Y2O3 inert com- layer formation. For that purpose, initially a composite powder
pound) reduced the thickness of the layer to 136 lm; however, the mixture of 10 wt.% Al (140 lm), 2 wt.% AlCl3 as an activator
addition of Y2O3 delayed the degradation of the aluminide layer at and 88 wt.% Al2O3 (0.9 lm) as an inert compound was used.
high temperatures. Polyvinyl butyral (PVB) at 2:1 mass ratio (powder mixture and
The main reason for the use of aluminide layers is to PVB, respectively) and ethyl alcohol as a solvent was added to
increase the oxidation resistance at elevated substrate temper- complete the mixture, making the slightly viscous mixture. The
atures. An aluminized component when exposed to a high addition of PVB is due to the binding effect of this polymer on
temperature oxidizing environment forms a thin layer of Al2O3, the metallic substrate, which allows a higher concentration of
which has high oxidation resistance (Ref 3, 10). Previous Al in the area covered during the process.
studies have reported that this Al2O3 layer grows slowly due to After deposition of slurry by dipping, the samples were left
its highly stoichiometric structure. Agüero et al. (Ref 11) for 15 min in the air to allow the slurry to dry at room
analyzed the behavior of a layer of aluminides in a P92 steel in temperature. For the aluminization treatments, the samples
a high temperature steam environment for 60,000 h. Samples already coated with the slurry were placed in crucibles sealed
were placed in a chamber with continuous N2 flow until with cement for protection. Samples were treated at tempera-
reaching the desired temperature, where N2 flow ceased and the tures of 500 and 650 °C, for periods of 2, 4, 6 and 8 h, and then
vapor flow was started at a velocity of 8 m/s. After 60,000 h, air-cooled. The obtained layers were characterized using optical
the untreated substrate had a mass gain of approximately microscopy and x-ray diffraction (XRD) analyses, and the
90 mg/cm2, while the layered sample gained only 5 mg/cm2 kinetics of the formation of the aluminides were determined as
over the same period of time. In addition, the researchers a function of the variation of time and temperature. The process
observed that in order to maintain a dense and pure Al2O3 layer, steps of (1) dipping, (2) drying, (3) placing the samples in
the presence of a minimum aluminum content is required to sealed crucibles, (4) aluminization treatment and (5) air-cooled
regenerate the layer, which depends on the composition of the are presented in Fig. 1.
coated substrate. The presence of chromium decreases the The layers were initially characterized by optical micro-
required minimum content of aluminum from 11 to 4% by scopy (Carl Zeiss Axiotech 100HD) to verify the formation and
reducing the diffusion rate into the sample. Boulesteix et al. thickness of the surface layers. Furthermore, XRD analyses
(Ref 12) evaluated the oxidation resistance of an aluminized were performed in a Rigaku Rotaflex x-ray unit (model RU 200
P92 steel exposed to steam at a temperature of 650 °C and high B) with normal scanning from 3° to 100°, step width of
pressure (300 bar) per 10,000 h. It has been observed that there Dh = 0.2 degrees per second, Cu rotational anode with
is a pre-oxidation step prior to the formation of the Al2O3 layer. wavelength of 1.5418 Å with speed of 2 degrees per minute
In addition, only a small part of the layer was consumed by and voltage of 40 kV with 60 mA. The datasheets provided by
oxidation and there was a small increase in the interdiffusion the DRX equipment were analyzed in conjunction with
layer with the diffusion of aluminum atoms into the sample. Lu datasheets obtained from the inorganic crystal structural
et al. (Ref 13) studied the corrosion resistance of the aluminide database (ICSD).

Journal of Materials Engineering and Performance

Fig. 1 Set of steps followed to produce iron aluminide layers by slurry aluminization

Fig. 2 Micrograph of the layers of aluminides produced at 500 °C by (a) 2, (b) 4, (c) 6 and (d) 8 h in AISI 304 stainless steel

3. Results and Discussion suggested that the nickel content may favor the formation of
austenitic vacancies that improve the quality of the diffusional
3.1 Layer Morphology and XRD Analyses layer and help to promote Al diffusion.
Layers of aluminides produced at 650 °C with varying
The layers obtained in the aluminized substrates at 500 °C treatment times are shown in Fig. 3.
varying the treatment time are shown in Fig. 2. In the substrates treated at 650 °C, layers were formed with
The aluminide layers presented good thickness regularity, the same characteristics observed in the treatment carried out at
with well-defined interfaces with the substrates. In this 500 °C, that is, with a compact structure and a well-defined
treatment, the entire surface of each material was completely interface with the substrate. The formation mechanism is
covered by the layers, which was expected for this type of steel initially given by the adsorption of the active Al atoms on the
which was studied by Monteiro et al. (Ref 14). Monteiro et al. surface of the substrate, thereby diffusing toward the crystalline

Journal of Materials Engineering and Performance

Fig. 3 Micrograph of the layers of aluminides produced at 650 °C by (a) 2, (b) 4, (c) 6 and (d) 8 h in stainless steel AISI 304

structure of the metal, forming a solid solution. As the Al layer. This contributes to an improvement in oxidation
content increases to a certain concentration in that region, the resistance and avoids early spallation of the oxidized layer
aluminide layers begin to take shape on the surface of the (Ref 17, 20). Bates et al. (Ref 21) varied the amount of
substrate (Ref 15). In general, as expected, the thicknesses of aluminum in the powder composition to aluminize a martensitic
the layers increased considerably due to the increase in ferritic steel. In the mixture containing up to 20 wt.% Al in the
treatment time and temperature, in which the high Cr content master alloy, an aluminide layer containing only FeAl was
had no negative effect on the total substrate coverage by the formed. While in the mixture containing 25 wt.% Al in the
aluminides, since this element appears to decrease the capacity master alloy, a layer of FeAl and a thin outer layer of Fe2Al5
of substrates covered by aluminides (Ref 14, 15). Sun et al. were formed.
(Ref 15) produced layers of aluminides combining the slurry
process and alumina powder, in which case the researchers 3.2 Study of Growth Kinetics of Iron Aluminide Layers
observed the presence of pits in the layers formed as the
The variation of the thicknesses of the layers produced as a
treatment time increased, the same defects observed in the
function of the different treatment times at the two working
layers produced in this work.
temperatures is shown in Fig. 5.
X-ray diffraction analysis was performed on the aluminide
In the studies of Xiang and Datta (Ref 22) on the kinetics of
layer, and their diffractogram is shown in Fig. 4.
aluminization on steel alloys, the authors observed that the
In the x-ray diffraction pattern of the aluminized sample, the
process time influences the thickness of the layers and does not
formation of layers with FeAl is observed (Ref 16). These
produce additional phases. As time increases, the supply of Al
results are in accordance with coatings produced with low-
as the diffusional product from the slurry does not decrease
activity aluminum slurries, which the slurry composition,
rapidly during the process. Even though it has a high chemical
mainly the aluminum quantity of the slurry can avoid the
reactivity and the atmosphere of the furnace is not controlled,
formation of Al-rich aluminide (Ref 17). The diffraction peaks
Al is not rapidly lost during the treatment time and is even more
indicate preferred crystal growth orientation in the planes (101)
effective in the production of aluminide layers during longer
and (211) at 2h incidence angles equal to 44.17° and 81.54°,
times, regardless of the temperature applied.
respectively. In addition, peaks of lower intensities indicate the
It will be seen that the thicknesses of the layers increased
presence of Fe, Cr and Ni from the substrate at 2h incidence
with increasing treatment temperatures, but only the rate of
angles equal to 42.62°, 67.44°, 74.68° and 90.72° (Ref 18, 19).
growth of the layer changed, not its formation mechanism (Ref
Low-activity slurries contain up to 50 wt.% of aluminum in its
22). This behavior is the same as seen when treatment time
composition. In low-activity coatings, due to the reduced
rises; the Al concentration remained constant and only the
aluminum supply, the aluminide layer growth is outward,
coating thickness is increased. Xiang and Datta (Ref 22)
resulting in larger aluminide grains, thus having fewer grain
evaluated that the increase in the temperature from 500 to
boundaries, making difficult the diffusion of substrate elements,
650 °C can increase the penetration of the Al into a metallic
as chromium, titanium, tungsten, molybdenum, among others.
substrate approximately 10 to 35 lm. Even though the
Because of this, there is no formation of precipitates in the outer
aluminization kinetics theory for different metal substrates is

Journal of Materials Engineering and Performance

Fig. 4 X-ray diffraction patterns of the aluminide layers produced on AISI 304 stainless steel

Fig. 5 Layer thickness as a function of time for treatment temperatures of (a) 500 °C and (b) 650 °C

well developed and grounded, most studies concerned the related to activation energy (Q) and the temperature in kelvin
powder pack process using high process temperatures. There- (T) using the Arrhenius equation as follows in Eq 2 (Ref 23-25)
fore, the basic theory for the slurry process at low temperatures  
Q
still lacks development and foundation. The continuation of this K ¼ K0 exp : ðEq 2Þ
research should focus on applying practical and simplified RT
experiments in combination with thermodynamic theory to In this Eq 2, K0 is the pre-exponential constant and R is the
study the kinetics of aluminide formation in metallic substrates. gas constant. From there the Eq 3 can be expressed as follows:
In this work, we use theoretical calculations to study the
kinetics of aluminides layers formation by the slurry process, Q
lnK ¼ ðlnK0 Þ  : ðEq 3Þ
using a parabolic law on the basis of classical kinetic theory as RT
follows in Eq 1 (Ref 22)
From Eq 3, the graph of ln K versus the inverse of the
l 2 ¼ K  t; ðEq 1Þ treatment temperature can be obtained and afterward calcula-
tions K0 and Q are made. The graph of variation in the
where l, K and t are the thickness (cm), diffusion coefficient thicknesses of the layers produced as a function of the two
(cm2/s) and time (s), respectively. The coefficient K can be working temperatures (500 and 650 °C) are shown in Fig. 6.

Journal of Materials Engineering and Performance

 Layer thicknesses increased with increasing treatment time and
temperature.
The production of these layers at relatively low temperatures
and with the use of small amounts of aluminizing agents allows
a significant reduction of cost, thus increasing the economic
feasibility of its application. Moreover, this process allowed the
production of FeAl layers that, according to the literature, have
excellent ductility and resistance to oxidation.

Acknowledgments
This study was financed in part by the Coordenação de
Aperfeiçoamento de Pessoal de Nı́vel Superior—Brazil
(CAPES)—Finance Code 001. The authors would also like to
Fig. 6 Curves of the square of the thickness of the layer as a thank the CNPq (Conselho Nacional de Desenvolvimento
function of temperature for the different treatment times Cientı́fico e Tecnológico) Finance code 305.294/2015-6
and University of São Paulo (USP).

Conflict of interest
The authors of this manuscript declare that they have no conflict
of interest.

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